Title of Invention	"METHOD FOR PRODUCING A SACCHAROSE COMPOSITION, RESULTING PRODUCT AND USE THEREOF"
Abstract	The present invention pertains to a directly compressible saccharose composition. It discloses a powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules.

Title of Invention

"METHOD FOR PRODUCING A SACCHAROSE COMPOSITION, RESULTING PRODUCT AND USE THEREOF"

Abstract

The present invention pertains to a directly compressible saccharose composition. It discloses a powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules.

Full Text	FIELD OF INVENTION The present invention pertains to chemistry. More specifically it pertains to a process for the production of a directly compressible sugar (saccharose) composition and also relates to the use of the said product, for example for the production of tablets, such as pharmaceutical tablets. BACKGROUND OF THE INVENTION The presently commercially available, direct compression powders based on saccharose contain at least one binder or additive that lends the sugar its compression properties. Several products are used at present as directly compressible sugar and are obtained by co-crystallisation (Domino Dipac®), by fluidised bed agglomeration (Sudzucker Compri-Sugar®), by wet granulation (Tereos Alveo sugar®) or by compaction (Chr. Hansen Nu-Tab®). Up to now, a directly compressible saccharose powder does not exist, bearing in mind that all current processes for the preparation of directly compressed sugar cannot be used with saccharose by itself. The processes for manufacturing directly compressed sugars can be classified into four categories: agglomeration, atomisation, compaction and micro crystallisation. An agglomeration process (wet granulation and drying) relates to a process in which the sugar in solid form (often icing sugar) is agglomerated with a solution of binder, often added by spraying, followed by drying in warm air. In fact, the technique is a process for agglomerating particles of small dimension with the binder, which involves an increase in size of the particles by agglomeration. This is the process used notably for Palveosucre® (Tereos) or for Compri-Sugar® (Sudzucker). In this regard, the European patent 0 334 617 describes a process for obtaining a novel sweetener in the form of hollow spheres, said process comprising the atomisation of a solution of sugar and in the presence of C02 as the blowing agent. The bulk density of the resulting granules was approximately 0.15 to 0.2. The resulting product is therefore not made of pure saccharose and due to its low density is not compressible. A drying process by atomisation concerns drying a saccharose solution by dividing it into fine droplets that are then dried in a current of warm air. In the documents of the prior art, the processes that comprise the drying of a solution of pure saccharose require a step involving pre-crystallisation from the solution. The suspension of small crystals is then dried by atomisation. The international application WO 02/06538 describes a process for atomisation of sugars, especially saccharose, by co-atomisation of an aqueous solution of sugars or of a diluted solution of molasses with a solid material, such as powdered sugar or icing sugar. The sole products described in this document as being directly compressible are obtained by atomisation of a solution of inverted sugar, of lactose, of maltodextrins or of a mixture of these compounds: therefore they are not solely constituted by saccharose because they contain a binding agent. The patent GB 1,240,691 relates to a process for the production of a composition of non-compressible solid sugar comprising drying by atomisation of a saccharose syrup having an invert sugar content of less than 10% by weight and an inorganic ash content of less than 4% by weight. Furthermore, the percentage of residual moisture in the resulting product is more than 1%, thereby posing storage problems with the product. The patent GB 1,282,878 describes a process of atomisation by the simultaneous centrifugal dispersion of a concentrated solution of saccharose and particles of solid sugar. The process notably comprises a step of simultaneously adding the sugar solution and sugar crystals to the centrifuge. The resulting product is a powder composed of agglomerates of microcrystalline sugar, having a residual moisture content of about 0.5%, which is too high to prevent clumping of the product during storage. In the same way, other patents (GB 1 386 378, GB 1 386 379 and GB 1 387 062) describe atomisation processes for a syrup of saccharose on an added or recycled powder support. The quantity of solid used is generally very high (> 50% of the dry material of the added syrup). These processes relate to a granulation / drying of powder with a syrup deposited by atomisation. This method generally leads to an increase in granulometry and a reduction in density. A crushing step is often required to maintain a stable density and granulometry during the whole of the production. Furthermore, all the described powders have a residual moisture greater than 0.1%, thus not permitting the saccharose powders to be stored without the risk of clumping. In a process of preparation by compaction, which corresponds to a dry granulation, all the ingredients are dried and the resulting powdery composition is agglomerated under pressure, milled and sifted. Lubricants have to be added in order to avoid sticking problems. This is the process used notably for Nu-Tab® (Chr. Hansen). In a process for preparation by micro crystallisation, the sugar solution is concentrated to a dry matter content of greater than 90%, and the resulting pasty mixture is cooled under mechanical beating. A crystallisation-agglomeration of the product enables a compressible powder to be manufactured. This is the process used notably for Dipac® (Domino). Documents from the prior art do not describe a process enabling the production of a compressible saccharose powder with a residual water content that is appropriate for its conservation. Consequently, a saccharose composition adapted for direct compression and sufficiently stable for conservation has never been described up to now. SUMMARY OF THE INVENTION The present invention describes a directly compressible saccharose powder without the use of any additives and a process for making the same. OBJECTS OF THE INVENTION Accordingly, the object of the present invention is to provide a powdery, compressible saccharose exempt from other added glucides, apart from those naturally present in the saccharose, and exhibiting properties adapted to storage. A further object of the present invention is to propose a process for the preparation of a compressible, powdery saccharose composition, which is suitable for industrial application. DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules. The term "powdery saccharose composition" means saccharose micro crystals agglomerated into particles that can be themselves agglomerated together. According to a preferred embodiment, the composition according to the invention consists of hollow spheres. The term "compressible" means the ability of a powder to be formed into compressed tablets of a regular size, shape and weight in a compression machine. A directly compressible sugar is a powdery sugar that only requires one mixing step for the various ingredients (aromas, colorants, active principles, lubricants...) prior to processing in a compression machine for manufacturing compressed tablets. The powdery saccharose composition obtained according to the invention is directly compressible; thus it can be used for the preparation of compressed tablets. However, this characteristic of the composition does not limit in any way its utilisation in the manufacture of compressed tablets. The residual moisture content can be measured by a Karl Fischer determination. A residual moisture content greater than 0.1% is not appropriate for storage of the composition. In fact, with a content as high as this, the composition is not stable due to real risks of clumping. According to a preferred embodiment, the compressible, powdery saccharose composition according to the invention does not contain binders, and in particular does not contain anti-crystallisation agents. When required, the powdery composition according to the invention can also comprise aromas or colorants in amounts of less than 0.9% by weight based on the total weight of the composition. Preferably, the sugar used is a sugar manufactured from or refined from cane sugar or beetroot, comprising when dry at least 99.1% by weight of saccharose determined by the polarimetric method. The present invention relates to a powdery composition as defined above comprising at least 99.7% by weight of saccharose. Preferably, the qualities sugar or white sugar, refined sugar or refined white sugar are used, which comprise a minimum of 99.7% saccharose and which moreover conform to the Directive EU nr. 2001/111 (OJEU 12 January 2002), in particular with an invert sugar content of less than or equal to 0.04% by weight. It is also possible to use semi-white sugar, which comprises a minimum of 99.5% saccharose and which moreover conforms to the European Directive EU nr. 2001/111 (OJEU 12 January 2002) and all sugar containing, in the dry state, at least 99.1% saccharose and with an invert sugar content of less than or equal to 0.1%. In all cases, the invert sugar, present in minor amounts, results from the manufacture or the refining of sugar and is not subsequently added by mixing; thus at this minor level it cannot act as an anti-crystallisation agent that enables the crystallisation of the saccharose to be controlled during drying, as defined in the international application WO 03/000936. Maltodextrins, monosaccharides, oligosaccharides and polyols can be cited as other examples of anti-crystallisation agents. Accordingly, none of the compounds that are naturally present apart from the 99.1% and particularly the 99.7% of saccharose are in sufficient quantity to play the role of anti-crystallisation agent, even if maltodextrins, monosaccharides, oligosaccharides and polyols are found among these compounds. According to an advantageous embodiment, the powdery composition according to the invention does not comprise any added glucides other than the saccharose. Therefore, this composition does not comprise any other glucides than those present naturally in the utilised saccharose. According to an advantageous embodiment, the powdery composition according to the invention comprises only saccharose resulting from the manufacture or refining of cane sugar or beetroot. Furthermore, the impurities contained in the saccharose used in the context of the present invention cannot in general be considered as binders or as anti-crystallisation agents. The present invention preferably relates to a powdery composition as defined above, comprising 100% by weight of saccharose. The present invention also relates to a powdery composition as defined above, characterised in that the average granulometry or average opening of the hollow particles alone or agglomerated varies from about 140 to about 350 urn. As the granulometric analyses are carried out by sieving, the average opening (AC)) corresponds to the mesh size that retains 50% by weight of the sample. When the size of the particles is greater than 350 urn, then such a composition is no longer suitable for the manufacture of small size compressed tablets because of the difficulty associated with filling the die of the compression machine. When the size of the particles is less than 140 µm, the flow properties of the powder are debased resulting in significant variations in the weight of the compressed tablets. The present invention relates to a powdery composition as defined above, characterised in that the coefficient of variation of said particles varies from about 35 to about 55, especially from about 40 to about 50. The term "coefficient of variation" denotes the level of dispersion about the average opening, i.e. the mesh size that retains 50% by weight of the sample. More precisely, the coefficient of variation is equal to the standard deviation of the distribution expressed as a percentage of the average opening. These granulometric dispersion limits enable a compressible powder to be obtained that offers the best compromise in terms of powder flow and the fillability of the dies of the compression machine. The present invention also relates to a powdery composition as defined above, characterised in that its bulk density is in the range of about 0.45 to about 0.75. The term "bulk density" denotes the measured density of the powder; this is therefore the ratio of the mass of the powder to the volume occupied by the powder. This bulk density differs from the true density of the powder, which refers to the ratio of the mass of the powder to the volume totally filled by said powder without any volume of air. The degree of compaction of a powder is the relation between the density of the compressed tablet and the true density of the powder. The tap density and the non-tapped bulk density are defined according to the method described by the European Pharmacopoeia (5th edition - Methods of pharmaceutical technology 2.9.15). For evaluating the flow properties and the packing capacity of a powder, one can also measure the Carr's Index which allows the flowability of a powder to be evaluated and corresponds to the following ratio: Carr's Index = 100 x tap density - bulk density tap density Thus, the flowability and packing capacity of powders as a function of Carr's Index are shown in the Table below: (Table Removed) In the context of the present invention, the Carr's Indeces of the powdery compositions obtained according to the invention are comprised between 8 and 17%. A preferred powdery composition according to the present invention is a composition as defined above and exhibiting a flow time of less than about 15 seconds. The flow is that defined according to the method described in the European Pharmacopoeia (5th edition - Methods of pharmaceutical technology 2.9.15). According to an advantageous embodiment, the present invention relates to a powdery composition as defined above, characterised in that it exhibits a degree of crystallinity greater than or equal to 95%, especially greater than or equal to 99%. The degree of crystallinity is determined by means of an X-ray diffraction measurement of the crystallinity of the powdery composition compared with the crystallinity of pure crystals of saccharose. The powdery composition according to the invention is characterised in that it comprises substantially no vitreous or amorphous phase. The present invention also relates to a powdery composition such as defined above, characterised in that it is able to be compressed, the strength of the compressed powder obtained from the powdery composition being greater than about 1 MPa, said strength being measured for a compression force greater than about 15 kN, and the compressed powder meeting an ejection force ranging between about 50 to about 80 N, said ejection force being measured for a compression force comprised between about 15 to about 20 kN. The resistance of the obtained compressed tablets is measured according to the method described in the European Pharmacopoeia, chapter 2.9.8 (1997). The compression mechanism used for compressing the sugar composition according to the invention is, for example a compression machine commercialised by the FROGERAIS Company, and equipped with two punches, only the upper punch being used for the compression. It should be noted that the strength measurement partially depends on the type of compression machine used; thus, if the lower and upper punches are used simultaneously for the compression then the strength of the resulting compressed tablets will be greater. The ejection force is the force that has to be applied to the lower punch in order to free the compressed tablet. The measured values on the powders according to the invention are indicated on the curves and compared on the same curves to the values obtained with the powder of the prior art (see Figures 2 and 3). Description of the manufacturing process The present invention also relates to a continuous process for manufacturing a compressible, powdery saccharose composition such as defined above and comprising: a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and an optional cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition ranging from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. The term "nebulised saccharose solution" denotes the dispersion of a saccharose solution, particularly in the form of a syrup, into fine droplets by means of a nozzle or a centrifuge. The term "atomisation tower" denotes the installation that enables a nebulised saccharose solution to be dried. The term "drying step" denotes the dehydration step of the droplets of sugar syrup by hot air. The term "glassy particles of saccharose" denotes the dehydrated but still not crystallised droplets of syrup. A saccharose solution (input saccharose solution or initial saccharose solution), including in the form of syrup, is fed into an enclosure equipped with atomisation and drying means. The first step of the process consists of a drying step of the saccharose solution, including in the form of a syrup in the form of droplets, nebulised by means of a nozzle or a centrifuge. Thus, this step consists in drying the drops of saccharose formed by nebulisation to solid particles with a hot air flow, whose entrance temperature into the atomisation tower (or drying chamber) varies from about 140 to about 180 °C. The hot air used for drying is recovered at the exit of the atomisation tower charged with humidity. The term "stabilisation and crystallisation step" denotes the process of crystallisation of the glassy sugar particles on contacting the crystalline saccharose particles. The expression "essentially crystallised powdery composition" denotes the still not cooled powdery saccharose composition. The second step of the process consists in contacting the glassy particles resulting from the first drying step with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible powdery saccharose composition. This second step notably enables the crystallisation of the saccharose to be initiated. This step of contacting corresponds to a collision between the unstable glassy particles resulting from the first drying step with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible powdery saccharose composition. The composition obtained from this contacting step is essentially crystallised. In fact, this two-step drying mode retards the crystallisation of the saccharose syrup by passing through an amorphous (or glassy) state. This initiation of the crystallisation, retarded by adding essentially crystallised saccharose and/or recycled compressible saccharose outside the nebulization/drying zone of the syrup, permits the formation of crystals of reduced size in each hollow particle. By adopting this processing mode, an arrangement of crystals is obtained, which is similar to that obtained, for example, by the process described in the international application WO 03/000396, in which the addition of an anti-crystallisation agent is required. In the following, the term "recycled powdery composition" denotes either a part of the recycled, essentially crystallised powdery composition, i.e. part of the powdery composition obtained prior to the cooling step in air (non-cooled composition), or part of the recycled, compressible powdery saccharose, i.e. part of the powdery composition obtained after drying in air (composition cooled at a temperature below 30 °C). Consequently, the process of the invention is characterised by the use of a recycled powdery composition as defined above. Thus, a percentage of the recycled, essentially crystallised powdery composition or of the compressible powdery saccharose composition is removed in order to reuse it in the stabilisation and crystallisation step, and therefore to contact said recycled powdery composition with the abovementioned glassy particles. The amount of recycle of the powdery composition or of the powder varies from 30 to 70% by weight of dry matter of the nebulised saccharose solution. Of course it is possible to obtain the desired powdery composition by working with a higher recycle rate, particularly higher than 70%. On the other hand, if the recycle rate is less than 30%, the number of collisions of the glassy particles with the recycled crystalline powder is insufficient, thereby causing a part of the powder to stick to the walls of the atomisation tower and limiting the industrial interest of the process. According to a preferred embodiment, the preparation process of the invention is characterised in that the recycled powdery composition comes from the compressible powdery saccharose composition such as obtained at the end of the cooling step as defined above. Accordingly, in this preferred embodiment, the recycled powdery composition used during the contacting with the glassy particles obtained at the end of the drying step, comes from the composition as obtained in the cooling step. If the residual moisture content is greater than 1%, the resulting product is an unstable product that continues to lose water, and this water can condense onto any wall whose temperature is lower than that of the water. This phenomenon generally leads to clumping. This characteristic is important because it affects the ability of the powder to remain powder/ and to retain its flowability. For a direct compression powder, this parameter directly influences the regularity of the weight and density of the compressed tablets. Thus, a powder that is too moist will contain agglomerates that will impede the facile filling of the dies of the compression machine and will lead to a rapid increase in the ejection forces of the compressed tablets and a premature fouling of the equipment. The product obtained from the conclusion of the contacting step as defined above is a non-cooled and unstable product. Accordingly, for storage, it is advantageous, if not necessary, to subject the product to a cooling step. Without this cooling step, the product obtained is too sensitive to climatic changes and becomes rapidly unusable. The compressible powdery saccharose composition according to the invention is obtained at the conclusion of the process. The present invention also relates to a continuous process for manufacturing a compressible, powdery saccharose composition such as defined above and comprising: a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, a contacting step of said glassy particles as obtained at the conclusion of the preceding step with a powder of saccharose crystals, said powder being present in a quantity corresponding to about 30 to about 70% by weight of dry matter of the nebulised saccharose solution, to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and an optional cooling step in air of the essentially crystallised powdery composition to obtain the compressible powdery saccharose composition, said composition being crystallised and having a temperature of less than 30 °C. According to a preferred embodiment, the powder of saccharose crystals is a recycled powder coming from either an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight, such as obtained at the conclusion of the contacting step as defined above, or from the compressible powdery saccharose composition such as obtained at the conclusion of the cooling step. Preferably, the powder of saccharose crystals is a recycled powder coming from the compressible powdery saccharose composition such as obtained at the conclusion of the cooling step. The process of the present invention is characterised in that it corresponds to a continuous process carried out after a start-up phase to obtain a steady state. Consequently, the granulometry does not increase and a powder exhibiting constant properties is obtained from this process. Process start-up is carried out with saccharose powder from a previous production until the desired powdery composition is obtained. For the first start-up of the process of the invention, a crystallisation initiator is used, i.e. an initial crystallisation initiator as the recycled powdery composition (or powder of saccharose crystals) such as defined above. An initiator of this type is a compound that serves to initiate the crystallisation during drying, as long as no powdery composition obtained according to the invention is available. In particular, icing sugar or any other sugar crystal is used as the crystallisation initiator. Once a sufficient quantity of the powdery composition has been obtained for use as the crystallisation initiator, i.e. as the recycled powdery composition (or powder of saccharose crystals) for the contacting step, then the icing sugar used as the crystallisation initiator is eliminated. The present invention also relates to a continuous process for manufacturing a compressible, powdery saccharose composition such as defined above and comprising: a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after the drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, and a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said recycled, essentially crystallised powdery composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. This embodiment comprises the use of a part of the recycled, essentially crystallised powdery composition for the stabilisation and crystallisation step. The present invention relates to a continuous process for manufacturing a compressible, powdery saccharose composition such as defined above and comprising the following steps: a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. This embodiment comprises three steps: the drying step, the stabilisation and crystallisation step (collision of the glassy particles with the recycled powdery composition) and the cooling step. A specific embodiment of the process of the present invention comprises the use of both a part of the essentially crystallised powdery composition and a part of the compressible powdery composition as the recycled powdery composition. The present invention also relates to a continuous process for manufacturing a compressible, powdery saccharose composition such as defined above and comprising the following steps: a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and a cooling step in air of the essentially crystallised powdery composition to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. This embodiment comprises three steps: the drying step, the stabilisation and crystallisation step (collision of the glassy particles with the recycled powdery composition) and the cooling step. It is also characterised by the use of a part of the recycled, essentially crystallised powdery composition for the contacting step with the glassy particles. The present invention also relates to a continuous process for manufacturing a compressible, powdery saccharose composition such as defined above and comprising the following steps: a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose. a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. This embodiment comprises three steps: the drying step, the stabilisation and crystallisation step (collision of the glassy particles with the recycled powdery composition) and the cooling step. It is also characterised by the use of a part of the recycled, compressible powdery saccharose composition for the contacting step with the glassy particles. The present invention also relates to a continuous process for the manufacture of a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than or equal to 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising: a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and an optional cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition ranging from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. The present invention also relates to the product as obtained by the process as defined above. The present invention also relates to a continuous process for the manufacture of a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than or equal to 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising: a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after the drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, and a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. The present invention also relates to the product as obtained by the process as defined above. The present invention also relates to a continuous process for the manufacture of a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than or equal to 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising: a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. The present invention also relates to the product as obtained by the process as defined above. The present invention also relates to a continuous process for the manufacture of a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than or equal to 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising: a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and a cooling step in air of the essentially crystallised powdery composition to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. The present invention also relates to the product as obtained by the process as defined above. The present invention also relates to a continuous process for the manufacture of a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than or equal to 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising: a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the saccharose solution. The present invention also relates to the product as obtained by the process as defined above. The present invention also relates to a continuous process for the manufacture of a compressible, powdery saccharose composition comprising at least 99.7% by weight of saccharose, exhibiting a residual moisture content of less than or equal to 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising: a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air used for drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. The present invention also relates to the product as obtained by the process as defined above. According to a preferred embodiment, the process of the invention is characterised in that the drying step is carried out in the immediate vicinity of the nebulization zone, especially in the upper part of the atomisation tower. The term "nebulisation zone" denotes the zone where the nebulisation step of the process is carried out, i.e. the zone where the drying step by hot air is carried out. The term "upper part of an atomisation tower" denotes the nebulisation and drying zone of the sugar syrup. The process of the invention is preferably characterised in that the contacting step is carried out in the atomisation tower, under conditions such that the recycled composition is added at the level of a zone comprised between the first third and the second third of said atomisation tower, and especially at the level of the middle zone of said atomisation tower. According to yet another preferred embodiment, the contacting step is carried out outside the nebulisation and drying zone as described above. The present invention also relates to a process as defined above, characterised in that the cooling step is carried out outside the atomisation tower. According to an advantageous embodiment, the process of the invention is characterised in that the cooling step is carried out under conditions that enable the residual moisture content of the essentially crystallised powdery composition to be reduced and also the crystallisation of said composition to be terminated so as to obtain the compressible powdery crystallised saccharose composition. Either a fluidised bed, a drum dryer or any other means to cool the powdery composition can be used for this cooling step. The present invention also relates to a process as defined above, in which the initial saccharose solution has a dry matter content of about 55 to 80% by weight. The dry matter content of a product corresponds to the percentage of dry extract of said product. Moreover, as an illustrative and non-limiting example, the input flow of saccharose syrup to be nebulised varies from about some kg/h to about several thousands of kg/h, particularly from about 500 kg to about 2000 kg/h, depending on the size of the atomisation tower and its drying capacity. The present invention relates to the use of a compressible powdery sugar composition as defined above, for the manufacture of compressed tablets, such as pharmaceuticals. The present invention relates to the use of a compressible powdery sugar composition as defined above, for the manufacture of powdery mixtures. The present invention relates to the use of a compressible powdery sugar composition as defined above, for the manufacture of fast-dissolving formulations. The present invention also relates to the use of a compressible powdery sugar composition as defined above, in a mixture with at least one other product, said other product being in soluble or powdery form. Advantageously, said other product is an active principle, a sweetener, a colorant, an aroma, an enzyme or a surfactant. According to an advantageous embodiment, the mixture obtained in this way, comprising the compressible powdery sugar composition as defined above and said other product, comprises 10% by weight at most of said other product based on the weight of the mixture. The present invention also relates to the use of a compressible powdery sugar composition as defined above, for the manufacture of sugar spheres, such as by coating and/or lamination and/or sugar coating. The sugar spheres are spherical or quasi-spherical particles constituted by a saccharose core, onto which can be deposited successive layers of glucides and/or colloids and/or waxes or fats. The size of the resulting particles can vary from some tens of micrometres to some millimetres. Considering the shape of the particles and their surface characteristics (Figures 4A and 4B), the compressible powdery sugar composition according to the invention is perfectly adapted for the manufacture of sugar spheres. In fact, with an almost spherical shape, the powder obtained by atomisation enables spheres to be very easily formed by lamination, coating or sugar coating. Due to its surface characteristics, this powder permits the deposition of both hydrophilic (glucides, colloids, etc..) as well as hydrophobic substances (oils, waxes etc.). DESCRIPTION OF THE ACCOMPANYING DRAWINGS Figure 1 represents a general scheme of the process of the invention. The arrow 1 indicates the introduction of the saccharose syrup into the atomisation tower (A). The drying air (2) is introduced into the drying zone (4) and the moist air (3) is recovered at a temperature of between 80 and 140 °C. Zone (5) corresponds to the zone of the atomisation tower where the stabilisation and crystallisation step takes place. A part of the essentially crystallised powdery composition obtained from this stabilisation and crystallisation step can be recycled and reintroduced (6) for example into the atomisation tower (A). The essentially crystallised powdery composition is subjected to a cooling step (7) to obtain a cooled compressible powdery composition (9). A part of this cooled compressible powdery composition can likewise be recycled and reintroduced (8) into the atomisation tower (A), it being understood that the process of the invention necessarily comprises recycling of the powdery composition, i.e. either step (6) or step (8). Figure 2 represents the comparative graphs of the crushing strength (in MPa) of the compressed tablets obtained from pilot plant experiments as a function of the compression force (in kN). The curve with the black squares refer to the sugar Dipac; the curve with the black triangles refer to the powdery composition of example 1; the curve with the black lozenges refers to the powdery composition of example 2 and the curve with the black circles refers to the powdery composition of example 3. An examination of the graphs of Figure 2 reveals that the powdery compositions from examples 1 to 3 according to the invention exhibit higher strengths for a given compression force than the reference commercial product (Dipac). Figure 3 represents the comparative graphs of the ejection force (in N) supported by the obtained compressed tablets as a function of the compression force (in kN). The curve with the black squares refer to the sugar Dipac; the curve with the black triangles refer to the powdery composition of example 1; the curve with the black lozenges refers to the powdery composition of example 2 and the curve with the black circles refers to the powdery composition of example 3. The graphs of Figure 3 demonstrate that the results obtained with the compressible saccharose powders of the invention are comparable with those obtained for the commercial product Dipac® in terms of ejection force for a given compressive force. The graphs of Figures 2 and 3 should be analysed in conjunction because the ejection force supported by a compressed tablet without risk of breakage cannot be disassociated from the strength of the compressed tablet. Thus, the compressed tablets obtained and made up from powdery saccharose compositions according to the invention exhibit the strength/ejection force relationships comparable to those obtained from the commercial product Dipac®. Figures 4A and 4B represent scanning electronic microscopy images of the directly compressible powdery composition. Figure 4A shows that the powdery composition obtained is composed of isolated hollow particles or associated particles that form granules. Figure 4B represents in detail a hollow particle of about 200 urn, made up of agglomerated micro crystals and associated with other particles of variable dimensions. EXAMPLES Example 1 A saccharose solution (65% dry matter) was nebulised at 102 bars in a drying chamber under a hot air flow. The temperature of the drying air was adjusted as a function of the required exit temperature of the moist air. The powder exiting the drying chamber was cooled and partially recycled (recycle rate was 40 % based on the dry matter of the syrup feed) towards the lower part of the chamber, outside the nebulisation zone of the solution. Operating parameters: Entrance (Table Removed) Properties of the dried powder (Table Removed) Example 2 A saccharose solution (65% dry matter) was nebulised at 210 bars in a drying chamber under a hot air flow. The temperature of the drying air was adjusted as a function of the required exit temperature of the moist air. The powder exiting the drying chamber was cooled and partially recycled (recycle rate was 40% based on the dry matter of the syrup feed) towards the lower part of the chamber, outside the nebulisation zone of the solution. Operating parameters: Entrance (Table Removed) Exit Properties of the dried powder (Table Removed) The powdery saccharose composition obtained according to the invention performs as well as an obtained powder formulated with binders (see Figures 2 and 3). Example 3 A saccharose solution (55% dry matter) was nebulised at 210 bars in a drying chamber under a hot air flow. The temperature of the drying air was adjusted as a function of the required exit temperature of the moist air. The powder exiting the drying chamber and not cooled was partially recycled (recycle rate was 35% based on the dry matter of the syrup feed) towards the lower part of the chamber, outside the nebulisation zone of the solution. Operating parameters: Entrance (Table Removed) Properties of the dried powder The powdery saccharose composition obtained according to the invention performs as well as an obtained powder formulated with binders (see Figures 2 and 3). Recycling the essentially crystallised powder enabled a product to be obtained that was absolutely comparable with the products obtained according to examples 1 and 2. Composition and procedure for obtaining compressed tablets The compressed tablets were obtained from an alternating machine Frogerais OA equipped with compression chamber having an 11.28 mm section. The machine speed was 3350 cps/hour. Prior to the compression step, the powdery compositions were mixed with 0.5 (Dipac) or 0.75% (atomised powders according to the invention) magnesium stearate for 5 minutes in a mixer with a three-dimensional random action. The round and flat compressed tablets were prepared with compression forces of 10, 20 and 30 kN. Example 4 In this example, a colorant was chosen to simulate an ingredient (active principle, aroma, enzyme, surfactants etc....). The colorant of chosen granulometry was mixed with the sugar dried by atomisation (composition of the invention). The homogeneity of the mixture was evaluated as a function of the mixing time, the addition level and the size of the colorant particles. Due to its morphology and its surface characteristics, the sugar dried by atomisation enabled perfectly homogeneous mixtures to be obtained. In fact, even with a blade mixer, the mixtures obtained under the above-described conditions have a homogeneous distribution with a standard deviation of always less than 2% (average of 10 samples). Homogeneity of the mixture as a function of mixing time (Table Removed) Homogeneity of the mixture as a function of additive content (Table Removed) Homogeneity of the mixture as a function of particle size of the colorant (Table Removed) According to these results, it can be observed that all the mixtures obtained were homogeneous mixtures because no subsequent demixing was observed (stable mixture). Method for analysing the colorant The colorant in the mixture was analysed by measuring the absorbance in a UV/visible spectrometer UNICAM UV4 at a wavelength of 500 nm with a 10 mm long cell. The percentage of colorant was calculated from measurements carried out on standard solutions. ' We claim: 1. Compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules. 2. Powdery composition according to claim 1, comprising at least 99.7% by weight of saccharose. 3. Powdery composition according to claim 1 or 2, characterised in that the average granulometric distribution of the hollow or agglomerated particles varies from about 140 to about 350 urn. 4. Powdery composition according to claim 3, characterised in that the coefficient of variation of said particles varies from about 35 to about 55, particularly from about 40 to about 50. 5. Powdery composition according to any one of claims 1 to 4, characterised in that its bulk density is in the range of about 0.45 to about 0.75. 6. Powdery composition according to any one of claims 1 to 5, characterised in that its flow time is less than about 15 seconds. 7. Powdery composition according to any one of claims 1 to 6, characterised in that it is able to be compressed, the strength of the compressed powder obtained from the powdery composition being greater than about 1 MPa, said strength being measured for a compression force greater than about 15 kN, and the compressed powder meeting an ejection force comprised between about 50 to about 80 N, said ejection force being measured for a compression force comprised between about 15 to about 20 kN. 8. Continuous process for manufacturing a compressible, powdery saccharose composition such as defined in any one of claims 1 to 7, comprising: - a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose, - a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and - an optional cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition ranging from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. 9. Continuous process for manufacturing a compressible, powdery saccharose composition such as defined in any one of claims 1 to 7, comprising: - a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after the drying and exiting said tower being comprised between about 80°C to 140 °C, for obtaining the glassy particles of saccharose, and - a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30% to about 70% by weight of dry matter of the nebulised saccharose solution. 10. Continuous process for manufacturing a compressible, powdery saccharose composition such as defined in any one of claims 1 to 7, comprising the following steps: - a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air used for drying and exiting said tower being comprised between about 80°C to 140 °C, for obtaining the glassy particles of saccharose, - a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and - a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. 11. Continuous process for manufacturing a compressible, powdery saccharose composition such as defined in any one of claims 1 to 7, comprising the following steps: - a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose, - a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and - a cooling step in air of the essentially crystallised powdery composition to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. 12. Continuous process for manufacturing a compressible, powdery saccharose composition such as defined in any one of claims 1 to 7, comprising the following steps: - a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose, - a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and - a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. 13. Process according to any one of claims 8 to 12, wherein the drying step is carried out in the immediate vicinity of the nebulisation zone, especially in the upper part of the atomisation tower. 14. Process according to any one of claims 8 to 13, wherein the contacting step is carried out in the atomisation tower, under conditions such that the recycled composition is added at the level of a zone comprised between the first third and the second third of said atomisation tower, and especially at the level of the middle zone of said atomisation tower. 15. Process according to any one of claims 8 to 14, characterised in that the cooling step is carried out outside the atomisation tower. 16. Process according to any one of claims 8 to 15, characterised in that the cooling step is carried out under conditions enabling the residual moisture content of the essentially crystallised powdery composition to be reduced and also the crystallisation of said composition to be completed in order to obtain the compressible, powdery, crystallised saccharose composition. 17. Process according to any one of claims 8 to 16, wherein the initial saccharose solution has a dry matter content of about 55 to 80% by weight. 18. Continuous process for manufacturing a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising: - a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose, - a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and - an optional cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30°C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition ranging from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. 19. Continuous process for manufacturing a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising: - a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after the drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose, and - a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised, powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30% to about 70% by weight of dry matter of the nebulised saccharose solution. 20. Continuous process for manufacturing a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising: - a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose, - a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and - an cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. 21. Continuous process for manufacturing a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising: - a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose, - a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and - a cooling step in air of the essentially crystallised powdery composition to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30°C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. 22. Continuous process for manufacturing a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising: - a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose, - a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and - a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, compressible, powdery composition, the amount of recycle of said compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution. 23. Continuous process for manufacturing a compressible, powdery saccharose composition comprising 100% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising: - a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air used for drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose, - a stabilisation and crystallisation step of the glassy particles obtained from the drying step, to obtain an essentially crystallised, powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and - a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition varying from about 30% to about 70% by weight of dry matter of the nebulised saccharose solution. 24. Compressible, powdery sugar composition such as obtained by the process according to one of claims 18 to 23. 25. Use of a compressible, powdery sugar composition according to one of claims 1 to 7 or 24, for manufacturing compressed tablets, such as pharmaceuticals. 26. Use of a compressible, powdery sugar composition according to one of claims 1 to 7 or 24, for manufacturing powdery mixtures. 27. Use of a compressible, powdery sugar composition according to one of claims 1 to 7 or 24, for manufacturing fast-dissolving formulations. 28. Use of a compressible powdery sugar composition according to one of claims 1 to 7 or 24, in a mixture with at least one other product, said other product being in soluble or powdery form, and being selected from among the following products: active principle, sweetener, colorant, aroma, enzyme or surfactant. 29. Use of a compressible, powdery sugar composition according to one of claims 1 to 7 or 24, for manufacturing sugar spheres, especially by coating and/or lamination and/or sugar coating.

Full Text

FIELD OF INVENTION
The present invention pertains to chemistry. More specifically it pertains to a process for the production of a directly compressible sugar (saccharose) composition and also relates to the use of the said product, for example for the production of tablets, such as pharmaceutical tablets.
BACKGROUND OF THE INVENTION
The presently commercially available, direct compression powders based on saccharose contain at least one binder or additive that lends the sugar its compression properties.
Several products are used at present as directly compressible sugar and are obtained by co-crystallisation (Domino Dipac®), by fluidised bed agglomeration (Sudzucker Compri-Sugar®), by wet granulation (Tereos Alveo sugar®) or by compaction (Chr. Hansen Nu-Tab®).
Up to now, a directly compressible saccharose powder does not exist, bearing in mind that all current processes for the preparation of directly compressed sugar cannot be used with saccharose by itself.
The processes for manufacturing directly compressed sugars can be classified into four categories: agglomeration, atomisation, compaction and micro crystallisation.
An agglomeration process (wet granulation and drying) relates to a process in which the sugar in solid form (often icing sugar) is agglomerated with a solution of binder, often added by spraying, followed by drying in warm air.
In fact, the technique is a process for agglomerating particles of small dimension with the binder, which involves an increase in size of the particles by agglomeration.
This is the process used notably for Palveosucre® (Tereos) or for Compri-Sugar® (Sudzucker).
In this regard, the European patent 0 334 617 describes a process for obtaining a novel sweetener in the form of hollow spheres, said process comprising the
atomisation of a solution of sugar and in the presence of C02 as the blowing agent. The bulk density of the resulting granules was approximately 0.15 to 0.2. The resulting product is therefore not made of pure saccharose and due to its low density is not compressible.
A drying process by atomisation concerns drying a saccharose solution by dividing it into fine droplets that are then dried in a current of warm air. In the documents of the prior art, the processes that comprise the drying of a solution of pure saccharose require a step involving pre-crystallisation from the solution. The suspension of small crystals is then dried by atomisation.
The international application WO 02/06538 describes a process for atomisation of sugars, especially saccharose, by co-atomisation of an aqueous solution of sugars or of a diluted solution of molasses with a solid material, such as powdered sugar or icing sugar. The sole products described in this document as being directly compressible are obtained by atomisation of a solution of inverted sugar, of lactose, of maltodextrins or of a mixture of these compounds: therefore they are not solely constituted by saccharose because they contain a binding agent.
The patent GB 1,240,691 relates to a process for the production of a composition of non-compressible solid sugar comprising drying by atomisation of a saccharose syrup having an invert sugar content of less than 10% by weight and an inorganic ash content of less than 4% by weight. Furthermore, the percentage of residual moisture in the resulting product is more than 1%, thereby posing storage problems with the product.
The patent GB 1,282,878 describes a process of atomisation by the simultaneous centrifugal dispersion of a concentrated solution of saccharose and particles of solid sugar. The process notably comprises a step of simultaneously adding the sugar solution and sugar crystals to the centrifuge. The resulting product is a powder composed of agglomerates of microcrystalline sugar, having a residual moisture content of about 0.5%, which is too high to prevent clumping of the product during storage.
In the same way, other patents (GB 1 386 378, GB 1 386 379 and GB 1 387 062) describe atomisation processes for a syrup of saccharose on an added or
recycled powder support. The quantity of solid used is generally very high (> 50% of the dry material of the added syrup). These processes relate to a granulation / drying of powder with a syrup deposited by atomisation. This method generally leads to an increase in granulometry and a reduction in density. A crushing step is often required to maintain a stable density and granulometry during the whole of the production. Furthermore, all the described powders have a residual moisture greater than 0.1%, thus not permitting the saccharose powders to be stored without the risk of clumping.
In a process of preparation by compaction, which corresponds to a dry granulation, all the ingredients are dried and the resulting powdery composition is agglomerated under pressure, milled and sifted. Lubricants have to be added in order to avoid sticking problems. This is the process used notably for Nu-Tab® (Chr. Hansen).
In a process for preparation by micro crystallisation, the sugar solution is concentrated to a dry matter content of greater than 90%, and the resulting pasty mixture is cooled under mechanical beating. A crystallisation-agglomeration of the product enables a compressible powder to be manufactured. This is the process used notably for Dipac® (Domino).
Documents from the prior art do not describe a process enabling the production of a compressible saccharose powder with a residual water content that is appropriate for its conservation.
Consequently, a saccharose composition adapted for direct compression and sufficiently stable for conservation has never been described up to now.
SUMMARY OF THE INVENTION
The present invention describes a directly compressible saccharose powder without the use of any additives and a process for making the same.
OBJECTS OF THE INVENTION
Accordingly, the object of the present invention is to provide a powdery, compressible saccharose exempt from other added glucides, apart from those
naturally present in the saccharose, and exhibiting properties adapted to storage.
A further object of the present invention is to propose a process for the preparation of a compressible, powdery saccharose composition, which is suitable for industrial application.
DETAILED DESCRIPTION OF THE INVENTION
The present invention relates to a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules.
The term "powdery saccharose composition" means saccharose micro crystals agglomerated into particles that can be themselves agglomerated together. According to a preferred embodiment, the composition according to the invention consists of hollow spheres.
The term "compressible" means the ability of a powder to be formed into compressed tablets of a regular size, shape and weight in a compression machine.
A directly compressible sugar is a powdery sugar that only requires one mixing step for the various ingredients (aromas, colorants, active principles, lubricants...) prior to processing in a compression machine for manufacturing compressed tablets.
The powdery saccharose composition obtained according to the invention is directly compressible; thus it can be used for the preparation of compressed tablets. However, this characteristic of the composition does not limit in any way its utilisation in the manufacture of compressed tablets.
The residual moisture content can be measured by a Karl Fischer determination.
A residual moisture content greater than 0.1% is not appropriate for storage of the composition. In fact, with a content as high as this, the composition is not stable due to real risks of clumping.
According to a preferred embodiment, the compressible, powdery saccharose composition according to the invention does not contain binders, and in particular does not contain anti-crystallisation agents.
When required, the powdery composition according to the invention can also comprise aromas or colorants in amounts of less than 0.9% by weight based on the total weight of the composition.
Preferably, the sugar used is a sugar manufactured from or refined from cane sugar or beetroot, comprising when dry at least 99.1% by weight of saccharose determined by the polarimetric method.
The present invention relates to a powdery composition as defined above comprising at least 99.7% by weight of saccharose.
Preferably, the qualities sugar or white sugar, refined sugar or refined white sugar are used, which comprise a minimum of 99.7% saccharose and which moreover conform to the Directive EU nr. 2001/111 (OJEU 12 January 2002), in particular with an invert sugar content of less than or equal to 0.04% by weight.
It is also possible to use semi-white sugar, which comprises a minimum of 99.5% saccharose and which moreover conforms to the European Directive EU nr. 2001/111 (OJEU 12 January 2002) and all sugar containing, in the dry state, at least 99.1% saccharose and with an invert sugar content of less than or equal to 0.1%.
In all cases, the invert sugar, present in minor amounts, results from the manufacture or the refining of sugar and is not subsequently added by mixing; thus at this minor level it cannot act as an anti-crystallisation agent that enables the crystallisation of the saccharose to be controlled during drying, as defined in the international application WO 03/000936.
Maltodextrins, monosaccharides, oligosaccharides and polyols can be cited as other examples of anti-crystallisation agents.
Accordingly, none of the compounds that are naturally present apart from the 99.1% and particularly the 99.7% of saccharose are in sufficient quantity to play the role of anti-crystallisation agent, even if maltodextrins, monosaccharides, oligosaccharides and polyols are found among these compounds.
According to an advantageous embodiment, the powdery composition according to the invention does not comprise any added glucides other than the saccharose. Therefore, this composition does not comprise any other glucides than those present naturally in the utilised saccharose.
According to an advantageous embodiment, the powdery composition according to the invention comprises only saccharose resulting from the manufacture or refining of cane sugar or beetroot.
Furthermore, the impurities contained in the saccharose used in the context of the present invention cannot in general be considered as binders or as anti-crystallisation agents.
The present invention preferably relates to a powdery composition as defined above, comprising 100% by weight of saccharose.
The present invention also relates to a powdery composition as defined above, characterised in that the average granulometry or average opening of the hollow particles alone or agglomerated varies from about 140 to about 350 urn.
As the granulometric analyses are carried out by sieving, the average opening (AC)) corresponds to the mesh size that retains 50% by weight of the sample.
When the size of the particles is greater than 350 urn, then such a composition is no longer suitable for the manufacture of small size compressed tablets because of the difficulty associated with filling the die of the compression machine.
When the size of the particles is less than 140 µm, the flow properties of the powder are debased resulting in significant variations in the weight of the compressed tablets.
The present invention relates to a powdery composition as defined above, characterised in that the coefficient of variation of said particles varies from about 35 to about 55, especially from about 40 to about 50.
The term "coefficient of variation" denotes the level of dispersion about the average opening, i.e. the mesh size that retains 50% by weight of the sample. More precisely, the coefficient of variation is equal to the standard deviation of the distribution expressed as a percentage of the average opening.
These granulometric dispersion limits enable a compressible powder to be obtained that offers the best compromise in terms of powder flow and the fillability of the dies of the compression machine.
The present invention also relates to a powdery composition as defined above, characterised in that its bulk density is in the range of about 0.45 to about 0.75.
The term "bulk density" denotes the measured density of the powder; this is therefore the ratio of the mass of the powder to the volume occupied by the powder. This bulk density differs from the true density of the powder, which refers to the ratio of the mass of the powder to the volume totally filled by said powder without any volume of air. The degree of compaction of a powder is the relation between the density of the compressed tablet and the true density of the powder.
The tap density and the non-tapped bulk density are defined according to the method described by the European Pharmacopoeia (5th edition - Methods of pharmaceutical technology 2.9.15).
For evaluating the flow properties and the packing capacity of a powder, one can also measure the Carr's Index which allows the flowability of a powder to be evaluated and corresponds to the following ratio:
Carr's Index = 100 x tap density - bulk density tap density
Thus, the flowability and packing capacity of powders as a function of Carr's Index are shown in the Table below: (Table Removed)
In the context of the present invention, the Carr's Indeces of the powdery compositions obtained according to the invention are comprised between 8 and 17%.
A preferred powdery composition according to the present invention is a composition as defined above and exhibiting a flow time of less than about 15 seconds.
The flow is that defined according to the method described in the European Pharmacopoeia (5th edition - Methods of pharmaceutical technology 2.9.15).
According to an advantageous embodiment, the present invention relates to a powdery composition as defined above, characterised in that it exhibits a degree of crystallinity greater than or equal to 95%, especially greater than or equal to 99%.
The degree of crystallinity is determined by means of an X-ray diffraction measurement of the crystallinity of the powdery composition compared with the crystallinity of pure crystals of saccharose.
The powdery composition according to the invention is characterised in that it comprises substantially no vitreous or amorphous phase.
The present invention also relates to a powdery composition such as defined above, characterised in that it is able to be compressed, the strength of the compressed powder obtained from the powdery composition being greater than about 1 MPa, said strength being measured for a compression force greater than about 15 kN, and the compressed powder meeting an ejection force ranging between about 50 to about 80 N, said ejection force being measured for a compression force comprised between about 15 to about 20 kN.
The resistance of the obtained compressed tablets is measured according to the method described in the European Pharmacopoeia, chapter 2.9.8 (1997).
The compression mechanism used for compressing the sugar composition according to the invention is, for example a compression machine commercialised by the FROGERAIS Company, and equipped with two punches, only the upper punch being used for the compression. It should be noted that the strength measurement partially depends on the type of compression machine used; thus, if the lower and upper punches are used simultaneously for the compression then the strength of the resulting compressed tablets will be greater.
The ejection force is the force that has to be applied to the lower punch in order to free the compressed tablet.
The measured values on the powders according to the invention are indicated on the curves and compared on the same curves to the values obtained with the powder of the prior art (see Figures 2 and 3).
Description of the manufacturing process
The present invention also relates to a continuous process for manufacturing a compressible, powdery saccharose composition such as defined above and comprising:
a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being
comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose,
a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and
an optional cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition ranging from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
The term "nebulised saccharose solution" denotes the dispersion of a saccharose solution, particularly in the form of a syrup, into fine droplets by means of a nozzle or a centrifuge.
The term "atomisation tower" denotes the installation that enables a nebulised saccharose solution to be dried.
The term "drying step" denotes the dehydration step of the droplets of sugar syrup by hot air.
The term "glassy particles of saccharose" denotes the dehydrated but still not crystallised droplets of syrup.
A saccharose solution (input saccharose solution or initial saccharose solution), including in the form of syrup, is fed into an enclosure equipped with atomisation and drying means.
The first step of the process consists of a drying step of the saccharose solution, including in the form of a syrup in the form of droplets, nebulised by means of a nozzle or a centrifuge. Thus, this step consists in drying the drops of saccharose formed by nebulisation to solid particles with a hot air flow, whose entrance temperature into the atomisation tower (or drying chamber) varies from about 140 to about 180 °C. The hot air used for drying is recovered at the exit of the atomisation tower charged with humidity.
The term "stabilisation and crystallisation step" denotes the process of crystallisation of the glassy sugar particles on contacting the crystalline saccharose particles.
The expression "essentially crystallised powdery composition" denotes the still not cooled powdery saccharose composition.
The second step of the process consists in contacting the glassy particles resulting from the first drying step with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible powdery saccharose composition.
This second step notably enables the crystallisation of the saccharose to be initiated.
This step of contacting corresponds to a collision between the unstable glassy particles resulting from the first drying step with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible powdery saccharose composition. The composition obtained from this contacting step is essentially crystallised.
In fact, this two-step drying mode retards the crystallisation of the saccharose syrup by passing through an amorphous (or glassy) state. This initiation of the crystallisation, retarded by adding essentially crystallised saccharose and/or recycled compressible saccharose outside the nebulization/drying zone of the syrup, permits the formation of crystals of reduced size in each hollow particle. By adopting this processing mode, an arrangement of crystals is obtained, which is similar to that obtained, for example, by the process described in the
international application WO 03/000396, in which the addition of an anti-crystallisation agent is required.
In the following, the term "recycled powdery composition" denotes either a part of the recycled, essentially crystallised powdery composition, i.e. part of the powdery composition obtained prior to the cooling step in air (non-cooled composition), or part of the recycled, compressible powdery saccharose, i.e. part of the powdery composition obtained after drying in air (composition cooled at a temperature below 30 °C).
Consequently, the process of the invention is characterised by the use of a recycled powdery composition as defined above. Thus, a percentage of the recycled, essentially crystallised powdery composition or of the compressible powdery saccharose composition is removed in order to reuse it in the stabilisation and crystallisation step, and therefore to contact said recycled powdery composition with the abovementioned glassy particles.
The amount of recycle of the powdery composition or of the powder varies from 30 to 70% by weight of dry matter of the nebulised saccharose solution.
Of course it is possible to obtain the desired powdery composition by working with a higher recycle rate, particularly higher than 70%.
On the other hand, if the recycle rate is less than 30%, the number of collisions of the glassy particles with the recycled crystalline powder is insufficient, thereby causing a part of the powder to stick to the walls of the atomisation tower and limiting the industrial interest of the process.
According to a preferred embodiment, the preparation process of the invention is characterised in that the recycled powdery composition comes from the compressible powdery saccharose composition such as obtained at the end of the cooling step as defined above.
Accordingly, in this preferred embodiment, the recycled powdery composition used during the contacting with the glassy particles obtained at the end of the drying step, comes from the composition as obtained in the cooling step.
If the residual moisture content is greater than 1%, the resulting product is an unstable product that continues to lose water, and this water can condense onto any wall whose temperature is lower than that of the water. This phenomenon generally leads to clumping.
This characteristic is important because it affects the ability of the powder to remain powder/ and to retain its flowability. For a direct compression powder, this parameter directly influences the regularity of the weight and density of the compressed tablets. Thus, a powder that is too moist will contain agglomerates that will impede the facile filling of the dies of the compression machine and will lead to a rapid increase in the ejection forces of the compressed tablets and a premature fouling of the equipment.
The product obtained from the conclusion of the contacting step as defined above is a non-cooled and unstable product. Accordingly, for storage, it is advantageous, if not necessary, to subject the product to a cooling step. Without this cooling step, the product obtained is too sensitive to climatic changes and becomes rapidly unusable.
The compressible powdery saccharose composition according to the invention is obtained at the conclusion of the process.
The present invention also relates to a continuous process for manufacturing a compressible, powdery saccharose composition such as defined above and comprising:
a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose,
a contacting step of said glassy particles as obtained at the conclusion of the preceding step with a powder of saccharose crystals, said powder being present in a quantity corresponding to about 30 to about 70% by weight of dry matter of the nebulised saccharose solution, to obtain an essentially crystallised powdery composition at a temperature comprised between about
50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and
an optional cooling step in air of the essentially crystallised powdery composition to obtain the compressible powdery saccharose composition, said composition being crystallised and having a temperature of less than 30 °C.
According to a preferred embodiment, the powder of saccharose crystals is a recycled powder coming from either an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight, such as obtained at the conclusion of the contacting step as defined above, or from the compressible powdery saccharose composition such as obtained at the conclusion of the cooling step.
Preferably, the powder of saccharose crystals is a recycled powder coming from the compressible powdery saccharose composition such as obtained at the conclusion of the cooling step.
The process of the present invention is characterised in that it corresponds to a continuous process carried out after a start-up phase to obtain a steady state. Consequently, the granulometry does not increase and a powder exhibiting constant properties is obtained from this process.
Process start-up is carried out with saccharose powder from a previous production until the desired powdery composition is obtained.
For the first start-up of the process of the invention, a crystallisation initiator is used, i.e. an initial crystallisation initiator as the recycled powdery composition (or powder of saccharose crystals) such as defined above. An initiator of this type is a compound that serves to initiate the crystallisation during drying, as long as no powdery composition obtained according to the invention is available.
In particular, icing sugar or any other sugar crystal is used as the crystallisation initiator.
Once a sufficient quantity of the powdery composition has been obtained for use as the crystallisation initiator, i.e. as the recycled powdery composition (or powder of saccharose crystals) for the contacting step, then the icing sugar used as the crystallisation initiator is eliminated.
The present invention also relates to a continuous process for manufacturing a compressible, powdery saccharose composition such as defined above and comprising:
a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after the drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, and
a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said recycled, essentially crystallised powdery composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
This embodiment comprises the use of a part of the recycled, essentially crystallised powdery composition for the stabilisation and crystallisation step.
The present invention relates to a continuous process for manufacturing a compressible, powdery saccharose composition such as defined above and comprising the following steps:
a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose,
a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition
at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and
a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
This embodiment comprises three steps: the drying step, the stabilisation and crystallisation step (collision of the glassy particles with the recycled powdery composition) and the cooling step.
A specific embodiment of the process of the present invention comprises the use of both a part of the essentially crystallised powdery composition and a part of the compressible powdery composition as the recycled powdery composition.
The present invention also relates to a continuous process for manufacturing a compressible, powdery saccharose composition such as defined above and comprising the following steps:
a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose,
a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and
a cooling step in air of the essentially crystallised powdery composition to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
This embodiment comprises three steps: the drying step, the stabilisation and crystallisation step (collision of the glassy particles with the recycled powdery composition) and the cooling step. It is also characterised by the use of a part of the recycled, essentially crystallised powdery composition for the contacting step with the glassy particles.
The present invention also relates to a continuous process for manufacturing a compressible, powdery saccharose composition such as defined above and comprising the following steps:
a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose.
a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and
a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said compressible, powdery saccharose
composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
This embodiment comprises three steps: the drying step, the stabilisation and crystallisation step (collision of the glassy particles with the recycled powdery composition) and the cooling step. It is also characterised by the use of a part of the recycled, compressible powdery saccharose composition for the contacting step with the glassy particles.
The present invention also relates to a continuous process for the manufacture of a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than or equal to 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising:
a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose,
a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and
an optional cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition ranging from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.

The present invention also relates to the product as obtained by the process as defined above.
The present invention also relates to a continuous process for the manufacture of a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than or equal to 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising:
a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after the drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose, and
a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
The present invention also relates to the product as obtained by the process as defined above.
The present invention also relates to a continuous process for the manufacture of a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than or equal to 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising:
a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being
comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose,
a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and
a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
The present invention also relates to the product as obtained by the process as defined above.
The present invention also relates to a continuous process for the manufacture of a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than or equal to 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising:
a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose,
a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting
a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and
a cooling step in air of the essentially crystallised powdery composition to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
The present invention also relates to the product as obtained by the process as defined above.
The present invention also relates to a continuous process for the manufacture of a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than or equal to 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising:
a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose,
a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and
a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy
particles with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the saccharose solution.
The present invention also relates to the product as obtained by the process as defined above.
The present invention also relates to a continuous process for the manufacture of a compressible, powdery saccharose composition comprising at least 99.7% by weight of saccharose, exhibiting a residual moisture content of less than or equal to 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising:
a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air used for drying and exiting said tower being comprised between about 80 to 140 °C, for obtaining the glassy particles of saccharose,
a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and
a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
The present invention also relates to the product as obtained by the process as defined above.
According to a preferred embodiment, the process of the invention is characterised in that the drying step is carried out in the immediate vicinity of the nebulization zone, especially in the upper part of the atomisation tower.
The term "nebulisation zone" denotes the zone where the nebulisation step of the process is carried out, i.e. the zone where the drying step by hot air is carried out.
The term "upper part of an atomisation tower" denotes the nebulisation and drying zone of the sugar syrup.
The process of the invention is preferably characterised in that the contacting step is carried out in the atomisation tower, under conditions such that the recycled composition is added at the level of a zone comprised between the first third and the second third of said atomisation tower, and especially at the level of the middle zone of said atomisation tower.
According to yet another preferred embodiment, the contacting step is carried out outside the nebulisation and drying zone as described above.
The present invention also relates to a process as defined above, characterised in that the cooling step is carried out outside the atomisation tower.
According to an advantageous embodiment, the process of the invention is characterised in that the cooling step is carried out under conditions that enable the residual moisture content of the essentially crystallised powdery composition to be reduced and also the crystallisation of said composition to be terminated so as to obtain the compressible powdery crystallised saccharose composition.
Either a fluidised bed, a drum dryer or any other means to cool the powdery composition can be used for this cooling step.
The present invention also relates to a process as defined above, in which the initial saccharose solution has a dry matter content of about 55 to 80% by weight.
The dry matter content of a product corresponds to the percentage of dry extract of said product.
Moreover, as an illustrative and non-limiting example, the input flow of saccharose syrup to be nebulised varies from about some kg/h to about several thousands of kg/h, particularly from about 500 kg to about 2000 kg/h, depending on the size of the atomisation tower and its drying capacity.
The present invention relates to the use of a compressible powdery sugar composition as defined above, for the manufacture of compressed tablets, such as pharmaceuticals.
The present invention relates to the use of a compressible powdery sugar composition as defined above, for the manufacture of powdery mixtures.
The present invention relates to the use of a compressible powdery sugar composition as defined above, for the manufacture of fast-dissolving formulations.
The present invention also relates to the use of a compressible powdery sugar composition as defined above, in a mixture with at least one other product, said other product being in soluble or powdery form. Advantageously, said other product is an active principle, a sweetener, a colorant, an aroma, an enzyme or a surfactant.
According to an advantageous embodiment, the mixture obtained in this way, comprising the compressible powdery sugar composition as defined above and said other product, comprises 10% by weight at most of said other product based on the weight of the mixture.
The present invention also relates to the use of a compressible powdery sugar composition as defined above, for the manufacture of sugar spheres, such as by coating and/or lamination and/or sugar coating.
The sugar spheres are spherical or quasi-spherical particles constituted by a saccharose core, onto which can be deposited successive layers of glucides and/or colloids and/or waxes or fats. The size of the resulting particles can vary from some tens of micrometres to some millimetres.
Considering the shape of the particles and their surface characteristics (Figures 4A and 4B), the compressible powdery sugar composition according to the invention is perfectly adapted for the manufacture of sugar spheres. In fact, with an almost spherical shape, the powder obtained by atomisation enables spheres to be very easily formed by lamination, coating or sugar coating. Due to its surface characteristics, this powder permits the deposition of both hydrophilic (glucides, colloids, etc..) as well as hydrophobic substances (oils, waxes etc.).
DESCRIPTION OF THE ACCOMPANYING DRAWINGS
Figure 1 represents a general scheme of the process of the invention.
The arrow 1 indicates the introduction of the saccharose syrup into the atomisation tower (A). The drying air (2) is introduced into the drying zone (4) and the moist air (3) is recovered at a temperature of between 80 and 140 °C. Zone (5) corresponds to the zone of the atomisation tower where the stabilisation and crystallisation step takes place.
A part of the essentially crystallised powdery composition obtained from this stabilisation and crystallisation step can be recycled and reintroduced (6) for example into the atomisation tower (A). The essentially crystallised powdery composition is subjected to a cooling step (7) to obtain a cooled compressible powdery composition (9). A part of this cooled compressible powdery composition can likewise be recycled and reintroduced (8) into the atomisation tower (A), it being understood that the process of the invention necessarily comprises recycling of the powdery composition, i.e. either step (6) or step (8).
Figure 2 represents the comparative graphs of the crushing strength (in MPa) of the compressed tablets obtained from pilot plant experiments as a function of the compression force (in kN). The curve with the black squares refer to the sugar Dipac; the curve with the black triangles refer to the powdery composition of example 1; the curve with the black lozenges refers to the powdery composition of example 2 and the curve with the black circles refers to the powdery composition of example 3. An examination of the graphs of Figure 2 reveals that the powdery compositions from examples 1 to 3 according to the
invention exhibit higher strengths for a given compression force than the reference commercial product (Dipac).
Figure 3 represents the comparative graphs of the ejection force (in N) supported by the obtained compressed tablets as a function of the compression force (in kN). The curve with the black squares refer to the sugar Dipac; the curve with the black triangles refer to the powdery composition of example 1; the curve with the black lozenges refers to the powdery composition of example 2 and the curve with the black circles refers to the powdery composition of example 3.
The graphs of Figure 3 demonstrate that the results obtained with the compressible saccharose powders of the invention are comparable with those obtained for the commercial product Dipac® in terms of ejection force for a given compressive force.
The graphs of Figures 2 and 3 should be analysed in conjunction because the ejection force supported by a compressed tablet without risk of breakage cannot be disassociated from the strength of the compressed tablet. Thus, the compressed tablets obtained and made up from powdery saccharose compositions according to the invention exhibit the strength/ejection force relationships comparable to those obtained from the commercial product Dipac®.
Figures 4A and 4B represent scanning electronic microscopy images of the directly compressible powdery composition.
Figure 4A shows that the powdery composition obtained is composed of isolated hollow particles or associated particles that form granules.
Figure 4B represents in detail a hollow particle of about 200 urn, made up of agglomerated micro crystals and associated with other particles of variable dimensions.
EXAMPLES
Example 1
A saccharose solution (65% dry matter) was nebulised at 102 bars in a drying chamber under a hot air flow. The temperature of the drying air was adjusted as a function of the required exit temperature of the moist air. The powder exiting the drying chamber was cooled and partially recycled (recycle rate was 40 % based on the dry matter of the syrup feed) towards the lower part of the chamber, outside the nebulisation zone of the solution.
Operating parameters: Entrance
(Table Removed)
Properties of the dried powder (Table Removed)
Example 2
A saccharose solution (65% dry matter) was nebulised at 210 bars in a drying chamber under a hot air flow. The temperature of the drying air was adjusted as a function of the required exit temperature of the moist air. The powder exiting the drying chamber was cooled and partially recycled (recycle rate was 40% based on the dry matter of the syrup feed) towards the lower part of the chamber, outside the nebulisation zone of the solution.
Operating parameters:
Entrance (Table Removed) Exit
Properties of the dried powder (Table Removed)
The powdery saccharose composition obtained according to the invention performs as well as an obtained powder formulated with binders (see Figures 2 and 3).
Example 3
A saccharose solution (55% dry matter) was nebulised at 210 bars in a drying chamber under a hot air flow. The temperature of the drying air was adjusted as a function of the required exit temperature of the moist air. The powder exiting the drying chamber and not cooled was partially recycled (recycle rate was 35% based on the dry matter of the syrup feed) towards the lower part of the chamber, outside the nebulisation zone of the solution.
Operating parameters:
Entrance (Table Removed)
Properties of the dried powder
The powdery saccharose composition obtained according to the invention performs as well as an obtained powder formulated with binders (see Figures 2 and 3).
Recycling the essentially crystallised powder enabled a product to be obtained that was absolutely comparable with the products obtained according to examples 1 and 2.
Composition and procedure for obtaining compressed tablets
The compressed tablets were obtained from an alternating machine Frogerais OA equipped with compression chamber having an 11.28 mm section. The machine speed was 3350 cps/hour.
Prior to the compression step, the powdery compositions were mixed with 0.5 (Dipac) or 0.75% (atomised powders according to the invention) magnesium stearate for 5 minutes in a mixer with a three-dimensional random action. The round and flat compressed tablets were prepared with compression forces of 10, 20 and 30 kN.
Example 4
In this example, a colorant was chosen to simulate an ingredient (active principle, aroma, enzyme, surfactants etc....). The colorant of chosen granulometry was mixed with the sugar dried by atomisation (composition of the invention). The homogeneity of the mixture was evaluated as a function of the mixing time, the addition level and the size of the colorant particles. Due to its morphology and its surface characteristics, the sugar dried by atomisation enabled perfectly homogeneous mixtures to be obtained. In fact, even with a blade mixer, the mixtures obtained under the above-described conditions have a homogeneous distribution with a standard deviation of always less than 2% (average of 10 samples).
Homogeneity of the mixture as a function of mixing time
(Table Removed) Homogeneity of the mixture as a function of additive content

(Table Removed)
Homogeneity of the mixture as a function of particle size of the colorant
(Table Removed)
According to these results, it can be observed that all the mixtures obtained were homogeneous mixtures because no subsequent demixing was observed (stable mixture).
Method for analysing the colorant
The colorant in the mixture was analysed by measuring the absorbance in a UV/visible spectrometer UNICAM UV4 at a wavelength of 500 nm with a 10 mm long cell. The percentage of colorant was calculated from measurements carried out on standard solutions.
'

We claim:
1. Compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules.
2. Powdery composition according to claim 1, comprising at least 99.7% by weight of saccharose.
3. Powdery composition according to claim 1 or 2, characterised in that the average granulometric distribution of the hollow or agglomerated particles varies from about 140 to about 350 urn.
4. Powdery composition according to claim 3, characterised in that the
coefficient of variation of said particles varies from about 35 to about 55,
particularly from about 40 to about 50.
5. Powdery composition according to any one of claims 1 to 4, characterised in that its bulk density is in the range of about 0.45 to about 0.75.
6. Powdery composition according to any one of claims 1 to 5, characterised in that its flow time is less than about 15 seconds.
7. Powdery composition according to any one of claims 1 to 6, characterised in that it is able to be compressed, the strength of the compressed powder obtained from the powdery composition being greater than about 1 MPa, said strength being measured for a compression force greater than about 15 kN, and the compressed powder meeting an ejection force comprised between about 50 to about 80 N, said ejection force being measured for a compression force comprised between about 15 to about 20 kN.
8. Continuous process for manufacturing a compressible, powdery saccharose composition such as defined in any one of claims 1 to 7, comprising:
- a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being

comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose,
- a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of the composition, and
- an optional cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition ranging from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
9. Continuous process for manufacturing a compressible, powdery saccharose composition such as defined in any one of claims 1 to 7, comprising:
- a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after the drying and exiting said tower being comprised between about 80°C to 140 °C, for obtaining the glassy particles of saccharose, and
- a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30% to about 70% by weight of dry matter of the nebulised saccharose solution.

10. Continuous process for manufacturing a compressible, powdery
saccharose composition such as defined in any one of claims 1 to 7,
comprising the following steps:
- a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air used for drying and exiting said tower being comprised between about 80°C to 140 °C, for obtaining the glassy particles of saccharose,
- a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and
- a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
11. Continuous process for manufacturing a compressible, powdery
saccharose composition such as defined in any one of claims 1 to 7,
comprising the following steps:
- a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose,
- a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a

residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and
- a cooling step in air of the essentially crystallised powdery composition to
obtain the compressible, powdery saccharose composition, said composition
being crystallised and being at a temperature of less than 30 °C, said
stabilisation and crystallisation step being carried out by contacting said glassy
particles with part of the recycled, essentially crystallised powdery composition,
the amount of recycle of said essentially crystallised powdery composition
varying from about 30 to about 70% by weight of dry matter of the nebulised
saccharose solution.
12. Continuous process for manufacturing a compressible, powdery saccharose composition such as defined in any one of claims 1 to 7, comprising the following steps:
- a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose,
- a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and
- a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.

13. Process according to any one of claims 8 to 12, wherein the drying step is carried out in the immediate vicinity of the nebulisation zone, especially in the upper part of the atomisation tower.
14. Process according to any one of claims 8 to 13, wherein the contacting step is carried out in the atomisation tower, under conditions such that the recycled composition is added at the level of a zone comprised between the first third and the second third of said atomisation tower, and especially at the level of the middle zone of said atomisation tower.
15. Process according to any one of claims 8 to 14, characterised in that the cooling step is carried out outside the atomisation tower.
16. Process according to any one of claims 8 to 15, characterised in that the cooling step is carried out under conditions enabling the residual moisture content of the essentially crystallised powdery composition to be reduced and also the crystallisation of said composition to be completed in order to obtain the compressible, powdery, crystallised saccharose composition.
17. Process according to any one of claims 8 to 16, wherein the initial
saccharose solution has a dry matter content of about 55 to 80% by weight.
18. Continuous process for manufacturing a compressible, powdery
saccharose composition comprising at least 99.1% by weight of saccharose,
exhibiting a residual moisture content of less than 0.1% by weight, based on
the total weight of said composition, said composition consisting of hollow
particles, optionally agglomerated together in the form of granules, said
process comprising:
- a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose,
- a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a

residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and
- an optional cooling step in air of the essentially crystallised powdery
composition, to obtain the compressible, powdery saccharose composition,
said composition being crystallised and being at a temperature of less than
30°C, said stabilisation and crystallisation step being carried out by contacting
said glassy particles with part of the recycled, essentially crystallised powdery
composition or with part of the recycled, compressible, powdery saccharose
composition, the amount of recycle of said essentially crystallised powdery
composition or of the compressible, powdery saccharose composition ranging
from about 30 to about 70% by weight of dry matter of the nebulised
saccharose solution.
19. Continuous process for manufacturing a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising:
- a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after the drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose, and
- a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised, powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30% to about 70% by weight of dry matter of the nebulised saccharose solution.

20. Continuous process for manufacturing a compressible, powdery
saccharose composition comprising at least 99.1% by weight of saccharose,
exhibiting a residual moisture content of less than 0.1% by weight, based on
the total weight of said composition, said composition consisting of hollow
particles, optionally agglomerated together in the form of granules, said
process comprising:
- a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose,
- a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and
- an cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
21. Continuous process for manufacturing a compressible, powdery
saccharose composition comprising at least 99.1% by weight of saccharose,
exhibiting a residual moisture content of less than 0.1% by weight, based on
the total weight of said composition, said composition consisting of hollow
particles, optionally agglomerated together in the form of granules, said
process comprising:
- a drying step, by air, of a nebulised saccharose solution in an atomisation
tower, the temperature of the air after drying and exiting said tower being

comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose,
- a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and
- a cooling step in air of the essentially crystallised powdery composition to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30°C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition, the amount of recycle of said essentially crystallised powdery composition varying from about 30 to about 70% by weight of dry matter of the nebulised saccharose solution.
22. Continuous process for manufacturing a compressible, powdery saccharose composition comprising at least 99.1% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising:
- a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air after drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose,
- a stabilisation and crystallisation step of the glassy particles obtained from the drying step to obtain an essentially crystallised powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and

- a cooling step in air of the essentially crystallised powdery composition, to
obtain the compressible, powdery saccharose composition, said composition
being crystallised and being at a temperature of less than 30 °C, said
stabilisation and crystallisation step being carried out by contacting said glassy
particles with part of the recycled, compressible, powdery composition, the
amount of recycle of said compressible, powdery saccharose composition
varying from about 30 to about 70% by weight of dry matter of the nebulised
saccharose solution.
23. Continuous process for manufacturing a compressible, powdery saccharose composition comprising 100% by weight of saccharose, exhibiting a residual moisture content of less than 0.1% by weight, based on the total weight of said composition, said composition consisting of hollow particles, optionally agglomerated together in the form of granules, said process comprising:
- a drying step, by air, of a nebulised saccharose solution in an atomisation tower, the temperature of the air used for drying and exiting said tower being comprised between about 80 °C to 140 °C, for obtaining the glassy particles of saccharose,
- a stabilisation and crystallisation step of the glassy particles obtained from the drying step, to obtain an essentially crystallised, powdery composition at a temperature comprised between about 50 °C to about 80 °C and exhibiting a residual moisture content of less than or equal to 1% by weight based on the total weight of said composition, and
- a cooling step in air of the essentially crystallised powdery composition, to obtain the compressible, powdery saccharose composition, said composition being crystallised and being at a temperature of less than 30 °C, said stabilisation and crystallisation step being carried out by contacting said glassy particles with part of the recycled, essentially crystallised powdery composition or with part of the recycled, compressible, powdery saccharose composition, the amount of recycle of said essentially crystallised powdery composition or of the compressible, powdery saccharose composition varying from about 30% to about 70% by weight of dry matter of the nebulised saccharose solution.

24. Compressible, powdery sugar composition such as obtained by the process according to one of claims 18 to 23.
25. Use of a compressible, powdery sugar composition according to one of claims 1 to 7 or 24, for manufacturing compressed tablets, such as pharmaceuticals.
26. Use of a compressible, powdery sugar composition according to one of claims 1 to 7 or 24, for manufacturing powdery mixtures.
27. Use of a compressible, powdery sugar composition according to one of claims 1 to 7 or 24, for manufacturing fast-dissolving formulations.
28. Use of a compressible powdery sugar composition according to one of claims 1 to 7 or 24, in a mixture with at least one other product, said other product being in soluble or powdery form, and being selected from among the following products: active principle, sweetener, colorant, aroma, enzyme or surfactant.
29. Use of a compressible, powdery sugar composition according to one of claims 1 to 7 or 24, for manufacturing sugar spheres, especially by coating and/or lamination and/or sugar coating.

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Patent Number

270049

Indian Patent Application Number

4286/DELNP/2008

PG Journal Number

48/2015

Publication Date

27-Nov-2015

Grant Date

26-Nov-2015

Date of Filing

21-May-2008

Name of Patentee

TEREOS

Applicant Address

11, RUE PASTEUR F-02390 ORIGNY SAINTE BENOITE FRANCE

Inventors:

#	Inventor's Name	Inventor's Address
1	WONG, EMILE	LES ANCIENNES ECURIES, RUE DE SAINT-DIDIER F-01700 NEYRON FRANCE
2	DELHORBE, PHILIPPE	35, RUE PHILIPPE DE GIRARD F-59139 WATTIGNIES FRANCE

PCT International Classification Number

C13F 3/00

PCT International Application Number

PCT/FR2006/002393

PCT International Filing date

2006-10-25

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1	N 05/11070	2005-10-28	France