Indian Patents. 260416:A PROCESS FOR PREPARING A DETERGENT

Title of Invention	A PROCESS FOR PREPARING A DETERGENT
Abstract	The invention relates to a process for preparing a detergent including methyl ester sulphonate comprising micronizing the methyl ester sulphonate; dispersing the micronized methyl ester sulphonate in a dispersing agent and spraying the dispersion on the detergent constituents.

Full Text	FORM 2 THE PATENTS ACT, 1970 (39 of 1970) & THE PATENTS RULES, 2003 COMPLETE SPECIFICATION (See section 10, rule 13) 1. Title of the invention "A DETERGENT COMPOSITION AND A PROCESS FOR PREPARING THE SAME" 2. Applicant(s) Name Nationality Address TATA CHEMICALS LTD. INDIA BOMBAY HOUSE, 24 HOMI MODI STREET MUMBAl - 400001 3. Preamble to the description COMPLETE SPECIFICATION The following specification particularly describes the invention and the manner in which it is to be performed. The disclosure relates to a detergent. More particularly, the invention relates to a detergent composition including methyl ester sulphonate and a method of manufacturing the same. DESCRIPTION OF RELATED ART Conventional dry mix detergent product formulations are based on synthetic soda ash. Dry detergent compositions are formed by mixing soda ash with one or more surfactants. In addition to soda ash arid surfactants, other additives such as builders, brighteners, soil release agents, perfumes etc are also added to detergents. However, since soda ash has to be manufactured, the cost of manufacturing soda ash adds to the cost of the detergent. There have been attempts to use methyl ester sulphonate as an active detergent. As methyl ester sulphonate is easily obtainable from renewable sources such as natural oil or fats and due to its biodegradable nature, it may be preferable over other surfactants conventionally used in detergent formulations. Furthermore, the use of certain commercial grades of methyl ester sulphonate as active detergent may result in a considerably low price detergent formulation. However, methyl ester sulphonate present in conventional detergent formulations hydrolyzes in the presence of moisture and high pH detergent components including builders such as carbonates, an9.0) results in poor detergency performance and reduced application flexibility. Moreover, as methyl ester sulphonate tends to form lumps it cannot be effectively niixed with the other detergent constituents and thus, addition of methyl ester sulphonate as such in the detergent deteriorates the free flowing nature of the detergent. In view of the above, there is a need to formulate a detergent composition enabling effective and maximum utilization of methyl ester sulphonate as an active detergent. Moreover, the detergent should be free flow and have good lather and foam generation property, improved detergency performance and should be cost effective. 2 SUMMARY The invention relates to a process for preparing a detergent including methyl ester sulphonate comprising micronizing the methyl ester sulphonate; dispersing the micronized methyl ester sulphonate in a dispersing agent and spraying the dispersion on the detergent constituents. The invention also relates to a process for preparing a detergent including methyl ester sulphonate comprising micronizing the methyl ester sulphonate, micronization of methyl ester sulphonate including addition of a flow aid to the methyl ester sulphonate; dispersing the micronized methyl ester sulphonate in a dispersing agent and spraying the dispersion on the detergent constituents, the detergent constituents including a source of bicarbonate. The invention further relates to a process for manufacturing a detergent comprising micronizing the methyl ester sulphonate; adding the micronized methyl ester sulphonate in a dispersing agent to obtain a dispersion and spraying the dispersion on the detergent constituents, the detergent constituents including beneficiated crushed refined soda fmes obtained by drying and reducing the size of the crushed refined soda fines to below 500 micron while retaining its bicarbonate content. BRIEF DESCRIPTION OF ACCOMPANYING DRAWINGS The accompanying drawings illustrate the preferred embodiments of the invention and together with the following detailed description serve to explain the principles of the invention. Figure 1 tabulates comparative particle size distribution data of methyl ester sulphonate, micronized methyl ester sulphonate and micronized methyl ester sulphonate along with a flow aid. Figure 2 tabulates the ratio of methyl ester sulphonate to sulphonic acid in accordance with an embodiment. Figure 3 tabulates comparative detergency of methyl ester sulphonate, milled methyl ester sulphonate and linear alkyl benzene sulphonic acid (non dispersion), a dispersion of milled methyl ester sulphonate and linear alkyl benzene sulphonic acid in accordance with an aspect. Figure 4 tabulates the composition of beneficiated crushed refined soda ash fines developed for detergent formulation in accordance with an aspect of the invention in comparison with synthetic soda ash. 3 Figure 5 tabulates the results of analysis of pH and percent methyl ester sulphonate in detergent formulations 1, 2 and 3 in accordance with embodiments of the invention in comparison with a control detergent formulation. Figure 6 tabulates detergent formulations in accordance with embodiments in comparison with soda ash control formulations. Figure 7 tabulates the results of tests carried out on samples of detergent formulations in accordance with embodiments of the invention in comparison with soda ash control formulations. Figure 8 tabulates the result of detergency test carried out on samples of detergent formulations with enzymes in accordance with an embodiment against soda ash control formulations. Figure 9 schematic illustration of the method of manufacturing a detergent and preparation of detergent in accordance with an embodiment of the invention. DETAILED DESCRIPTION To promote an understanding of the principles of the invention, reference will be made to the embodiment and specific language will be used to describe the same. It will nevertheless be understood that no limitation on scope of the invention is thereby intended, such alterations and further modifications in the described composition and such further applications of the principles of the inventions as disclosed therein being contemplated as would normally occur to one skilled in art to which the invention relates. A detergent composition using methyl ester sulphonate is described. More particularly, a detergent composition using micronized methyl ester sulphonate is described. The invention further relates to a detergent composition comprising crushed refined soda fines, the crushed refined soda fines are typically obtained from the effluent generated from a soda ash production plant using trona soda as raw material. In accordance with an aspect, the micronized methyl ester sulphonate as used in the detergent includes a flow aid. In accordance with an aspect, the detergent may further comprise a dispersing agent and other constituents including but not limited to salt, secondary surfactant, optical brightener, 4 colour, anti caking agent, fragrance, anti redeposition agent, speckles, enzymes, builders or the like. In accordance with an embodiment, the detergent composition comprises micronized methyl ester sulphonate including a flow aid, a dispersing agent and at least one bicarbonate source. In accordance with an embodiment, the detergent composition comprises micronized methyl ester sulphonate including a flow aid, a dispersing agent and crushed refined soda fines. In accordance with an alternative embodiment, the detergent comprises micronized methyl ester sulphonate including a flow aid, a dispersing agent, at least one enzyme and crushed refined soda fines. In accordance with an embodiment, the detergent comprises micronized methyl ester sulphonate including a flow aid, a dispersing agent, at least one enzyme, a salt, a secondary surfactant, an optical brightener, a colour or dye, an anti caking agent, fragrance, an anti redeposition agent, speckles, a builder and crushed refined soda fines. A process for preparing a detergent containing methyl ester sulphonate is also described. A process for preparing a detergent, in accordance with the invention, involves micronization of methyl ester sulphonate, mixing the micronized methyl ester sulphonate with a dispersing agent and adding the dispersion so obtained to other detergent constituents. In accordance with an aspect, the micronization of methyl ester sulphonate includes the addition of a flow aid. In accordance with an aspect, the process for preparing a detergent includes the addition of a bicarbonate source to the detergent. In accordance with an aspect, methyl ester sulphonate used in the present formulation is an alpha-sulpho fatty acid ester, which is generally of the following formula (I): RCHCOOCH3 (I) SO3M+ wherein R is an alkyl chain having 4 to 24 carbon atoms, preferably 12 to 18 carbon atoms, and M+ is a monovalent or divalent alkali metal. For example, R is a C8, C10, C12, CM, C16 or C18 alkane and M is typically an alkali metal, such as sodium or potassium. In accordance with an 5 aspect, methyl ester sulphonate is a sodium methyl ester sulphonate, such as a sodium C8 to C18 methyl ester sulphonate. In one embodiment, the methyl ester sulphonate is a C8, C10, C12 CI4, C16 or C18 methyl ester sulphonate. In another embodiment the mefhy) ester sulphonsle comprises a mixture of different chain length Methyl ester sulphonate esters such as a mixture of C8, Ci0, Cl2, C14, Cl6 and/or C18 methyl estet- sulphonate. Such a mixture of methyl ester sulphonate can be prepared from a natural fat or oil, or synthetic fatty alcohols. In alternative embodiment, methyl ester sulphonate is a mixture of methyl ester sulphonates having different chain lengths. Suitable mixtures of such methyl ester sulphonate include about C8, Cl0, C12 and/or CM methyl ester sulphonate combined with C16 and/or C18 methyl ester sulphonate m ratios from about 1: 99 to about 99: 1. In another embodiment, the mixture comprises about 1 to 99 weight % of C16 methyl ester sulphonate and about 99 to about 1 weight % of C18 methyl ester sulphonate. Methyl ester sulphonate can be prepared from a variety of sources including beef tallow, palm kernel oil, palm kaernel (olein) oil, palm kernel (stearin) oil, coconut oil, soybean oil, canola oil, caster oil, Cohume oil, coco butter, linseed oil, palm oil, white grease, cotton seed oil, corn oil, rape seed oil, yellow grease or mixtures thereof. Suitable fatty acids to make methyl ester sulphonates include but not limited to, caprylic (C8), capric (C10), lauric (C12), myristic (C 14), myrisloleic (CM), Palmitic (C16), palmitoleic (C16), stearic (C18), oleic (C18), linoleic (C 18), linolenic (C18), ricinoleic (C18), arachidic (C20), gadolic (C20), behenic (C22) and erucic (C 22) fatty acids. In accordance with an aspect, the detergent comprises about 2 to 8 weight %, preferably 4 to 6 weight % of methyl ester sulphonate. In accordance with an aspect, a flow aid is added to methyl ester sulphonate. The flow aid is added to improve the granularity of the product, for example by preventing aggregation and/or caking of the granules. In addition, detergent formulation comprising flow aid exhibits higher solubility and cleaning performance. Suitable flow aid according to the present invention includes, but not limited to crystalline or amorphous alkali metal silicates, aluminosilicates including zeolites, citrates, dicamol, calcite, diatomaceous earths, talc or silica. In accordance with a preferred embodiment, the flow aid is precipitated silica. 6 The cleaning performance (% detergency) of deterget incliding methyl ester sulphonate as commercially available in the formulation has been found to be very low. The experimental results showed that the cleaning performance (% detergency) 0f detergent formulation including methyl ester sulphonate as such was 18.50 only. In accordance with an aspect, the methyl ester sulphonate is micronized prior mixing it with other detergent constituents. The micronized methyl ester sulphonate is not completely free flow and forrns small jumps, jn accordance with an aspect, methyl ester sulphonate is micronised with addition of flow aid such as precipitated silica. In accordance with an aspect, addition of about 0.25 t0 2.0 weight % precipitated silica during micronization of methyl ester sulphonate is required so as top obtain free flow micronized methyl ester sulphonate. By way of specific example, 100 gm of memyi ester sulphonate is micronized along with 0.50 gm of precipitated silica. With referance t0 Figure 1, the particle size distribution of micronized methyl ester sulphonate along with the flow aid in comparison with imliomixtf'irrctlry os'il'r ttfomat wilhrtufauidiliflr oifa" ifl%. agrfme&yi ester safafioctaCe is illustrated. In accordance with an aspect, the detergent composition mrther comprises a dispersing agent. The dispersing agent is used to suspend solid particles ind to prevent settling thereof so as to obtain a suspension capable of mixing effectively with other detergent constituents. In accordance with an embodiment, the dispersing agent may by a non--surface active polymer. In accordance with an alternative embodiment, the dispersing agent may be a surfactant. In accordance with a preferred embodiment, the dispersing agent is linear alkyl benzene sulfonic acid. The detergent composition, in accordance with an aspect contains 8 to 15 weight % of a dispersing agent, preferably 8 to 10 weight % of dispersing agent. By way of specific example, micronized methyl ester sulphonate including precipitated silica is mixed with linear alkyl benzene sulfonic acid so as to obtain a dispersion thereof with reference to Figure 2, ratio of micronized methyl ester sulphonate to linear alkyl benzene sulfonic acid in accordance with an aspect is illustrated. By way of specific example, ratio of micronized methlythyl ester sulphonate to linear alkyl benzene sulfonic acid is 2:3. Experimental results showed that mixing of the methly ester sulphonate dispersion so prepared with other detergent constituents substantially enhanced the performance of the detergent. With reference to Figure 3, the cleaning performance (o/0 detergency) of detergent 7 including methyl ester sulphonate dispersion in comparison with detergents including methyl ester sulphonate, and milled methyl ester sulphonate and linear alkyl benzene sulfonic acid (non-dispersion) is illustrated. In accordance with an embodiment, the cleaning performance (% detergency) of the detergent composition including methyl ester sulphonate dispersion is 56. In accordance with an aspect, the detergent comprises a bicarbonate source. In accordance with an embodiment, the bicarbonate source is crushed refined soda fines. The crushed refined soda fines are wastes that are generated from a soda ash plant using trona soda for the production of soda ash. The effluent that comes out from the overflow of washery of a soda ash plant is known as crushed refined soda fines slurry. The liquid is drained out to leave crushed refined soda fines that become dry by sunlight. In accordance with an aspect the crushed refined soda fines is treated and purified before it is used in a detergent formulation. The crushed refined soda fines are beneficiated by the sieving the raw crushed refined soda fines to obtain crushed refined soda fines having a particle size distribution of 2 mm or less, drying the crushed refined soda fines to reduce the moisture content, and reducing the particle size of the crushed refined soda fines to below 500 microns. In accordance with an aspect, the crushed refined soda fines must be dried in a manner that does not substantially deplete the sodium bicarbonate content. With reference to Figure 4, the composition of beneficiated crushed refined soda fines in comparison with synthetic soda ash is illustrated. The crushed refined soda fines may be added as a part or complete substitute for the soda ash. In accordance with an embodiment, crushed refined soda fines are added as a complete substitute for soda ash. In accordance with an aspect, the detergent composition contains 25 to 40 weight % of crushed refined soda fines and preferably the detergent composition contains about 30 weight % of crushed refined soda fines. Crushed refined soda fines included in the detergent formulation may act as a bicarbonate source so as to control the pH of the detergent formulation at higher range (> pH 9) and to stabilize methyl ester sulphonate, which is prone to degradation at higher pH. In the detergent formulation, generation of hydroxyl ions occurs due to dissolution of alkaline salts in water and these ions may affect the effectiveness of methyl ester sulphonate. The bicarbonate present in the detergent formulation provides a buffering effect. The bicarbonate ions react with hydroxyl ion 8 (generated from salt hydrolysis) to form carbonate ion and water (II). This allows methyl ester sulphonate to be effective even at higher pH levels. HCXV + OH" = C03= + H20 (II) A higher pH detergent has better cleaning performance. However, addition of bicarbonate lowers the pH of the detergent, as seen in the experimental results tabulated in Figure 5. Detergent compositions 1, 2 and 3 having different concentrations of bicarbonate are developed in accordance with embodiments of the invention. A control composition without any bicarbonate is also prepared and compared with the compositions 1, 2 and 3. The amount of bicarbonate added to the composition is important, as excess bicarbonate tends to lower the pH in a manner that negates the advantage of addition of the bicarbonate. As indicated in Figure 5, the composition 3 containing 1.6 weight % of bicarbonate, showed the highest amount of methyl ester sulphonate (10.65 %) available in the composition at higher pH (pH 10.86). In accordance with an aspect the detergent composition may contain salt. In accordance with an aspect, the detergent composition contains 15 to 35 weight % of the salt and preferably the detergent composition contains 20.4 to 32.4 weight % of salt. Any suitable soluble salt may be added to the detergent composition. In accordance with an embodiment, the detergent composition may contain sodium chloride as salt. Sodium chloride helps in removing bloodstains in the garment and helps to retain color. In accordance with an aspect, the detergent composition may contain builder. Builders may comprise of organic or inorganic compounds. Builders added to the detergent composition help in dispersion and suspension of particulate matters, maintenance of an alkaline environment required for efficient cleaning, emulsification of organic oils and fats, softening of water, prevention of redeposition of soil and inhibition of corrosion of metals in processing and washing equipments. Suitable builders for the detergent formulation according to the present invention include, but not limited to, silicate containing builders such as polysilicates, alkali metal silicates, wholly or partially crystallite layer-form silicate, phyllosilicates or disilicates, silicated salt i.e. a salt such as a carbonate, sulphate, alkali metal carbonate, alkali metal sulphate, ammonium carbonate, bicarbonate, sesquicarbonate or mixture thereof, that has been treated with a silicate salt; aluminosilicate containing builders such as zeolites; and phosphate containing builders such as alkali metal phosphates, orthophosphates, polyphosphates, triopolyphophate, 9 pyropolyphosphate, or polymer phosphates; carbonate builders such as soda ash; oxygen releasing builders such as sodium perborate, sodium percarbonate. These builders may be used alone or in combination. In accordance with an embodiment, sodium tripolyphosphates may be used as a builder. In accordance with alternative embodiment, sodium silicate may be used as a builder. In accordance with a preferred embodiment, the detergent composition comprises sodium silicate having a ratio of Si02 toNa20 substantially in the range of 3.0 to about 3.10. In accordance with an embodiment, the detergent composition may contain 2 to 4 weight %, preferably 3 weight % of builder. In accordance with an alternative embodiment, the the detergent composition may contain 6 to 8 weight %, preferably 7 weight % of builder. In accordance with an aspect, the detergent composition may comprise a secondary surfactant. The secondary surfactant is added to the detergent formulation as a supplement to methyl ester sulphonate in respect of lather and foam generation. Any cationic, anionic or neutral surfactant may be added to the detergent composition as secondary surfactant including bat not limited to long-chain amino condensates with ethylene oxide and quaternary ammonium compounds, alpha olefin sulphonate, alkyl aryl sulphonic acids, alkyl sulphonic acids, salts of alkyl sulfuric acids, fatty acid derivatives and polyethylelene oxide ether condensates of alkylphenols, ethoxylated aliphatic alcohols, carboxylic esters 0r any combination thereof. The surfactants may be used alone or in combination with on.e another. In accordance with a preferred embodiment, the secondary surfactant is sodium lauryl sulphate. In accordance with an alternative embodiment, a mixture of linear alkyl benzene sulphonic acid and sodium salt of sulphonic acid may be used as a secondary surfactant. In accordance with an embodiment, the detergent composition may contain I to 3 weight %, preferably 2 weight % of secondary surfactant. In accordance with an alternative embodiment, the detergent composition may contain 3 to 5 weight %, preferably 4 weight % of secondary surfactant. In accordance with an aspect, optical brightener may be added to the detergent composition. Optical brighteners that may be added to the detergent include but are not limited to naphthotriazolylstilbenes, benzoxazolyl, benzimidazoyl, naphthylimide, or diaminostilbene disulfonates. In accordance with an embodiment, the optical brightener is tetrabenzotetra azaporphine. In accordance with an aspect, the detergent composition may contain 0.05 to 0.25 weight % of optical brightener and preferably 0.1 to 0.2 weight % of optical brightener. 10 The detergent composition in accordance with the present invention may further comprise an anti caking agent. The anti caking agent is incorporated in the detergent to make the detergent free flow. In accordance with an aspect the detergent contains about 7 to 20 weight %, preferably 8 to 15 weight % of anti caking agent. By way of specific example the anti caking agent is dolomite, preferably micronized dolomite having particle size distribution preferably less than 300 micron. In accordance with an aspect, an inorganic salt may be added to the detergent formulation. A mixture of two or more salts may also be added. In accordance with an embodiment, the detergent may contain about 4 to 8 weight %, preferably 6 weight % of inorganic salt. In accordance with an embodiment, the inorganic salt is an alkali metal salt of sulphuric acid. By way of specific example, the inorganic salt is sodium sulphate. In accordance with an aspect, an anti redeposition agent may be added to the detergent composition. The anti redeposition agent is added to the detergent to improve strength of the cotton fibre of fabrics on repeated wash. In accordance with an embodiment, sodium carboxy methyl cellulose may be added as an anti redeposition agent. In accordance with an aspect, the anti redeposition agent may be added to the detergent composition in the range of 1 to 5 weight % and preferably in the range of 2 to 4 weight %. In accordance with an aspect, the detergent composition may contain enzyme. Enzymes are added to the detergent to remove sweat gland secretions, dead skin cells, sebaceous gland secretions and blood stains. In accordance with an aspect, the detergent composition contains at least one enzyme. In accordance with an aspect, the enzyme used in the detergent composition may include but is not limited to protease, amylase, lipase, cellulose or any combination thereof. In accordance with a preferred embodiment, the enzymes used in the detergent composition are effective at higher pH range. In accordance with an aspect, the detergent composition may contain 0.2 to 0.6 weight % enzyme and preferably 0.4 weight % enzyme. In accordance with an aspect, color or dye may optionally be added to the detergent composition to improve the aesthetic quality of detergent. In accordance with an embodiment, the detergent composition may contain 0.03 to 0.05% weight % and preferably 0.04% by weight of color. Any suitable dye or color may be used. In accordance with a preferred embodiment, phthalocyanine blue is used as a color in the detergent composition. 11 In accordance with an aspect, the detergent composition may contain other additives such as fragrance and speckles. In accordance with an aspect, the detergent composition may contain 0.05 to 0.075 weight% of fragrance. In accordance with an aspect, the detergent composition may contain 1 to 3 weight%, preferably 2% of speckles. In accordance with an embodiment, the speckles are soda base speckles. Detergent formulations, in accordance with an aspect of the invention are prepared and their composition in comparison with control formulations using soda ash is tabulated in Figure 6. The results of tests carried out on such detergent against the soda ash control formulations are tabulated in Figure 7. It is observed that detergent formulations prepared in accordance with embodiments of the invention performed better than the control formulations when the parameters like surface tension, detergency, foam length, and differential flow rate are considered. By way of example, white cotton fabric of 5cm x 5cm was stained with chicken blood by dipping the fabric into the blood dispersed solution. Then the fabric was dried in sun and ironed. After measurement of reflectance of fresh and blood stained fabric, washing cycle was performed with 1.0% solutions of four detergents with blood stained fabric by Launder - o -meter. After washing, the washed fabric was sun dried and ironed and then its reflectance was measured. With reference to Figure 8, the results of detergency test carried out on the detergent formulations in accordance with embodiments of the invention in comparison with soda ash control formulations are illustrated. From the results of detergency reported in Figure 8, it is observed that detergent formulation prepared in accordance with an embodiment of the invention containing enzyme is more effective in removing blood stain from the fabric compared to soda ash control formulations. In accordance with an aspect, the pH of the detergent formulation is in the range of 9.0 to 11.0, may preferably be from 9.25 to 10.86. The invention will be illustrated by the following examples which are not to be construed as limiting the invention in any way: Example 1: By way of a specific example the detergent composition comprises of between 25 to 35 weight % of crushed refined soda fines, 15 to 35 weight % of salt, 1 to 3 weight % of sodium 12 lauryl sulphate, 5 to 8 weight % sodium sulphate (inorganic salt), 1 to 3 weight % dry sodium salt of sulphonic acid, 0.05 to 0.25 weight % optical brightener, 0.03 to 0.05 weight % color, 7 to 20 weight % micronized dolomite (anti caking agent), 8 to 12 weight % sulphonic acid, 0.05 to 0.1 weight % fragrance, 0.5 to 5 weight % precipitated silica (flow aid), 2 to 8 weight% methyl ester sulphonate, 1 to 5 weight % carboxy methyl cellulose (anti redeposition agent), 6 to 8 weight % sodium tripolyphosphate, 1 to 3 weight % speckle, and 0.2 to 0.5 weight % enzyme. This formulation is suited for both hard and soft water. Example 2: By way of a specific example the detergent composition comprises of between 25 to 35 weight % of crushed refined soda fines, 15 to 35 weight % of salt, 1 to 3 weight % sodium lauryl sulphate, 1 to 3 weight % dry sodium salt of sulphonic acid, 0.05 to 0.25 weight % optical brightener, 0.03 to 0.05 weight % of color, 7 to 20 weight % micronized dolomite (anti caking agent/, i% to 5% soaYum siiYcafe, # to iZ weignt % sulfonic acitf, (7.(75 Co (t.( weignf % fragrance, 0.5 to 5 weight % precipitated silica (flow aid), 2 to 8 weight % methyl ester sulphonate, 1 to 5 weight % carboxy methyl cellulose (anti redeposition agent), 1 to 3 weight % speckles, and 0.2 to 0.5 weight % enzyme. This formulation is suited for both hard and soft water. With reference to Figure 9, a process of preparing a. detergent in accordance with an embodiment is illustrated. The process involves micronization of methyl ester sulphonate by milling along with a flow aid (101). In the embodiment illustrated, the flow aid is precipitated silica. The micronized methyl ester sulphonate along with th^ flow aid is charged into a mixer (102) that also receives a dispersing agent (103). The micronized methyl ester sulphonate along with the flow aid is mixed with the dispersing agent so as to generate a dispersion thereof. In the embodiment illustrated, the dispersing agent is sulphonic acid. An optical brightener is added into the mixer (104). Crushed refined soda fines obtained fi-0m the effluent generated during washing of trona soda is beneficiated by sieving through 1 mm sieve (105), grinding (106), followed by sieving through 250 micron sieve (107) and drying (108). The crushed refined soda fines so obtained (109) and salt (110) are charged in a ribboii mixer. A colour or dye is added into the mixture (111). The methyl ester sulphonate dispersion (l 12) along with a builder (113) is added into the ribbon mixture. In the embodiment illustrated, the builder is sodium silicate. A 13 second surfactant (114), such as sodium lauryl sulphate, an inorganic salt (115), such as sodium sulphate, an anti redeposition agent (116), such as sodium carboxy methyl cellulose and a second builder (117), such as sodium trio polyphosphate are simultaneously added into the mixture. Immediately after that, an anti caking agent is charged into the mixture (118). In the embodiment illustrated, the anti caking agent is dolomite. This is followed by a further dosing of the flow aid, such as silica (119). Fragrance is also added into the mixture (120). The product is immediately discharged from the ribbon mixer and is subjected to milling in a cage mill (121) and sieving through 1mm sieve (122). The oversized particles are subjected to further milling (123). The product so obtained is mixed with enzyme (124) and speckles (125) and the final product so obtained is packed (126). In accordance with an aspect, the micronization of methyl ester sulphonate along with the flow aid is continued for 1 to 5 minutes. In accordance with an aspect, the micromzed methyl ester sulphonate including silica is mixed with the dispersing agent while agitating the dispersing agent continuously by stirring. The dispersion so obtained is mixed with other detergent constituents preferably by spraying. In accordance with an aspect, methyl ester sulphonate dispersion is sprayed within 10 to 20 seconds, preferably 15 seconds while continuing the mixing. In accordance with an aspect, the salt is mixed for 30 seconds to 2 minutes, preferably for 1 minute. In accordance with an embodiment, secondary surfactant, inorganic salt, anti redeposition agent, and a second builder may be charged simultaneously in the ribbon mixture while continuing the mixing. In accordance with an aspect, the charging time may vary from 5 to 20 seconds, preferably 10 to 15 seconds. In accordance with an aspect, the time for mixing the anti caking agent varies from 2 to 8 seconds, preferably 7 seconds. In accordance with an aspect, the color is mixed for 1 to 3 minutes, preferably for 2 minutes. The detergent composition as described is suitable for use in both soft and hard water. The invention will be illustrated by the following examples which are not to be construed as limiting the invention in any way: 14 Example 3: Crushed refined soda fines obtained from effluent generated during washing of trona soda is beneficiated through sieving, grinding and drying. The process further involves milling of 6 kg methyl ester sulphonate with addition of 2 kg precipitated silica. The milled methyl ester sulphonate along with the precipitated silica is charged into 10 kg sulphonic acid where methyl ester sulphonate gets completely dispersed in the sulphonic acid. 0.2 kg optical brightener is then added while continuing the mixing. 30 kg beneficiated crushed refined soda fines and 20.4 kg salt are charged first in a ribbon mixer keeping the mixer on and mixed for 1 minute. Milled methyl ester sulphonate so prepared along with 7 kg sodium tripolyphosphate are charged within 15 seconds while continuing the mixing. 2 kg dry sodium salt of sulphonic acid, 2 kg sodium lauryl sulphate, 6 kg sodium sulphate, and 4 kg sodium salt of carboxy methyl cellulose are simultaneously added to the mixture keeping the mixing on and the charging time varies from 10 to 15 seconds. Immediately after that 8 kg micronized dolomite is charged into the mixture and mixed for 5 seconds. This is followed by further dosing of substantial amount of precipitated silica spread over the whole mass to make the product free flow. 0.075 kg fragrance is then injected into the mixture. The product is immediately discharged from the ribbon mixer. The product is then charged to cage mill for mixing and size reduction. The product is screened through 1 mm sieve. The product so obtained is mixed with 0.4 kg enzyme and 2 kg speckles in a blender to obtain the detergent. The detergent is then packed. Example 4: Crushed refined soda fines obtained from effluent generated during washing of trona soda is beneficiated through sieving, grinding and drying. The process further involves milling of 4 kg methyl ester sulphonate with addition of 1 kg precipitated silica. The milled methyl ester sulphonate along with the precipitated silica is charged into 8 kg sulphonic acid where methyl ester sulphonate gets completely dispersed in the sulphonic acid. 0.1 kg optical brightener is then added while continuing the mixing. 30 kg beneficiated crushed refined soda fines and 32.4 kg salt are charged first in a ribbon mixer keeping the mixer on and mixed for 1 minute. 0.04 kg color is charged into the mixture and mixed for 2 minutes. Milled methyl ester sulphonate so prepared along with 3 kg sodium silicate are charged within 15 seconds while continuing the mixing. 2 kg sodium lauryl sulphate and 2 kg sodium salt of carboxy methyl cellulose are 15 simultaneously added to the mixture keeping the mixing on and the charging time varies from 10 to 15 seconds. Immediately after that 15 kg micronized dolomite is charged into the mixture and mixed for 5 seconds. This is followed by further dosing of substantial amount of precipitated silica spread over the whole mass to make the product free flow. 0.075 kg fragrance is then injected into the mixture. The product is immediately discharged from the ribbon mixer. The product is then charged to cage mill for mixing and size reduction. The product is screened through 1 mm sieve. The product so obtained is mixed with 0.4 kg enzyme and 2 kg speckles in a blender to obtain the detergent. The detergent is then packed. Specific embodiments are described below: A process for preparing a detergent including methyl ester sulphonate comprising micronizing the methyl ester sulphonate; dispersing the micronized methyl ester sulphonate in a dispersing agent and spraying the dispersion on the detergent constituents. A process for preparing a detergent including methyl ester sulphonate comprising micromzing the methyl ester sulphonate, micronization of methyl ester sulphonate including addition of a flow aid to the methyl ester sulphonate; dispersing the micronized methyl ester sulphonate in a dispersing agent and spraying the dispersion on the detergent constituents, the detergent constituents including a source of bicarbonate. Further specific embodiments are described below: Such process(s) wherein the dispersing agent is an alpha-sulpho fatty acid, preferably a linear alkyl benzene sulphonic acid. Such process(s) wherein the ratio of micronized methyl ester sulphonate to dispersing agent is substantially 2:3. Such process(s) wherein the flow aid is precipitated silica. Such process(s) wherein 0.25 to 2.0 weight % precipitated silica is added as a flow aid during micronization of methyl ester sulphonate. Such process(s) wherein the source of bicarbonate is crushed refined soda fines, the crushed refined soda fines obtained from the effluent generated from a soda ash production plant using trona soda as raw material. 16 Such process(s) wherein the crushed refined soda fines is beneficiated for use in the detergent; the benefication including drying and reducing the size of the crushed refined soda fines to below 500 micron while retaining its bicarbonate content. A process for manufacturing a detergent comprising micronizing the methyl ester sulphonate; adding the micronized methyl ester sulphonate in a dispersing agent to obtain a dispersion and spraying the dispersion on the detergent constituents, the detergent constituents including beneficiated crushed refined soda fines obtained by drying and reducing the size of the crushed refined soda fines to beiow 50o micron while retaining its bicarbonate content. INDUSTRIAL APPLICABILITY Incorporation of methyl ester sulphonate in the manner as described above in the detergent formulation improoves the deter gency performance. The detergent formulation is also found to exhibit improved hard water cleaning performance, and thus allows the detergent to be used in a wider variety 0f cleaning applications. The hard water tolerance is also beneficial because hard water is used in any areas of the world for cleaning. The use of crusne refined soda fines provides a substitute for synthetic soda ash used in conventional detergent formulation. The use of micronized methyl ester sulphonate including a flow aid shows higher solubility in water, thereby exhibiting improved detergency performance compared to the conventional detergent formulations using methyl ester sulphonate. The dispersion of me micronized methyl ester sulphonate in the manufacture of the detergent along with the use of secondary surfactant generates the lather and foam required for improved cleaning performance. The present detergent formulation based on methyl ester sulphonate and crushed; refined soda fines are effective in both hard and soft water system. In addition, the dispersioh of methyl ester sulphonate helps in efficient mixing of micronized methyl ester sulphonate wim the other constituents of the detergent thereby leading to better cleaning performance compared to conventional detergents using methyl ester sulphonate. The use of crushed refined soda fines as a bicarbonate source also helps in preventing degradation of methyl ester sulphonate at higher pH, thereby maximizing the utilization of methyl ester sulphonate in the detergent. Moreover, the beneficiated crushed refined soda fines 17 used in the detergent formulation are also less expensive compared to synthetic soda ash used in conventional detergents. Previously, the effluent generated from the trona soda washery is disposed in nearby lands. An attempt has been made to address the problem of effluent disposal by the way of re-utilizing the wastes in the manufacture of consumer goods, such as detergents. In addition, as linear alkylbenzene sulphonic acid and methyl ester sulphonate used in the present composition are straight chain structures, they confer bio degradability i.e. environment friendliness to the detergent. Use of economical grade methyl ester sulphonate in detergent formulation contributes to the reduction in formulation cost and particle size distribution has been controlled to increase product uniformity. Special enzymes, added to the detergent, serve specific purposes like removal of blood and sweat stains. Thus, the detergent composition in accordance with an aspect is capable of providing a complete packaged product to the consumers of detergent powder for their daily requirement of fabric wash. 18 We claim: 1. A process for preparing a detergent including methyl ester sulphonate comprising: micronizing the methyl ester sulphonate; dispersing the micronized methyl ester sulfonate in a dispersing agent and spraying the dispersion on the detergent constituents. 2. A process for preparing a detergent including methyl ester sulphonate comprising: micronizing the methyl ester sulphonate, micronization of methyl ester sulphonate including addition of a flow aid to the methyl ester sulphonate; dispersing the micronized methyl ester sulphonate in a dispersing agent and spraying the dispersion on the detergent constituents, the detergent constituents including a source or bicartionate. 3. A process as claimed in claim 1 or 2 wherein the dispersing agent is an alpha-sulpho fatty acid, preferably a linear alkyl benzene sulphonic acid. 4. A process as claimed in any preceding claim wherein the ratio of micronized methyl ester sulphonate to dispersing agent is substantially 2:3. 5. A process as claimed in claim 2 wherein the flow aid is precipitated silica. 6. A process as claimed in claim 5 wherein 0.25 to 2.0 Weight % precipitated silica is added as a flow aid during micronization of methyl ester sulphonate. 7. A process as claimed in claim 2 wherein the source of bicarbonate is crushed refined soda fines, the crushed refined soda fines obtained from the effluent generated from a soda ash production plant using trona soda as raw material. 19 8. A process as claimed in claim 7 wherein the crushed refined soda fines is beneficiated for use in the detergent; the beneficiation including drying and reducing the size of the crushed refined soda fines to below 500 micron while retaining its bicarbonate content. 9. A process for manufacturing a detergent comprising: micronizing the methyl ester sulphonate; adding the micronized methyl ester sulphonate in a dispersing agent to obtain a dispersion and spraying the dispersion on the detergent constituents, the detergent constituents including beneficiated crushed refined soda fines obtained by drying and reducing the size of the crushed refined soda fines to below 500 micron while retaining its bicarbonate content. 10. A method substantially as herein described with reference to and as illustrated by the accompanying drawings. 11. A detergent prepared by the method substantially as herein described with reference to and as illustrated by the accompanying drawings.

Full Text

FORM 2
THE PATENTS ACT, 1970
(39 of 1970)
&
THE PATENTS RULES, 2003
COMPLETE SPECIFICATION
(See section 10, rule 13)
1. Title of the invention
"A DETERGENT COMPOSITION AND A PROCESS FOR PREPARING THE SAME"
2. Applicant(s)
Name Nationality Address
TATA CHEMICALS LTD. INDIA BOMBAY HOUSE, 24 HOMI MODI STREET MUMBAl -
400001

3. Preamble to the description
COMPLETE SPECIFICATION
The following specification particularly describes the invention and the manner in which it is
to be performed.

The disclosure relates to a detergent. More particularly, the invention relates to a detergent composition including methyl ester sulphonate and a method of manufacturing the same.
DESCRIPTION OF RELATED ART
Conventional dry mix detergent product formulations are based on synthetic soda ash. Dry detergent compositions are formed by mixing soda ash with one or more surfactants. In addition to soda ash arid surfactants, other additives such as builders, brighteners, soil release agents, perfumes etc are also added to detergents. However, since soda ash has to be manufactured, the cost of manufacturing soda ash adds to the cost of the detergent.
There have been attempts to use methyl ester sulphonate as an active detergent. As methyl ester sulphonate is easily obtainable from renewable sources such as natural oil or fats and due to its biodegradable nature, it may be preferable over other surfactants conventionally used in detergent formulations. Furthermore, the use of certain commercial grades of methyl ester sulphonate as active detergent may result in a considerably low price detergent formulation.
However, methyl ester sulphonate present in conventional detergent formulations hydrolyzes in the presence of moisture and high pH detergent components including builders such as carbonates, an9.0) results in poor detergency performance and reduced application flexibility. Moreover, as methyl ester sulphonate tends to form lumps it cannot be effectively niixed with the other detergent constituents and thus, addition of methyl ester sulphonate as such in the detergent deteriorates the free flowing nature of the detergent.
In view of the above, there is a need to formulate a detergent composition enabling effective and maximum utilization of methyl ester sulphonate as an active detergent. Moreover, the detergent should be free flow and have good lather and foam generation property, improved detergency performance and should be cost effective.
2

SUMMARY
The invention relates to a process for preparing a detergent including methyl ester sulphonate comprising micronizing the methyl ester sulphonate; dispersing the micronized methyl ester sulphonate in a dispersing agent and spraying the dispersion on the detergent constituents.
The invention also relates to a process for preparing a detergent including methyl ester sulphonate comprising micronizing the methyl ester sulphonate, micronization of methyl ester sulphonate including addition of a flow aid to the methyl ester sulphonate; dispersing the micronized methyl ester sulphonate in a dispersing agent and spraying the dispersion on the detergent constituents, the detergent constituents including a source of bicarbonate.
The invention further relates to a process for manufacturing a detergent comprising micronizing the methyl ester sulphonate; adding the micronized methyl ester sulphonate in a dispersing agent to obtain a dispersion and spraying the dispersion on the detergent constituents, the detergent constituents including beneficiated crushed refined soda fmes obtained by drying and reducing the size of the crushed refined soda fines to below 500 micron while retaining its bicarbonate content.
BRIEF DESCRIPTION OF ACCOMPANYING DRAWINGS
The accompanying drawings illustrate the preferred embodiments of the invention and together with the following detailed description serve to explain the principles of the invention.
Figure 1 tabulates comparative particle size distribution data of methyl ester sulphonate, micronized methyl ester sulphonate and micronized methyl ester sulphonate along with a flow aid.
Figure 2 tabulates the ratio of methyl ester sulphonate to sulphonic acid in accordance with an embodiment.
Figure 3 tabulates comparative detergency of methyl ester sulphonate, milled methyl ester sulphonate and linear alkyl benzene sulphonic acid (non dispersion), a dispersion of milled methyl ester sulphonate and linear alkyl benzene sulphonic acid in accordance with an aspect.
Figure 4 tabulates the composition of beneficiated crushed refined soda ash fines developed for detergent formulation in accordance with an aspect of the invention in comparison with synthetic soda ash.
3

Figure 5 tabulates the results of analysis of pH and percent methyl ester sulphonate in detergent formulations 1, 2 and 3 in accordance with embodiments of the invention in comparison with a control detergent formulation.
Figure 6 tabulates detergent formulations in accordance with embodiments in comparison with soda ash control formulations.
Figure 7 tabulates the results of tests carried out on samples of detergent formulations in accordance with embodiments of the invention in comparison with soda ash control formulations.
Figure 8 tabulates the result of detergency test carried out on samples of detergent formulations with enzymes in accordance with an embodiment against soda ash control formulations.
Figure 9 schematic illustration of the method of manufacturing a detergent and preparation of detergent in accordance with an embodiment of the invention.
DETAILED DESCRIPTION
To promote an understanding of the principles of the invention, reference will be made to the embodiment and specific language will be used to describe the same. It will nevertheless be understood that no limitation on scope of the invention is thereby intended, such alterations and further modifications in the described composition and such further applications of the principles of the inventions as disclosed therein being contemplated as would normally occur to one skilled in art to which the invention relates.
A detergent composition using methyl ester sulphonate is described. More particularly, a detergent composition using micronized methyl ester sulphonate is described.
The invention further relates to a detergent composition comprising crushed refined soda fines, the crushed refined soda fines are typically obtained from the effluent generated from a soda ash production plant using trona soda as raw material.
In accordance with an aspect, the micronized methyl ester sulphonate as used in the detergent includes a flow aid.
In accordance with an aspect, the detergent may further comprise a dispersing agent and other constituents including but not limited to salt, secondary surfactant, optical brightener,
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colour, anti caking agent, fragrance, anti redeposition agent, speckles, enzymes, builders or the like.
In accordance with an embodiment, the detergent composition comprises micronized methyl ester sulphonate including a flow aid, a dispersing agent and at least one bicarbonate source.
In accordance with an embodiment, the detergent composition comprises micronized methyl ester sulphonate including a flow aid, a dispersing agent and crushed refined soda fines.
In accordance with an alternative embodiment, the detergent comprises micronized methyl ester sulphonate including a flow aid, a dispersing agent, at least one enzyme and crushed refined soda fines.
In accordance with an embodiment, the detergent comprises micronized methyl ester sulphonate including a flow aid, a dispersing agent, at least one enzyme, a salt, a secondary surfactant, an optical brightener, a colour or dye, an anti caking agent, fragrance, an anti redeposition agent, speckles, a builder and crushed refined soda fines.
A process for preparing a detergent containing methyl ester sulphonate is also described. A process for preparing a detergent, in accordance with the invention, involves micronization of methyl ester sulphonate, mixing the micronized methyl ester sulphonate with a dispersing agent and adding the dispersion so obtained to other detergent constituents.
In accordance with an aspect, the micronization of methyl ester sulphonate includes the addition of a flow aid.
In accordance with an aspect, the process for preparing a detergent includes the addition of a bicarbonate source to the detergent.
In accordance with an aspect, methyl ester sulphonate used in the present formulation is
an alpha-sulpho fatty acid ester, which is generally of the following formula (I):
RCHCOOCH3 (I)
SO3M+ wherein R is an alkyl chain having 4 to 24 carbon atoms, preferably 12 to 18 carbon atoms, and M+ is a monovalent or divalent alkali metal. For example, R is a C8, C10, C12, CM, C16 or C18 alkane and M is typically an alkali metal, such as sodium or potassium. In accordance with an
5

aspect, methyl ester sulphonate is a sodium methyl ester sulphonate, such as a sodium C8 to C18 methyl ester sulphonate.
In one embodiment, the methyl ester sulphonate is a C8, C10, C12 CI4, C16 or C18 methyl ester sulphonate. In another embodiment the mefhy) ester sulphonsle comprises a mixture of different chain length Methyl ester sulphonate esters such as a mixture of C8, Ci0, Cl2, C14, Cl6 and/or C18 methyl estet- sulphonate. Such a mixture of methyl ester sulphonate can be prepared from a natural fat or oil, or synthetic fatty alcohols.
In alternative embodiment, methyl ester sulphonate is a mixture of methyl ester sulphonates having different chain lengths. Suitable mixtures of such methyl ester sulphonate include about C8, Cl0, C12 and/or CM methyl ester sulphonate combined with C16 and/or C18 methyl ester sulphonate m ratios from about 1: 99 to about 99: 1. In another embodiment, the mixture comprises about 1 to 99 weight % of C16 methyl ester sulphonate and about 99 to about 1 weight % of C18 methyl ester sulphonate.
Methyl ester sulphonate can be prepared from a variety of sources including beef tallow, palm kernel oil, palm kaernel (olein) oil, palm kernel (stearin) oil, coconut oil, soybean oil, canola oil, caster oil, Cohume oil, coco butter, linseed oil, palm oil, white grease, cotton seed oil, corn oil, rape seed oil, yellow grease or mixtures thereof. Suitable fatty acids to make methyl ester sulphonates include but not limited to, caprylic (C8), capric (C10), lauric (C12), myristic (C 14), myrisloleic (CM), Palmitic (C16), palmitoleic (C16), stearic (C18), oleic (C18), linoleic (C 18), linolenic (C18), ricinoleic (C18), arachidic (C20), gadolic (C20), behenic (C22) and erucic (C 22) fatty acids.
In accordance with an aspect, the detergent comprises about 2 to 8 weight %, preferably 4 to 6 weight % of methyl ester sulphonate.
In accordance with an aspect, a flow aid is added to methyl ester sulphonate. The flow aid is added to improve the granularity of the product, for example by preventing aggregation and/or caking of the granules. In addition, detergent formulation comprising flow aid exhibits higher solubility and cleaning performance. Suitable flow aid according to the present invention includes, but not limited to crystalline or amorphous alkali metal silicates, aluminosilicates including zeolites, citrates, dicamol, calcite, diatomaceous earths, talc or silica. In accordance with a preferred embodiment, the flow aid is precipitated silica.
6

The cleaning performance (% detergency) of deterget incliding methyl ester sulphonate as commercially available in the formulation has been found to be very low. The experimental results showed that the cleaning performance (% detergency) 0f detergent formulation including methyl ester sulphonate as such was 18.50 only. In accordance with an aspect, the methyl ester sulphonate is micronized prior mixing it with other detergent constituents. The micronized methyl ester sulphonate is not completely free flow and forrns small jumps, jn accordance with an aspect, methyl ester sulphonate is micronised with addition of flow aid such as precipitated silica. In accordance with an aspect, addition of about 0.25 t0 2.0 weight % precipitated silica during micronization of methyl ester sulphonate is required so as top obtain free flow micronized methyl ester sulphonate. By way of specific example, 100 gm of memyi ester sulphonate is micronized along with 0.50 gm of precipitated silica. With referance t0 Figure 1, the particle size distribution of micronized methyl ester sulphonate along with the flow aid in comparison with imliomixtf'irrctlry os'il'r ttfomat wilhrtufauidiliflr oifa" ifl%. agrfme&yi ester safafioctaCe is illustrated.
In accordance with an aspect, the detergent composition mrther comprises a dispersing agent. The dispersing agent is used to suspend solid particles ind to prevent settling thereof so as to obtain a suspension capable of mixing effectively with other detergent constituents. In accordance with an embodiment, the dispersing agent may by a non--surface active polymer. In accordance with an alternative embodiment, the dispersing agent may be a surfactant. In accordance with a preferred embodiment, the dispersing agent is linear alkyl benzene sulfonic acid. The detergent composition, in accordance with an aspect contains 8 to 15 weight % of a dispersing agent, preferably 8 to 10 weight % of dispersing agent. By way of specific example, micronized methyl ester sulphonate including precipitated silica is mixed with linear alkyl benzene sulfonic acid so as to obtain a dispersion thereof with reference to Figure 2, ratio of micronized methyl ester sulphonate to linear alkyl benzene sulfonic acid in accordance with an aspect is illustrated. By way of specific example, ratio of micronized methlythyl ester sulphonate to linear alkyl benzene sulfonic acid is 2:3.
Experimental results showed that mixing of the methly ester sulphonate dispersion so prepared with other detergent constituents substantially enhanced the performance of the detergent. With reference to Figure 3, the cleaning performance (o/0 detergency) of detergent
7

including methyl ester sulphonate dispersion in comparison with detergents including methyl ester sulphonate, and milled methyl ester sulphonate and linear alkyl benzene sulfonic acid (non-dispersion) is illustrated. In accordance with an embodiment, the cleaning performance (% detergency) of the detergent composition including methyl ester sulphonate dispersion is 56.
In accordance with an aspect, the detergent comprises a bicarbonate source. In accordance with an embodiment, the bicarbonate source is crushed refined soda fines. The crushed refined soda fines are wastes that are generated from a soda ash plant using trona soda for the production of soda ash. The effluent that comes out from the overflow of washery of a soda ash plant is known as crushed refined soda fines slurry. The liquid is drained out to leave crushed refined soda fines that become dry by sunlight.
In accordance with an aspect the crushed refined soda fines is treated and purified before it is used in a detergent formulation. The crushed refined soda fines are beneficiated by the sieving the raw crushed refined soda fines to obtain crushed refined soda fines having a particle size distribution of 2 mm or less, drying the crushed refined soda fines to reduce the moisture content, and reducing the particle size of the crushed refined soda fines to below 500 microns. In accordance with an aspect, the crushed refined soda fines must be dried in a manner that does not substantially deplete the sodium bicarbonate content. With reference to Figure 4, the composition of beneficiated crushed refined soda fines in comparison with synthetic soda ash is illustrated.
The crushed refined soda fines may be added as a part or complete substitute for the soda ash. In accordance with an embodiment, crushed refined soda fines are added as a complete substitute for soda ash.
In accordance with an aspect, the detergent composition contains 25 to 40 weight % of crushed refined soda fines and preferably the detergent composition contains about 30 weight % of crushed refined soda fines.
Crushed refined soda fines included in the detergent formulation may act as a bicarbonate source so as to control the pH of the detergent formulation at higher range (> pH 9) and to stabilize methyl ester sulphonate, which is prone to degradation at higher pH. In the detergent formulation, generation of hydroxyl ions occurs due to dissolution of alkaline salts in water and these ions may affect the effectiveness of methyl ester sulphonate. The bicarbonate present in the detergent formulation provides a buffering effect. The bicarbonate ions react with hydroxyl ion
8

(generated from salt hydrolysis) to form carbonate ion and water (II). This allows methyl ester sulphonate to be effective even at higher pH levels.
HCXV + OH" = C03= + H20 (II)
A higher pH detergent has better cleaning performance. However, addition of bicarbonate lowers the pH of the detergent, as seen in the experimental results tabulated in Figure 5. Detergent compositions 1, 2 and 3 having different concentrations of bicarbonate are developed in accordance with embodiments of the invention. A control composition without any bicarbonate is also prepared and compared with the compositions 1, 2 and 3. The amount of bicarbonate added to the composition is important, as excess bicarbonate tends to lower the pH in a manner that negates the advantage of addition of the bicarbonate. As indicated in Figure 5, the composition 3 containing 1.6 weight % of bicarbonate, showed the highest amount of methyl ester sulphonate (10.65 %) available in the composition at higher pH (pH 10.86).
In accordance with an aspect the detergent composition may contain salt. In accordance with an aspect, the detergent composition contains 15 to 35 weight % of the salt and preferably the detergent composition contains 20.4 to 32.4 weight % of salt. Any suitable soluble salt may be added to the detergent composition. In accordance with an embodiment, the detergent composition may contain sodium chloride as salt. Sodium chloride helps in removing bloodstains in the garment and helps to retain color.
In accordance with an aspect, the detergent composition may contain builder. Builders may comprise of organic or inorganic compounds. Builders added to the detergent composition help in dispersion and suspension of particulate matters, maintenance of an alkaline environment required for efficient cleaning, emulsification of organic oils and fats, softening of water, prevention of redeposition of soil and inhibition of corrosion of metals in processing and washing equipments. Suitable builders for the detergent formulation according to the present invention include, but not limited to, silicate containing builders such as polysilicates, alkali metal silicates, wholly or partially crystallite layer-form silicate, phyllosilicates or disilicates, silicated salt i.e. a salt such as a carbonate, sulphate, alkali metal carbonate, alkali metal sulphate, ammonium carbonate, bicarbonate, sesquicarbonate or mixture thereof, that has been treated with a silicate salt; aluminosilicate containing builders such as zeolites; and phosphate containing builders such as alkali metal phosphates, orthophosphates, polyphosphates, triopolyphophate,
9

pyropolyphosphate, or polymer phosphates; carbonate builders such as soda ash; oxygen releasing builders such as sodium perborate, sodium percarbonate. These builders may be used alone or in combination. In accordance with an embodiment, sodium tripolyphosphates may be used as a builder. In accordance with alternative embodiment, sodium silicate may be used as a builder. In accordance with a preferred embodiment, the detergent composition comprises sodium silicate having a ratio of Si02 toNa20 substantially in the range of 3.0 to about 3.10. In accordance with an embodiment, the detergent composition may contain 2 to 4 weight %, preferably 3 weight % of builder. In accordance with an alternative embodiment, the the detergent composition may contain 6 to 8 weight %, preferably 7 weight % of builder.
In accordance with an aspect, the detergent composition may comprise a secondary surfactant. The secondary surfactant is added to the detergent formulation as a supplement to methyl ester sulphonate in respect of lather and foam generation. Any cationic, anionic or neutral surfactant may be added to the detergent composition as secondary surfactant including bat not limited to long-chain amino condensates with ethylene oxide and quaternary ammonium compounds, alpha olefin sulphonate, alkyl aryl sulphonic acids, alkyl sulphonic acids, salts of alkyl sulfuric acids, fatty acid derivatives and polyethylelene oxide ether condensates of alkylphenols, ethoxylated aliphatic alcohols, carboxylic esters 0r any combination thereof. The surfactants may be used alone or in combination with on.e another. In accordance with a preferred embodiment, the secondary surfactant is sodium lauryl sulphate. In accordance with an alternative embodiment, a mixture of linear alkyl benzene sulphonic acid and sodium salt of sulphonic acid may be used as a secondary surfactant. In accordance with an embodiment, the detergent composition may contain I to 3 weight %, preferably 2 weight % of secondary surfactant. In accordance with an alternative embodiment, the detergent composition may contain 3 to 5 weight %, preferably 4 weight % of secondary surfactant.
In accordance with an aspect, optical brightener may be added to the detergent composition. Optical brighteners that may be added to the detergent include but are not limited to naphthotriazolylstilbenes, benzoxazolyl, benzimidazoyl, naphthylimide, or diaminostilbene disulfonates. In accordance with an embodiment, the optical brightener is tetrabenzotetra azaporphine. In accordance with an aspect, the detergent composition may contain 0.05 to 0.25 weight % of optical brightener and preferably 0.1 to 0.2 weight % of optical brightener.
10

The detergent composition in accordance with the present invention may further comprise an anti caking agent. The anti caking agent is incorporated in the detergent to make the detergent free flow. In accordance with an aspect the detergent contains about 7 to 20 weight %, preferably 8 to 15 weight % of anti caking agent. By way of specific example the anti caking agent is dolomite, preferably micronized dolomite having particle size distribution preferably less than 300 micron.
In accordance with an aspect, an inorganic salt may be added to the detergent formulation. A mixture of two or more salts may also be added. In accordance with an embodiment, the detergent may contain about 4 to 8 weight %, preferably 6 weight % of inorganic salt. In accordance with an embodiment, the inorganic salt is an alkali metal salt of sulphuric acid. By way of specific example, the inorganic salt is sodium sulphate.
In accordance with an aspect, an anti redeposition agent may be added to the detergent composition. The anti redeposition agent is added to the detergent to improve strength of the cotton fibre of fabrics on repeated wash. In accordance with an embodiment, sodium carboxy methyl cellulose may be added as an anti redeposition agent. In accordance with an aspect, the anti redeposition agent may be added to the detergent composition in the range of 1 to 5 weight % and preferably in the range of 2 to 4 weight %.
In accordance with an aspect, the detergent composition may contain enzyme. Enzymes are added to the detergent to remove sweat gland secretions, dead skin cells, sebaceous gland secretions and blood stains. In accordance with an aspect, the detergent composition contains at least one enzyme. In accordance with an aspect, the enzyme used in the detergent composition may include but is not limited to protease, amylase, lipase, cellulose or any combination thereof. In accordance with a preferred embodiment, the enzymes used in the detergent composition are effective at higher pH range. In accordance with an aspect, the detergent composition may contain 0.2 to 0.6 weight % enzyme and preferably 0.4 weight % enzyme.
In accordance with an aspect, color or dye may optionally be added to the detergent composition to improve the aesthetic quality of detergent. In accordance with an embodiment, the detergent composition may contain 0.03 to 0.05% weight % and preferably 0.04% by weight of color. Any suitable dye or color may be used. In accordance with a preferred embodiment, phthalocyanine blue is used as a color in the detergent composition.
11

In accordance with an aspect, the detergent composition may contain other additives such as fragrance and speckles. In accordance with an aspect, the detergent composition may contain 0.05 to 0.075 weight% of fragrance. In accordance with an aspect, the detergent composition may contain 1 to 3 weight%, preferably 2% of speckles. In accordance with an embodiment, the speckles are soda base speckles.
Detergent formulations, in accordance with an aspect of the invention are prepared and their composition in comparison with control formulations using soda ash is tabulated in Figure 6. The results of tests carried out on such detergent against the soda ash control formulations are tabulated in Figure 7. It is observed that detergent formulations prepared in accordance with embodiments of the invention performed better than the control formulations when the parameters like surface tension, detergency, foam length, and differential flow rate are considered.
By way of example, white cotton fabric of 5cm x 5cm was stained with chicken blood by dipping the fabric into the blood dispersed solution. Then the fabric was dried in sun and ironed. After measurement of reflectance of fresh and blood stained fabric, washing cycle was performed with 1.0% solutions of four detergents with blood stained fabric by Launder - o -meter. After washing, the washed fabric was sun dried and ironed and then its reflectance was measured. With reference to Figure 8, the results of detergency test carried out on the detergent formulations in accordance with embodiments of the invention in comparison with soda ash control formulations are illustrated. From the results of detergency reported in Figure 8, it is observed that detergent formulation prepared in accordance with an embodiment of the invention containing enzyme is more effective in removing blood stain from the fabric compared to soda ash control formulations.
In accordance with an aspect, the pH of the detergent formulation is in the range of 9.0 to 11.0, may preferably be from 9.25 to 10.86.
The invention will be illustrated by the following examples which are not to be construed as limiting the invention in any way: Example 1:
By way of a specific example the detergent composition comprises of between 25 to 35 weight % of crushed refined soda fines, 15 to 35 weight % of salt, 1 to 3 weight % of sodium
12

lauryl sulphate, 5 to 8 weight % sodium sulphate (inorganic salt), 1 to 3 weight % dry sodium salt of sulphonic acid, 0.05 to 0.25 weight % optical brightener, 0.03 to 0.05 weight % color, 7 to 20 weight % micronized dolomite (anti caking agent), 8 to 12 weight % sulphonic acid, 0.05 to 0.1 weight % fragrance, 0.5 to 5 weight % precipitated silica (flow aid), 2 to 8 weight% methyl ester sulphonate, 1 to 5 weight % carboxy methyl cellulose (anti redeposition agent), 6 to 8 weight % sodium tripolyphosphate, 1 to 3 weight % speckle, and 0.2 to 0.5 weight % enzyme. This formulation is suited for both hard and soft water. Example 2:
By way of a specific example the detergent composition comprises of between 25 to 35 weight % of crushed refined soda fines, 15 to 35 weight % of salt, 1 to 3 weight % sodium lauryl sulphate, 1 to 3 weight % dry sodium salt of sulphonic acid, 0.05 to 0.25 weight % optical brightener, 0.03 to 0.05 weight % of color, 7 to 20 weight % micronized dolomite (anti caking agent/, i% to 5% soaYum siiYcafe, # to iZ weignt % sulfonic acitf, (7.(75 Co (t.( weignf % fragrance, 0.5 to 5 weight % precipitated silica (flow aid), 2 to 8 weight % methyl ester sulphonate, 1 to 5 weight % carboxy methyl cellulose (anti redeposition agent), 1 to 3 weight % speckles, and 0.2 to 0.5 weight % enzyme. This formulation is suited for both hard and soft water.
With reference to Figure 9, a process of preparing a. detergent in accordance with an embodiment is illustrated. The process involves micronization of methyl ester sulphonate by milling along with a flow aid (101). In the embodiment illustrated, the flow aid is precipitated silica. The micronized methyl ester sulphonate along with th^ flow aid is charged into a mixer (102) that also receives a dispersing agent (103). The micronized methyl ester sulphonate along with the flow aid is mixed with the dispersing agent so as to generate a dispersion thereof. In the embodiment illustrated, the dispersing agent is sulphonic acid. An optical brightener is added into the mixer (104). Crushed refined soda fines obtained fi-0m the effluent generated during washing of trona soda is beneficiated by sieving through 1 mm sieve (105), grinding (106), followed by sieving through 250 micron sieve (107) and drying (108). The crushed refined soda fines so obtained (109) and salt (110) are charged in a ribboii mixer. A colour or dye is added into the mixture (111). The methyl ester sulphonate dispersion (l 12) along with a builder (113) is added into the ribbon mixture. In the embodiment illustrated, the builder is sodium silicate. A
13

second surfactant (114), such as sodium lauryl sulphate, an inorganic salt (115), such as sodium sulphate, an anti redeposition agent (116), such as sodium carboxy methyl cellulose and a second builder (117), such as sodium trio polyphosphate are simultaneously added into the mixture. Immediately after that, an anti caking agent is charged into the mixture (118). In the embodiment illustrated, the anti caking agent is dolomite. This is followed by a further dosing of the flow aid, such as silica (119). Fragrance is also added into the mixture (120). The product is immediately discharged from the ribbon mixer and is subjected to milling in a cage mill (121) and sieving through 1mm sieve (122). The oversized particles are subjected to further milling (123). The product so obtained is mixed with enzyme (124) and speckles (125) and the final product so obtained is packed (126).
In accordance with an aspect, the micronization of methyl ester sulphonate along with the flow aid is continued for 1 to 5 minutes.
In accordance with an aspect, the micromzed methyl ester sulphonate including silica is mixed with the dispersing agent while agitating the dispersing agent continuously by stirring. The dispersion so obtained is mixed with other detergent constituents preferably by spraying. In accordance with an aspect, methyl ester sulphonate dispersion is sprayed within 10 to 20 seconds, preferably 15 seconds while continuing the mixing.
In accordance with an aspect, the salt is mixed for 30 seconds to 2 minutes, preferably for 1 minute.
In accordance with an embodiment, secondary surfactant, inorganic salt, anti redeposition agent, and a second builder may be charged simultaneously in the ribbon mixture while continuing the mixing. In accordance with an aspect, the charging time may vary from 5 to 20 seconds, preferably 10 to 15 seconds.
In accordance with an aspect, the time for mixing the anti caking agent varies from 2 to 8 seconds, preferably 7 seconds.
In accordance with an aspect, the color is mixed for 1 to 3 minutes, preferably for 2 minutes.
The detergent composition as described is suitable for use in both soft and hard water.
The invention will be illustrated by the following examples which are not to be construed as limiting the invention in any way:
14

Example 3:
Crushed refined soda fines obtained from effluent generated during washing of trona soda is beneficiated through sieving, grinding and drying. The process further involves milling of 6 kg methyl ester sulphonate with addition of 2 kg precipitated silica. The milled methyl ester sulphonate along with the precipitated silica is charged into 10 kg sulphonic acid where methyl ester sulphonate gets completely dispersed in the sulphonic acid. 0.2 kg optical brightener is then added while continuing the mixing. 30 kg beneficiated crushed refined soda fines and 20.4 kg salt are charged first in a ribbon mixer keeping the mixer on and mixed for 1 minute. Milled methyl ester sulphonate so prepared along with 7 kg sodium tripolyphosphate are charged within 15 seconds while continuing the mixing. 2 kg dry sodium salt of sulphonic acid, 2 kg sodium lauryl sulphate, 6 kg sodium sulphate, and 4 kg sodium salt of carboxy methyl cellulose are simultaneously added to the mixture keeping the mixing on and the charging time varies from 10 to 15 seconds. Immediately after that 8 kg micronized dolomite is charged into the mixture and mixed for 5 seconds. This is followed by further dosing of substantial amount of precipitated silica spread over the whole mass to make the product free flow. 0.075 kg fragrance is then injected into the mixture. The product is immediately discharged from the ribbon mixer. The product is then charged to cage mill for mixing and size reduction. The product is screened through 1 mm sieve. The product so obtained is mixed with 0.4 kg enzyme and 2 kg speckles in a blender to obtain the detergent. The detergent is then packed. Example 4:
Crushed refined soda fines obtained from effluent generated during washing of trona soda is beneficiated through sieving, grinding and drying. The process further involves milling of 4 kg methyl ester sulphonate with addition of 1 kg precipitated silica. The milled methyl ester sulphonate along with the precipitated silica is charged into 8 kg sulphonic acid where methyl ester sulphonate gets completely dispersed in the sulphonic acid. 0.1 kg optical brightener is then added while continuing the mixing. 30 kg beneficiated crushed refined soda fines and 32.4 kg salt are charged first in a ribbon mixer keeping the mixer on and mixed for 1 minute. 0.04 kg color is charged into the mixture and mixed for 2 minutes. Milled methyl ester sulphonate so prepared along with 3 kg sodium silicate are charged within 15 seconds while continuing the mixing. 2 kg sodium lauryl sulphate and 2 kg sodium salt of carboxy methyl cellulose are
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simultaneously added to the mixture keeping the mixing on and the charging time varies from 10 to 15 seconds. Immediately after that 15 kg micronized dolomite is charged into the mixture and mixed for 5 seconds. This is followed by further dosing of substantial amount of precipitated silica spread over the whole mass to make the product free flow. 0.075 kg fragrance is then injected into the mixture. The product is immediately discharged from the ribbon mixer. The product is then charged to cage mill for mixing and size reduction. The product is screened through 1 mm sieve. The product so obtained is mixed with 0.4 kg enzyme and 2 kg speckles in a blender to obtain the detergent. The detergent is then packed.
Specific embodiments are described below:
A process for preparing a detergent including methyl ester sulphonate comprising micronizing the methyl ester sulphonate; dispersing the micronized methyl ester sulphonate in a dispersing agent and spraying the dispersion on the detergent constituents.
A process for preparing a detergent including methyl ester sulphonate comprising micromzing the methyl ester sulphonate, micronization of methyl ester sulphonate including addition of a flow aid to the methyl ester sulphonate; dispersing the micronized methyl ester sulphonate in a dispersing agent and spraying the dispersion on the detergent constituents, the detergent constituents including a source of bicarbonate.
Further specific embodiments are described below:
Such process(s) wherein the dispersing agent is an alpha-sulpho fatty acid, preferably a linear alkyl benzene sulphonic acid.
Such process(s) wherein the ratio of micronized methyl ester sulphonate to dispersing agent is substantially 2:3.
Such process(s) wherein the flow aid is precipitated silica.
Such process(s) wherein 0.25 to 2.0 weight % precipitated silica is added as a flow aid during micronization of methyl ester sulphonate.
Such process(s) wherein the source of bicarbonate is crushed refined soda fines, the crushed refined soda fines obtained from the effluent generated from a soda ash production plant using trona soda as raw material.
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Such process(s) wherein the crushed refined soda fines is beneficiated for use in the detergent; the benefication including drying and reducing the size of the crushed refined soda fines to below 500 micron while retaining its bicarbonate content.
A process for manufacturing a detergent comprising micronizing the methyl ester sulphonate; adding the micronized methyl ester sulphonate in a dispersing agent to obtain a dispersion and spraying the dispersion on the detergent constituents, the detergent constituents including beneficiated crushed refined soda fines obtained by drying and reducing the size of the crushed refined soda fines to beiow 50o micron while retaining its bicarbonate content.
INDUSTRIAL APPLICABILITY
Incorporation of methyl ester sulphonate in the manner as described above in the detergent formulation improoves the deter gency performance. The detergent formulation is also found to exhibit improved hard water cleaning performance, and thus allows the detergent to be used in a wider variety 0f cleaning applications. The hard water tolerance is also beneficial because hard water is used in any areas of the world for cleaning.
The use of crusne refined soda fines provides a substitute for synthetic soda ash used in conventional detergent formulation. The use of micronized methyl ester sulphonate including a flow aid shows higher solubility in water, thereby exhibiting improved detergency performance compared to the conventional detergent formulations using methyl ester sulphonate.
The dispersion of me micronized methyl ester sulphonate in the manufacture of the detergent along with the use of secondary surfactant generates the lather and foam required for improved cleaning performance. The present detergent formulation based on methyl ester sulphonate and crushed; refined soda fines are effective in both hard and soft water system. In addition, the dispersioh of methyl ester sulphonate helps in efficient mixing of micronized methyl ester sulphonate wim the other constituents of the detergent thereby leading to better cleaning performance compared to conventional detergents using methyl ester sulphonate.
The use of crushed refined soda fines as a bicarbonate source also helps in preventing degradation of methyl ester sulphonate at higher pH, thereby maximizing the utilization of methyl ester sulphonate in the detergent. Moreover, the beneficiated crushed refined soda fines
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used in the detergent formulation are also less expensive compared to synthetic soda ash used in conventional detergents.
Previously, the effluent generated from the trona soda washery is disposed in nearby lands. An attempt has been made to address the problem of effluent disposal by the way of re-utilizing the wastes in the manufacture of consumer goods, such as detergents. In addition, as linear alkylbenzene sulphonic acid and methyl ester sulphonate used in the present composition are straight chain structures, they confer bio degradability i.e. environment friendliness to the detergent.
Use of economical grade methyl ester sulphonate in detergent formulation contributes to the reduction in formulation cost and particle size distribution has been controlled to increase product uniformity. Special enzymes, added to the detergent, serve specific purposes like removal of blood and sweat stains. Thus, the detergent composition in accordance with an aspect is capable of providing a complete packaged product to the consumers of detergent powder for their daily requirement of fabric wash.
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We claim:
1. A process for preparing a detergent including methyl ester sulphonate comprising:
micronizing the methyl ester sulphonate;
dispersing the micronized methyl ester sulfonate in a dispersing agent and spraying the dispersion on the detergent constituents.
2. A process for preparing a detergent including methyl ester sulphonate comprising:
micronizing the methyl ester sulphonate, micronization of methyl ester sulphonate including addition of a flow aid to the methyl ester sulphonate;
dispersing the micronized methyl ester sulphonate in a dispersing agent and spraying the dispersion on the detergent constituents, the detergent constituents including a source or bicartionate.
3. A process as claimed in claim 1 or 2 wherein the dispersing agent is an alpha-sulpho fatty acid, preferably a linear alkyl benzene sulphonic acid.
4. A process as claimed in any preceding claim wherein the ratio of micronized methyl ester sulphonate to dispersing agent is substantially 2:3.
5. A process as claimed in claim 2 wherein the flow aid is precipitated silica.
6. A process as claimed in claim 5 wherein 0.25 to 2.0 Weight % precipitated silica is added as a flow aid during micronization of methyl ester sulphonate.
7. A process as claimed in claim 2 wherein the source of bicarbonate is crushed refined soda fines, the crushed refined soda fines obtained from the effluent generated from a soda ash production plant using trona soda as raw material.
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8. A process as claimed in claim 7 wherein the crushed refined soda fines is beneficiated for use in the detergent; the beneficiation including drying and reducing the size of the crushed refined soda fines to below 500 micron while retaining its bicarbonate content.
9. A process for manufacturing a detergent comprising:
micronizing the methyl ester sulphonate;
adding the micronized methyl ester sulphonate in a dispersing agent to obtain a dispersion and spraying the dispersion on the detergent constituents, the detergent constituents including beneficiated crushed refined soda fines obtained by drying and reducing the size of the crushed refined soda fines to below 500 micron while retaining its bicarbonate content.
10. A method substantially as herein described with reference to and as illustrated by the accompanying drawings.
11. A detergent prepared by the method substantially as herein described with reference to and as illustrated by the accompanying drawings.

Documents:

976-mum-2009-abstract.doc

976-mum-2009-abstract.pdf

976-MUM-2009-ASSIGNMENT(8-6-2009).pdf

976-MUM-2009-CLAIMS(AMENDED)-(1-7-2013).pdf

976-MUM-2009-CLAIMS(AMENDED)-(19-3-2014).pdf

976-MUM-2009-CLAIMS(MARKED COPY)-(1-7-2013).pdf

976-MUM-2009-CLAIMS(MARKED COPY)-(19-3-2014).pdf

976-mum-2009-claims.doc

976-mum-2009-claims.pdf

976-MUM-2009-CORRESPONDENCE(11-11-2011).pdf

976-MUM-2009-CORRESPONDENCE(11-11-2013).pdf

976-MUM-2009-CORRESPONDENCE(15-4-2009).pdf

976-MUM-2009-CORRESPONDENCE(3-11-2010).pdf

976-MUM-2009-CORRESPONDENCE(30-12-2013).pdf

976-MUM-2009-CORRESPONDENCE(8-5-2009).pdf

976-MUM-2009-CORRESPONDENCE(8-6-2009).pdf

976-MUM-2009-CORRESPONDENCE(IPO)-(7-10-2009).pdf

976-mum-2009-correspondence.pdf

976-mum-2009-description(complete).doc

976-mum-2009-description(complete).pdf

976-mum-2009-drawing.pdf

976-MUM-2009-FORM 1(8-5-2009).pdf

976-mum-2009-form 1.pdf

976-MUM-2009-FORM 18(3-11-2010).pdf

976-mum-2009-form 2(title page).pdf

976-mum-2009-form 2.doc

976-mum-2009-form 2.pdf

976-MUM-2009-FORM 3(1-7-2013).pdf

976-MUM-2009-FORM 3(11-11-2011).pdf

976-mum-2009-form 3.pdf

976-MUM-2009-FORM PCT-IB-326(1-7-2013).pdf

976-MUM-2009-FORM PCT-ISA-237(1-7-2013).pdf

976-MUM-2009-OTHER DOCUMENT(1-7-2013).pdf

976-MUM-2009-PETITION UNDER RULE 137(19-3-2014).pdf

976-MUM-2009-POWER OF AUTHORITY(8-5-2009).pdf

976-MUM-2009-REPLY TO EXAMINATION REPORT(1-7-2013).pdf

976-MUM-2009-REPLY TO HEARING(19-3-2014).pdf

976-MUM-2009-WO INTERNATIONAL PUBLICATION REPORT A3(1-7-2013).pdf

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Patent Number

260416

Indian Patent Application Number

976/MUM/2009

PG Journal Number

18/2014

Publication Date

02-May-2014

Grant Date

29-Apr-2014

Date of Filing

15-Apr-2009

Name of Patentee

TATA CHEMICALS LTD

Applicant Address

BOMBAY HOUSE, 24 HOMI MODY STREET, MUMBAI

Inventors:

#	Inventor's Name	Inventor's Address
1	PRASUN MUKHERJEE	TATA CHEMICALS LTD, HALDIA FACTORY, DURGA CHOWK, MIDNAPORE EAST, WEST BENGAL-721604.
2	SOUMEN SENSARMA	TATA CHEMICALS LTD, INNOVATION CENTRE, S NO.270, ANMOL PRIDE, BANER ROAD, PUNE-411045
3	SOUMI CHATTARAJ	TATA CHEMICALS LTD., HALDIA FACTORY, DURGA CHOWK, MIDNAPORE EAST, WEST BENGAL-721604

PCT International Classification Number

A61K8/72; A61K8/73; A61Q19/10

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA