Title of Invention

AN IMPROVED CRYOGENIC PROCESS FOR THE PRODUCTION OF MIXED SPICE POWDERS

Abstract

The present invention relates to an improved cryogenic process and device for producing mixed spice powders, which process helps in higher retention of etheric oils, prevention of oxidation and rancidity, product with better sensory profile, increase in throughput and reduction in grinding power consumption, possibility to fine grind mixture of difficult -to- grind spices, and finer, uniform particle sizes of the mix.

Full Text

The present invention relates to an improved cryogenic process for the production of mixed spice powders, particularly the invention relates to a process which helps in higher retention of etheric oils, prevention of oxidation and rancidity, product with better sensory profile, increase in throughput and reduction in grinding power consumption, possibility to fine grind mixture of difficult -to- grind spices, and finer, uniform particle sizes of the mix. Spice mixes are indispensable in kitchens in individual homes and institutions, and in food manufacturing industries for providing individuality to otherwise insipid dishes and for adding tang and zest to beverages and serve as good appetizers. Those who buy and use spices casually are usually unaware or cannot believe that the ancient trade in spices shaped the course of early history. There was a time when spices were eagerly sought and the wealth and power of nations were involved in the control of the spice trade. Despite their economic importance in the world trade, they have not received the attention they so richly deserve, notably in their processing and quality aspects. Value added products such as spice mix powders, ground spices, oleoresins and spice oil extracts have vast industrial applications and with improvements in processing, could improve their share in the market. Reference may be made to Lowrison G.C. Crushing and Grinding. (London : Butterworths 1974) wherein it is reported that in most of the grinding operations the applied energy (>99%) gets dissipated into heat. This is primarily due to the non-uniformity of the feed material in size, structure, defects, dislocation etc., so that an accurately judged application of force to all sample elements is not possible. Also the fracture process results in particles of varying size, needing unnecessarily large forces to get the product milled to a particular particle size. Further, due to various metering characteristics of different constituents of spice mix there tend to be clogging or clumping of some of the products inhibiting continuous production making conventional grinding not suitable for producing ground spice mix powders. Reference may be made to Pruthi JS. Spices and condiments: Chemistry, Microbiology, Technology. Advances in Food Research Supp. 4, Academic Press Inc., New York wherein it is reported that during conventional milling of spices, with no cooling of the mill and the product, the temperature increases to over to 90 degree C in most of the fast rotating mills. Since etheric oils have boiling points ranging from 50 degree C to 320 degree C, some of the precious components are lost due to conventional milling of different constituents of spice mix, resulting in low quality product. Also due to two stage grinding operations volatiles of heat sensitive products such as spices are lost and thus result in low quality product. Reference may be made to McKee LH, Thomson LD and Harden ML. Effect of three grinding methods on some properties of Nutmeg. Food Sci. Technol. 26 (1980) P. 121-125 wherein it is reported that when material to be ground contains high level of fat or oils (Nutmeg, clove, maces etc.,) they cause clogging of the mill affecting throughput and quality of the product. A high moisture content also gives problems in milling. In some cases it is possible to grind only after drying. High moisture content materials often tend to stick to the parts of the mill. The acceptable moisture content in practice varies from material to material. Reference may be made to Rich Norman I., and Martin D. Rich. Ready-to-eat molded meat product US Patent No. US 4287218 (1981), wherein the preparation of ready -to -eat molded meat product is reported. Whole pieces of injected and tumbled meat are layered into the bottom of a preformed old and covered with a mixture of ground meat. Alternatively, ground meat is mixed with additives and/or an emulsion and placed in the mold. The product is cooked under a vacuum finally. The major drawback here is there is no mentioning of method or composition of additives and/or an emulsion to be mixed with ground meat. Reference may be made to Byong W.Yoo Enhanced kimchi mix composition US Patent No. US6024992 (2000), wherein a composition of kimchi mix is reported. The kimchi mix has the composition of a spice mix, vitamin C and an organic acid. The spice mix comprised of salt, pepper powder, onion powder, garlic powder, mustard powder, paprika powder, kelp powder, fish powder, monosodium glutamate, sesame powder or mixtures thereof. The major drawback here is that only the product composition or formulation of the same is mentioned. Method of preparing as well as quality aspects of spice mix is not reported. Reference may be made to Kawachi Yoshihiro, Morioka Yuriko, Kami Akiko and Hisada Yoji. Spices used in feed for meat type poultry Japan Patent No. JP 7031382A2 (1994) wherein to obtain the spice mix which can increase the freshness of raw chicken and reduce the consumption of antibiotics by formulating spices inhibiting the proliferation of microorganisms on chicken meat is reported. The major draw back here is that only the spices such clove, mace, marjoram, mustard or the like which can inhibit microorganisms from growing on chicken, that are added to the feed for meat type chicken are mentioned and the method of preparing spice mix and related quality parameters are not reported. One of the popular spice mixes in India is the "garam masala", which primarily consists of Cinnamon sticks, cumin Seeds, coriander seeds, black pepper, bay Leaves and cloves. Various types of this mix are reported and practiced in India. Therefore, the reference to a 'spice mix powder1 in the invention includes within its scope, the Garam masala made in India. Reference may be made to Sridhar B.S. Jagmohan Rao J. and Kumar M.A. An improved process for the preparation of dry and fine spice powders Indian Patent No. 441/Del/2001 wherein to obtain the spice powders through cryogenic process is reported. The major draw back here is that only the process of producing individual spice powders such as clove, mace, marjoram, mustard or the like are mentioned and the method of preparing spice mix and related quality parameters are not reported. The main object of the present invention is to develop an improved cryogenic process for the production of mixed spice powders, which obviates the drawbacks as detailed above. Another object of the present invention is to produce a spice mix powder with high retention of etheric oils of the composite mix Still another object of the present invention is to produce a spice mix powder as an improved poultry feed that can impart meat and fat of the chicken an antibiotic action. Yet another object of the present invention is to provide an inert atmosphere from the beginning to end of the grinding operation and for storage and package of ground product. Yet another object of the present invention is to obtain an increase in throughput and decrease in specific energy for grinding compared to conventional grinding. Another object of the present invention is to fine grind mixture of difficult spices. Yet another object of the present invention is to prevent dusting during grinding of mixture of spices. Still another object of the present invention is to produce fine particles of ground spices in order to eliminate speckling problems and to reduce settling rates in liquid preparations. Yet another object of the present invention is to develop a convenient method for production of curries of highly acceptable quality and an improved spice mixture powder for use in dehydrated mutton curries and the like with a desirable flavor characteristics. Accordingly, the present invention provides an improved cryogenic process for the production of mixed spice powders. The invention thus provides a device for producing dry, fine, spice mix powders, said device comprising: a. a filling hopper (1) for feeding mixture of spices to be ground, b. a vibratory feeder (2) having provision, feed rate control, into which the mixture of spices to be ground enters, c. a screw conveyed cryogenic pre-cooler (3) driven by motor, and having reduction gear, inverter control, into which the spice mixture is further metered and liquid nitrogen from a Dewar or liquid nitrogen container is sprayed in the cryogenic pre-cooler through the liquid Nitrogen flow control system (5), combining with the spice mixture cooling, embrittling and ensuring uniform lattice on the mixture, d. a grinding mill (6, 7) which pulverizes the mixture, and said mill having sensors monitoring the temperature of the grinding zone, with the digital signal processing system optimizing liquid Nitrogen spray through automatic feed back control, and e. a collecting bin (8) to collect finally the ground product. In an embodiment of the present invnetion, the conveying of the material to the grinding mill may be through the screw conveyed cryogenic pre-cooler having variable speed drive for capacity 10 -150 kg/h, jacketed with an insulated top cover. In another embodiment of the present invention, conveying screw of the cryogenic pre-cooler is a fin or needle type hollow screw having provision to pass liquid nitrogen inside to spray on the spice, with a screw diameter ranging between 65 to 80 mm, length varying between 1 to 2 m, infeed size between 2 to10 mm driven by 1 to 2 h.p. variable speed motor gear box drive. In still another embodiment of the present invention, spraying of liquid nitrogen in the cryogenic pre-cooler is from Dewar or liquid Nitrogen container with the pressure ranging between 1 to 4 kg/cm2 with the time of spraying on the material controlled by the speed of the drive. Accordingly, the present invention provides an improved cryogenic process for the production of mixed spice powders using a device, shown in the figure (1) of the drawing accompanying the specification: a) transferring mixture of raw material to a filling hopper (1) of the device shown in figure (1), where from the mixture of spices to be ground enters the vibratory feeder (2), having provision for feed rate control, b) metering into screw conveyed cryogenic pre-cooler (3) driven by motor, reduction gear, inverter control, wherein liquid nitrogen from Dewar or liquid Nitrogen container (4), c) spraying the cryogenic pre-cooler through the liquid Nitrogen flow control system(5) combining with the product thereby cooling, d) embrittling uniform lattice on the product, which is then transported , controlled by the speed of the drive along with the cold gas generated by the evaporation of the liquid Nitrogen to the grinding mill (6,7), e) ensuring uniform lattice through immersing spices constituting spice mix powder in liquid Nitrogen with immersion periods ranging from 3 to 20 minutes, f) injecting liquid Nitrogen by simultaneous injection or spraying of liquid Nitrogen to the material as well as in the grinding zone of the mill with the time of liquid Nitrogen spraying ranging from 3 to 15 minutes, g) maintaining the temperature of cryogen between -20°C to -60°C, h) pulverizing, with the sensors monitoring the temperature of the grinding zone, with the digital signal processing system optimizing liquid Nitrogen spray through automatic feed back control, i) collecting finally ground product in a collecting bin (8). zone, with the digital signal processing system optimizing liquid Nitrogen spray through automatic feed back control, i) collecting finally ground product in a collecting bin (8). In an embodiment of the present invention conveying of the mixture of materials to the grinding mill is through the screw conveyed cryogenic pre-cooler having variable speed drive for capacity 10-150 kg/h, jacketed with an insulated top cover. In yet another embodiment of the present invention, conveying screw of the cryogenic pre-cooler is a fin or needle type hollow screw having provision to pass liquid nitrogen inside to spray on the spice, with a screw diameter ranging between 65 to 80 mm, length varying between 1 to 2 m, infeed size between 2 to10 mm driven by 1 to 2 h.p. variable speed motor gear box drive. In another embodiment of the present invention, spraying of liquid nitrogen in the cryogenic pre-cooler is from Dewar or liquid Nitrogen container with the pressure ranging between 1-4 kg/cm2 with the time of spraying on the material controlled by the speed of the drive. In still another embodiment of the present invention, cooling, embrittling of the product to ensure uniform lattice may be through immersing spices constituting spice mix powder in liquid Nitrogen with immersion periods ranging from 3 to 20 minutes or may be through direct injection or spraying of liquid Nitrogen on the material from the liquid Nitrogen flow control system in the cryogenic screw conveyed pre-cooler or by injecting liquid Nitrogen at the grinding zone of the mill or by simultaneous injection or spraying of liquid Nitrogen to the material as well as in the grinding zone of the mill with the time of liquid Nitrogen spraying ranging from 3 to 20 minutes, maintaining temperature of cryogen between -20° to - 60° C that combines with the product to be transported further along with the cold gas generated by the evaporation of the liquid Nitrogen. In an embodiment of the present invention, the process for the preparation of dry, fine, spice mix powders and the like of the present invention is shown in Fig. 2 of the drawings accompanying this specification. The novelty of the present invention with respect to prior art lies in: (i) higher retention of etheric oils of the composite mix (ii) prevention of oxidation and rancidity, in turn having a pasteurizing effect on different spices constituting spice mix. (iii) as an improved poultry feed that can impart meat and fat of the chicken an antibiotic action (iv) producing an inert atmosphere from the start to the end of milling, (v) providing inexpensive, dry and inert atmosphere of nitrogen for storage and package of the ground product, (vi) a convenient method for the production of curries of highly acceptable quality (vii) a spice mixture (including Garam Masala) powder for use in dehydrated mutton curries and the like with a desired flavor characteristics (viii) substantial increase in throughput and decrease in specific energy for grinding compared to conventional grinding, (ix) keeping oil and moisture in the product in the crystallized conditions during milling and avoids clogging and gumming of walls during grinding since chilling makes the product brittle. (x) producing uniform, finer particle sizes of the ground spice mix (including Garam Masala) (xi) eliminating speckling problems and reducing settling rate of spice mixture powders in liquid preparations, (xii) eliminating dust explosion and buildup of product during grinding of mixture of spices, (xiii) achieving size reduction in a single pass. The following examples are given by way of illustration of the present invention and therefore should not be construed to limit the scope of the present invention. EXAMPLE -1 In this example, data on grinding characteristics of spice mix powder obtained by the proposed process along with the quality and quantity of essential oil, particle size are given. The values are compared with and without water cooling process to show the viability of the process. Ten kg batch of mixture of spices constituting spice mix powder were ground using Hammer mill (Make:Cadmach Ahmedabad), having a provision for cold water circulation around the grinding zone. The percentage constituents of various spices of spice mix are given in Table 1. The circulation temperature of water during grinding was maintained at 4°C. A perforated round hole, woven wire mesh screen (Tylor series No.24) was used. Grinding operation was carried out with and without cold water circulation. The ground spice mix powder was packed and sealed immediately after grinding in aluminium foil-polythene laminate pouches and stored in the cold room at 4degree C for subsequent analysis. Representative samples in triplicate were taken after grinding. An indigenously made sampling glass tube was used to collect samples. The feed rate conditions were, 25 and 35 kg/h respectively for the proposed and conventional methods employed. The feed rate was varied using screw feeder for the conventional methods. The feed rate for cryogenic grinding was varied through a cryogenic pre-cooler which is of fin type hollow screw, having a diameter of 75 mm and length of 2 m driven by 2 h.p variable speed gear drive that has the provision of circulating around liquid nitrogen on the material. The pressure of liquid nitrogen through Dewar was maintained at 2 kg/cm2 and the period of spraying liquid nitrogen was 5 minutes and 10 minutes respectively. Sensory analysis on the ground powders was done by the 8 members sensory panel. Essential oil analysis and oleoresin estimation of ground samples were done using Clavenger's method and Cold column extraction by percolation method respectively. Toluene distillation method was used to analyze the moisture contents of ground powders. Gas Chromatographic analysis was carried out using Gas Chromatograph (Model Shimadzu - 15A). Essential oil samples were diluted 5 times with acetone and 1 jal was injected for the analysis. The results of all the analysis are presented in the form of tables (1-4) EXAMPLE - 2 In this example, data on grinding characteristics of spice mix powder obtained under different feed rates and temperatures by the proposed process along with the quality and quantity of essential oil, particle size are given. Ten kg batch of mixture of spices constituting spice mix powder were used. The percentage constituents of various spices of a typical spice mix popularly known as "Garam Masala" in India is given in Tablel. The ground powder was packed and sealed immediately after grinding in aluminium foil-polythene laminate pouches and stored in the cold room at 4 degree C for subsequent analysis. Representative samples in triplicate were taken after grinding. An indigenously made sampling glass tube was used to collect samples. The mixture of spices to be ground was filled into the vibratory feeder where it is metered at a specific rate into the cryogenic pre-cooler. In the cryogenic pre-cooler liquid Nitrogen is injected and combines with the product thereby cooling and embrittling the product. The product is then transported, along with the cold gas generated by the evaporation of liquid Nitrogen, to the grinding mill where it is pulverized and collected in the bin. Excessive cold gas is vented out. The feed rate conditions were: 15, 30 and 40 kg/h, respectively. The feed rates were varied through a cryogenic pre-cooler which is of fin type hollow screw, having a diameter of 75 mm and length of 2 m driven by 2 h.p variable speed gear drive that has the provision of circulating around liquid nitrogen on the material. The pressure of liquid nitrogen through Dewar was maintained at 2 kg/cm2 and the period of spraying liquid nitrogen were 3,15 and 20 minutes respectively. Sensory analysis on the ground powders was done by the 8 members sensory panel. Essential oil analysis and oleoresin estimation of ground samples were done using Clavenger's method and Cold column extraction by percolation method respectively. Toluene distillation method was used to analyze the moisture contents of ground powders. Gas Chromatographic analysis was carried out using Gas Chromatograph (Model Shimadzu - 15A). Essential oil samples were diluted 5 times with acetone and 1 |al was injected for the analysis. The results of all the analysis are presented in the form of tables (1-4) Table-1: Percentage constituents of spice mix powder Spices Percentage composition 1. Coriander 2. Cumin 3. Black pepper 4. Black cardamom 5. Cinnamon 6. Clove 7. Bay Leaves 8. Nut Meg 9. Turmeric 10. Red Chillies 11. Mace 12. Rock flower 13. Green cardamom 14.Anistar 15. Salt 20% 20% 3% 3% 4% 3% 3% 2% 9% 13% 3% 2% 5% 5% 5% Table-2 : Volatile and essential oil content analysis of spice mix Powder (Table Removed) S1 -S2 - Samples from the proposed process C1 - C2 - Samples obtained from without water cooling grinding C3 - C4 - Samples obtained from water cooled grinding Variance-0.19% Inference: Processed samples have more yield (ml/100g), finer particle size than the present ones Table-3 : Volatile and essential oil content analysis of spice mix Powder (Table Removed) • S1 -S3 - Samples from the proposed process • Variance-0.21% • Table-4: Total percentage concentration of essential oil samples of spice mix powder as determined by Gas chromatography (Table Removed) Inference: Better total concentration of fatty acids in the samples obtained from proposed process than the conventional ones Values shown in the tables 1-4 are the averages of three replications Sensory analysis: Sensory analysis revealed that proposed process samples attained higher ranks for major attributes of spice mix powder such as cumin, clove, cardamom, cinnamon, coriander, turmeric, harsh, bitter pungent and astringent as compared to the ones prepared under the with and without water cooled processes. There were no off-notes in all the types of samples. Profilogram of spice mix powder indicated distinct segregation of samples obtained from the proposed process as shown in fig 3. As it can be seen from the tables 1-4, as well from the sensory analysis that quality of spice mix powder obtained from the proposed process is better than the conventional methods (with and without cooling water) qualitatively and quantitatively. Also based on variance (0.19 - 0.26%) it can be confirmed that the analytical results are reproducible. Description of the accompanying drawings In Fig. 1 of the drawing accompanying this specification is schematic diagram of the device used for the present invention, has been shown. In the figure the various parts are, 1- Hopper, 2- Vibrating feeder, 3- Cryogenic pre-cooler, 4- Liquid Nitrogen container, 5- Liquid Nitrogen flow control system, 6- Grinding mill, 7- Mill motor, 8- Collecting bin Fig 2: is a schematic diagram of the process for the preparation of dry, fine, spice mix powders Fig 3: shows the profilogram of spice mix powder The main advantages of the present invention are: 1. development of an reproducible, suitable processing method for spice mixtures and its products to get the desired organoleptic characteristics 2. better retention of natural flavouring principles when compared to conventional methods 3. efficient size reduction, improve product flow, dispersion characteristics and throughtput 4. elimination of fire hazards and dust explosion 5. large potential for commercial exploitation and can be adopted for situations where stringent quality specifications are required 6. can be used as an improved poultry feed that can impart meat and fat of chicken an antibiotic action 7. can be used as a convenient method for the production of curries of highly acceptable quality 8. can be used in dehydrated mutton curries and the like with a desired flavor characteristics 9. takes lesser quantity of spice to generate the same flavor potency as opposed to conventionally milled spices, offering economic advantage We Claim: 1. An improved cryogenic process for the production of mixed spice powders using a device, shown in the figure (1) of the drawing accompanying the specification: a) transferring mixture of raw material to a filling hopper (1) of the device shown in figure (1), where from the mixture of spices to be ground enters the vibratory feeder (2), having provision for feed rate control, b) metering into screw conveyed cryogenic pre-cooler (3) driven by motor, reduction gear, inverter control, wherein liquid nitrogen from Dewar or liquid Nitrogen container (4), c) spraying the cryogenic pre-cooler through the liquid Nitrogen flow control system(5) combining with the product thereby cooling, d) embrittling uniform lattice on the product, which is then transported controlled by the speed of the drive along with the cold gas generated by the evaporation of the liquid Nitrogen to the grinding mill (6,7), e) ensuring uniform lattice through immersing spices constituting spice mix powder in liquid Nitrogen with immersion periods ranging from 3 to 20 minutes, f) injecting liquid Nitrogen by simultaneous injection or spraying of liquid Nitrogen to the material as well as in the grinding zone of the mill with the time of liquid Nitrogen spraying ranging from 3 to 15 minutes, g) maintaining the temperature of cryogen between -20°C to -60°C, h) pulverizing, with the sensors monitoring the temperature of the grinding zone, with the digital signal processing system optimizing liquid Nitrogen spray through automatic feed back control, i) collecting finally ground product in a collecting bin (8). 2. An improved cryogenic process as claimed in claim 1, wherein conveying of the material to the grinding mill is through the screw conveyed cryogenic pre-cooler having variable speed drive for capacity 10-150 kg/h, jacketed with an insulated top cover. 3. An improved cryogenic process as claimed in claims 1 & 2, wherein conveying screw of the cryogenic pre-cooler is a fin or needle type hollow screw having provision to pass liquid nitrogen inside to spray on the spice, with a screw diameter ranging between 65 to 80 mm, length varying between 1 to 2 m, infeed size between 2 to 10 mm driven by 1 to 2 h.p. variable speed motor gear box drive. 4. An improved cryogenic process as claimed in claims 1-3 wherein spraying of liquid nitrogen in the cryogenic pre-cooler is from Dewar or liquid Nitrogen container with the pressure ranging between 1 to 4 kg/cm2 with the time of spraying on the material controlled by the speed of the drive. 5. An improved cryogenic process as claimed in claims 1-4, wherein a device for producing dry, fine, spice mix powders, said device comprising: a) a filling hopper (1) for feeding mixture of spices to be ground, connected to a, b) vibratory feeder (2) having provision, feed rate control, into which the mixture of spices to be ground enters, and the said vibratory feeder connected to a, c) screw conveyed cryogenic pre-cooler (3) driven by motor, and having reduction gear, inverter control, into which the spice mixture is further metered and liquid nitrogen from a Dewar or liquid nitrogen container is sprayed in the cryogenic pre-cooler through the liquid Nitrogen flow control system (5), combining with the spice mixture cooling, embrittling and ensuring uniform lattice on the mixture, and the said pre cooler is connected to a, d) grinding mill (6,7) which pulverizes the mixture, and said mill having sensors monitoring the temperature of the grinding zone, with the digital signal processing system optimizing liquid Nitrogen spray through automatic feed back control, and the mill connected to a, e) collecting bin (8) to collect finally the ground product. 6. An improved cryogenic process for the production of mixed spice powders substantially as herein described with reference to the drawings and examples.

Documents:

331-del-2002-abstract.pdf

331-DEL-2002-Claims-(05-08-2008).pdf

331-del-2002-claims.pdf

331-DEL-2002-Correspondence-Others-(05-08-2008).pdf

331-del-2002-correspondence-others.pdf

331-del-2002-correspondence-po.pdf

331-del-2002-description (complete)-05-08-2008.pdf

331-del-2002-description (complete).pdf

331-del-2002-drawings.pdf

331-del-2002-form-1.pdf

331-del-2002-form-18.pdf

331-del-2002-form-2.pdf

331-del-2002-form-3.pdf

331-DEL-2002-Petition-137-(05-08-2008).pdf

3682-DEL-2002-Abstract-(25-08-2008).pdf

3682-DEL-2002-Claims-(25-08-2008).pdf

3682-DEL-2002-Description (Complete)-(25-08-2008).pdf

3682-DEL-2002-Form-2-(25-08-2008).pdf