RU2021992C1 - Method of gelatine production - Google Patents

Abstract

FIELD: medical industry. SUBSTANCE: method of gelatine production provides for maceration of bones grist, its cleansing, ossein treatment with ash, ash removal, boiling, broth concentration, gelatine drying. In the case, after cleaning they exercise additional drying, sterilization in UHF, grinding up to particles of 1.0 - 0.05 mm size and smaller. Maceration is carried out in hydrochloric acid solution of 0.5 - 2 % concentration with liquid factor of 40-120 during 5 - 40 minutes with continuous mixing. Ossein cleansing is carried out by water up to pH 5.0. Ash treatment is exercised with continuous mixing under solution temperature of 20 -35 C and liquid factor of not less than 10 during 30 minutes. Neutralization is carried out by hydrochloric acid of not less than 0.5 % concentration with its slow addition into solution until pH 5.0 is achieved with following separation of suspension. Last cleansing is exercised by distilled water. Boiling is carried out in distilled water by temperature fractions during 2 - 4 hours each. Cleaned broth is concentrated by inertial separation or by centrifuging. Drying is exercised by spraying under dryer outgoing gasses temperature of not less than 90 C. Produced powder of gelatine is granulated up to 2 - 3 mm granules by broth spraying on boiling layer of particles. EFFECT: method of gelatine production is used in medical industry. 1 dwg, 1 tbl

Description

 The invention relates to the production of gelatin and can be used in the food and chemical industries.

 A known method of producing gelatin [1], including the purification of collagen-containing raw materials, crushing, demineralization (maceration), washing and neutralizing, gritting, desoldering (washing from calcium, neutralization and washing final), extraction (cooking) of gelatin, cleaning broths, their evaporation, gelatinization and drying. The duration of the technological processes of the method reaches 60 days or more. To accelerate individual stages, several methods are proposed.

 In a method for preparing collagen-containing raw materials for gelatin production [2] to accelerate the process of ashing, it is proposed that calcium hydroxide treatment in the second stage be carried out in the presence of 10-15 g / l sodium sulfite or sodium carbonate. The duration of ashing is reduced by 7-10 times, i.e. up to 6 days.

 In the method for processing wool collagen-containing raw materials [3] it is proposed, after crushing the raw material, to process it with sodium hydroxide of 15-16% concentration for 2-2.5 hours.

 In the method for the production of gelatin and similar products [4], in order to accelerate the process of extracting gluten from raw materials, it was proposed to heat the raw materials with steam, grind the raw materials to 5-10 mm, and use a centrifuge to separate the liquid, the processing time is 20 s.

The method of cooking food broths from bone [5] in order to intensify the process of boiling proposed to implement it in an autoclave at a temperature of 125-130 ^C and a pressure of 0.25-0.35 MPa, and the particles are pulverized to a size of 3-5 mm and processing is carried out in a microwave field.

 In the method for the production of glue and gelatin from gelatin wastes, it is proposed to carry out acid treatment with a solution of 13-15% hydrochloric acid.

 Closest to the invention is a method [6], including purification of collagen-containing raw materials, crushing to particle sizes of 20-50 mm, demineralization (maceration) in a 5-7% solution of hydrochloric acid for 5-10 days at a liquid ratio of about 10, washing, neutralization, galling in a lime solution for 30-60 days with a liquid coefficient of 1-1.5 with periodic stirring with air and with a change of solution 3-4 times, desalination for 20-25 hours (washing from lime, neutralization and final washing to pH 5.8-6.2), extraction (cooking) elatina fractions from the temperature for 6-7 h each fraction, preserving broth preservative additives (e.g., sulfur dioxide), with hydrogen peroxide bleaching, filtering broths, evaporation broths, gelatinization and drying the jelly.

 According to this method, it is difficult to achieve a significant increase in the speeds of individual processes, since particles of large sizes of 20-50 mm are used in the processing. A significant increase in the speed of processes is possible only when crushing particles to sizes of the order of 1.0 mm or less.

The essence of the invention lies in the fact that to speed up the preparation of collagen-containing raw materials, improve the quality of the final product, increase the yield of gelatin from the raw material, the purified meal is crushed to particle sizes of 1.0-0.05 mm or less, the meal is pre-dried and sterilized in a microwave field , maceration is carried out in a solution of 0.5-2.0% hydrochloric acid with continuous vigorous stirring, with a liquid coefficient of 40-120 for 5-40 minutes, the separation of ossein from the solution is carried out, for example, by filtration on synthetic tissues with a cell 30 microns, ossein washing with water is carried out to pH 5 or more, the separation is carried out solid part, liming is carried out in a lime solution at a pH of at least 12, with continuous vigorous stirring at 20-35 ^{° C} and a solution liquid ratio of at least 10 for 0, 5-3,0 hours. Carry one perezolku at a temperature of 10-20 ^{° C} for 0.5 hours, after liming is carried out by gradual addition of weak neutralization, e.g., 0.5% hydrochloric acid to a pH not lower than 5. separated from the collagen solution by filtration.

Then, washing is performed in two stages - one tap water, distilled another to pH 5,8-6,2, separation is carried out, cooking is carried out with distilled or demineralized water at a ratio of 1.5-2 liquid fractions from the temperature, e.g., at ⁶⁰ C, 65, 70, 85, 100 ^about With continuous stirring. The gelatin solution is separated from the residue, then the broths are cleaned, the broths are concentrated, for example, by inertial separation (centrifugation) to a gelatin concentration of 10-20%, drying is carried out, for example, by spraying. Gelatin powder is granulated to a granule size of 2-3 mm, for example, by coarse spraying of the initial broth into a fluidized bed in a granulator dryer with the output of medium strength granules and instant ones in water.

 The feedstock (meal) with a particle size of 0.05 mm is difficult to separate by filtration, especially in the processes of ash and cooking, therefore, the separation of solid particles with a size of less than 0.05 mm from liquids is carried out by centrifugation.

 Salient features of the claimed object from the prototype are the use of ground meal to sizes of 1.0-0.05 mm and less and an acid concentration of 0.5-2%, the use of drying - sterilization of meal, cooking in purified water, the use of inertial concentration of the broth, drying spray broth followed by granulation.

 Fine grinding of the initial product allows hundreds of times to accelerate the processes of maceration, gritting, neutralization and washing, while the material is processed more evenly to the depth of the particles and more fully, which ensures an increase in the yield of gelatin from the feedstock by a factor of 1.5, and an increase in gelatin quality indicators (jelly viscosity, strength, sterility and chemical purity).

 The drawing shows a graph explaining the method.

 The maximum particle size at which a significant increase in the speed of the chemical process is achieved due to crushing, i.e. the increase in the reaction surface of the particle layer is determined by the dependence of the specific surface on the particle size. Since the speed of the heterogeneous reaction is proportional to the surface of the layer, and the surface size begins to increase significantly with a decrease in the particle size of the fraction to tenths of a millimeter, the maximum size is taken to be about 0.63-1.0 mm. With these sizes, mass transfer processes inside the particles are also significantly accelerated. The minimum size is taken based on the technical capabilities of the filtration separation of solid and liquid fractions, obtained experimentally about 0.05 mm, or is not limited when using separation in a centrifuge.

 The maximum concentration of hydrochloric acid in the initial solution during maceration is determined experimentally by the degree of color change (darkening) of ossein: for small particles - about 0.5% HCl, for large - up to 2% HCl. In this case, the liquid coefficient is selected on the basis of stoichiometric ratios of chemical reactions, for example, assuming that the meal contains about 75 wt.% Of the mineral part. The lower the concentration of the solution, the greater the liquid coefficient.

 The time of arrival of particles in the reactor is determined experimentally. From this time it is necessary to exclude the time of pumping the suspension to the filter and the residence time of particles in solution during filtration.

 The time of ashes is determined experimentally.

 PRI me R 1. Wet purified meal obtained by a known method, dried and sterilized in a microwave drum dryer. Dry sterilized meal is crushed in a hammer mill to a particle size of less than 1.0 mm and a fraction, for example, 0.63-0.315 mm, is sieved. Maceration is carried out with continuous vigorous stirring of a 2% HCl solution at a liquid coefficient of 40 for about 20 minutes.

The end of the process is determined by the absence of calcium in the particles after washing. The suspension is filtered through a mesh with a mesh size of, for example, 0.1 mm. Washing is carried out with water with continuous stirring to pH 5. The washed ossein is separated by filtration on a mesh. Liming is carried out in lime solution pH 12 with continuous stirring at a liquid ratio of at least 10 at a temperature of 30-35 ^{° C} for one hour with perezolkoy at a temperature of 10-20 ^{° C} for 0.5 hours.

 After zoleniya carry out washing, replacing the solution by decantation. At pH 8, neutralization is carried out with a 0.5% solution, pH 5. Separation of the suspension is carried out by filtration on a grid. Then the particles are washed to pH 6.0 with cold tap water and, for the last time, with distilled or chemically purified water to a pH of 5.8-6.2. The solid part is separated by filtration and sent to cooking (gelatin extraction), which is carried out by temperature fractions for 3 hours, each fraction. Next, the broth is cleaned by known methods.

Sterilization is not required if the room was clean. Drying of the gelatin is performed in a spray dryer at a temperature of gas entering the dryer is not more than 350 ^{° C} and at the outlet of the dryer is not more than 90 ^C. The granulation is carried out starting gelatin powder spray broth into the fluidized bed of particles with the output of granule size 2-3 mm average strength quickly soluble in water.

 PRI me R 2. The cleaned meal is dried, sterilized in a microwave field, crushed and dispersed by screening. The fraction remaining after scattering (less than 0.05 mm) of the particles of the dry sterilized meal is directed to maceration in a solution of hydrochloric acid, with a concentration of 0.5% with a liquid coefficient of at least 120, with continuous vigorous stirring. The residence time of the meal in acid is short compared with the time of mixing the acid solution and the meal. Mixing can be accelerated, for example, by crushing the lumps with a wide stream of water directed to the surface of the suspension. Maceration time is about one minute. Ossein is separated by centrifugation. Washing is carried out in water with continuous vigorous stirring to pH 5.

Washed ossein is separated by centrifugation. Liming is carried out in a lime solution at a pH of 12 with continuous vigorous stirring at 25-30 ° ^C at a liquid ratio of at least 20 within 20 minutes.

 In milk of lime, there should be no particles larger than 0.05 mm. Refilling is carried out in cold water, then washing with cold water is carried out to pH 6 and the last time is clean. In this case, the separation of the suspension is carried out by centrifugation or decantation, the use of which allows you to more fully wash ossein from ballast insoluble proteins. Centrifugation reduces product losses, but increases its turbidity. Cooking and subsequent processes are carried out in the same way as in example 1, using separation only by centrifugation.

 Other examples are presented in the table and differ from examples 1, 2 only in regime parameters given in the table.

 From the above examples, it is seen that when using finely dispersed meal according to the proposed technology, the residence time in the process of maceration and ashing is reduced by hundreds of times compared with the prototype. When processing raw materials in the form of a suspension, intensive mixing with a stirrer is possible (in the prototype, with air), which allows for deep and uniform processing of raw materials and, therefore, to improve the quality of the final product. The processes are greatly simplified. Such processes can be mechanized and automated.

Claims (1)

METHOD FOR PRODUCING ZHELATIN, including maceration of bone meal, washing, ossein golding, cooking, concentration of broth, drying gelatin, characterized in that the meal is pre-dried, sterilized by microwave, crushed to particle sizes of 1.0 - 0.05 mm or less, maceration is carried out in a solution of hydrochloric acid with a concentration of 0.5 - 2% with a liquid coefficient of 40 - 120 for 5 to 40 minutes with continuous stirring, washing ossein is carried out with water to a pH of 5.0, the granulation is carried out with continuous stirring at a solution temperature of 20 - 35 ^o C and liquid coe coefficient of not less than 10 for 0.5 - 3.0 hours with a perezolkoy at a temperature 10 - 20 ^o C for 30 min, the neutralization is carried out with hydrochloric acid at a concentration of not more than 0.5% with a gradual addition of its solution to pH 5 , 0 followed by separation of the suspension, the last washing is carried out with distilled water, the cooking is carried out in distilled water by temperature fractions for 2 to 4 hours, each fraction, the purified broth is concentrated by inertial separation or centrifugation, drying is carried out by spraying at a temperature of gases at the exit of the land sludge not more than 90 ^o C, the resulting gelatin powder is granulated to 2 to 3 mm, spraying the original broth into it in a fluidized bed of particles.

Images