RU2679884C1 - Method of obtaining keratin monoproduct (options) - Google Patents

Abstract

FIELD: processing and recycling of waste.SUBSTANCE: invention relates to the field of processing animal waste to obtain a keratin monoproduct intended for use in veterinary medicine, medicine, cosmetology, biotechnology, food industry, and also as a protein feed additive to the basic diet of animals and birds. In both variants of the implementation of the original keratin-containing material is soaked for 4–6 h in a solution containing 1.0–7 % hydrochloric acid and 0.1–0.3 % hydrogen peroxide when the LR liquid ratio of 12–15, followed by washing with deionized water to neutral pH values, spend from 1 to 4 consecutive processing cycles, each of which is a treatment of keratin-containing semi-finished product in a solution containing 0.05–2.5 % sodium hydroxide and 0.1–1.0 % hydrogen peroxide for 8–12 hours at a temperature of 28–32 °C at LR from 6 to 10, precipitating keratin from the reaction mixture for 0.5–1.0 h with 7–10 % hydrochloric acid and rinsing the precipitate with deionized water until neutral pH. To obtain a liquid keratin monoproduct (in the first embodiment), upon completion of the treatment cycles, the product purified from non-keratic impurities is redissolved in 0.1–1.0 % sodium hydroxide solution for 4–6 h, at occasional stirring, homogenized to a particle size of 180–220 microns and filtered, and then its pH is stabilized to 6.7–7.3 using a 0.1–1.0 % solution of sodium hydroxide and bring the dry residue to 3.0–15.0 % using the same solution, to obtain a monoproduct containing 95–98 % keratin, to which a preservative is added before packaging. To obtain the dry form of the keratin monoproduct (according to the second variant), after the completion of the treatment cycles, the sediment purified from impurities is redissolved in 0.1–1.0 % sodium hydroxide solution, keeping it for 4–6 hours at periodic stirring, a preservative is added and the resulting volume of product is poured into cuvettes to a layer thickness of 1–2 cm. Product is then lyophilized using stepwise dehydration in the range of cryoscopic temperatures from -30 to -60 °C for 24–36 h, bringing the moisture content in the product to 0.5–5.0 %, then the product is gradually heated to a temperature of up to 10–20 °C and crushed to a powder with a particle size of 1–3 mm, and then packed.EFFECT: improvement of technological processes made it possible to increase the solubility of the initial keratin-containing raw materials and increase the yield of native keratin to 95–98 wt% with a mass fraction of dry substances in monoproduct 5–15 wt%, id est ensure the achievement of the technical result – the possibility of obtaining a single product with a high environmental friendliness of its production.2 cl, 2 ex

Description

The invention relates to the field of processing animal waste to produce a keratin single product intended for use in veterinary medicine, cosmetology, biotechnology, as well as a protein feed additive to the main diet of animals and birds.

Known methods for producing keratin-containing products, for example, molecularly soluble keratin (RF 2113225 A61K 35/36, 1995), protein feed additives from waste from the wool industry (RF 2105495, A23K 1/10, 1994) - hair straightening agents . However, some of the proposed technologies require the use of expensive reagents in high concentrations, while others lead to the complete hydrolysis of keratin and, accordingly, the loss of biological activity inherent in native keratin.

Closest to the invention in both variants of its implementation is a method for producing keratin (RF 2092072, A23K 1/10, 1995), which includes a series of sequential operations during which the feedstock is first treated with a mixture of formic acid and an oxidizing agent, and after washing, Sodium hydroxide and an oxidizing agent are added to the obtained semi-finished product, the resulting precipitate is dialyzed, then redissolved in a slightly alkaline medium and a preservative is added, after which the target product is homogenized and filtered. The advantage of this method is a more advanced method of fiberization of the fibrillar structure of keratin, facilitating the process of subsequent dissolution of the protein. However, due to the use of several types of acids (hydrochloric, acetic and formic) in the technological cycle, a large number of different salts are formed in working solutions, which inhibits the dissolution of fibrillar keratin and increases the amount of undissolved keratin, and, naturally, the amount of waste, which negatively affects ecology. In addition, using the known method, it is practically impossible to obtain a single product (with a high percentage of keratin content), which, due to its properties and quality indicators, is most in demand in the modern consumer market.

The technical result that can be achieved in both variants of the invention is the possibility of obtaining a single product with high environmental friendliness of its production.

The technical result according to the first embodiment of the invention is achieved by the fact that in the method for producing a keratin mono product, the initial keratin-containing material is treated for 4-6 hours with a solution containing 1.0-7% hydrochloric acid and 0.1-0, 3% hydrogen peroxide with a liquid coefficient (LC) of 12-15, followed by washing with deionized water to neutral pH values, after which 1 to 4 consecutive treatment cycles are carried out, which include exposure to the keratin-containing semi-finished product for 8-12 h. at a temperature of 28-32 ° C with a solution containing 0.05-2.5% sodium hydroxide and 0.1-1.0% hydrogen peroxide with an FA of 6 to 10, purification of the semi-finished product by precipitation of keratin from the reaction mixture for 0, 5-1.0 hours with 7-10% hydrochloric acid and washing the precipitated keratin with deionized water to neutral pH values; upon completion of the treatment cycles, the product purified from non-keratinic impurities is redissolved in a 0.1-1.0% sodium hydroxide solution for 4 -6 hours periodically mixing, homogenize to a particle size of 180-220 microns and filter, and then stabilize its pH to 6.7-7.3 using a 0.1-1.0% sodium hydroxide solution and adjust the solids content to 3.0-15.0% using the same solution, obtaining a single product containing 95- 98% keratin, to which a preservative is added before packaging.

The technical result according to the second embodiment of the invention is achieved by the fact that in the method for producing a keratin mono product, the initial keratin-containing material is treated for 4-6 hours with a solution containing 1.0-7% hydrochloric acid and 0.1-0, 3% hydrogen peroxide with a liquid coefficient (LC) of 12-15, followed by washing with deionized water to neutral pH values, after which 1 to 4 consecutive treatment cycles are carried out, which include exposure to the keratin-containing semi-finished product for 8-12 h. at a temperature of 28-32 ° C with a solution containing 0.05-2.5% sodium hydroxide and 0.1-1.0% hydrogen peroxide with an FA of 6 to 10, purification of the semi-finished product by precipitation of keratin from the reaction mixture for 0, 5-1.0 hours with 7-10% hydrochloric acid and washing the precipitated keratin with deionized water to neutral pH values; upon completion of the treatment cycles, the product purified from impurities is redissolved in a 0.1-1.0% sodium hydroxide solution for 4- 6 hours with periodic stirring, resulting in a single product containing 95-98% keratin, in which they preserve the preservative, and the resulting volume is poured into cuvettes to a layer thickness of 1-2 cm and subjected to lyophilization, with stepwise dehydration in the range of cryoscopic temperatures from -30 to -60 ° C for 24-36 hours, bringing the moisture content in the single product to 0 5 - 5.0%, after which it is gradually heated to a temperature of 10-20 ° C and ground to a powder state with a particle size of 1-3 mm, and then packaged.

The first option allows you to get a liquid keratin monoproduct, suitable for use in veterinary medicine, medicine, pharmaceutical and cosmetic industries.

The second embodiment of the invention allows to obtain a dry keratin monosubstance suitable for use as a protein supplement to animal feed and agricultural products. poultry, as well as in the food industry.

Both options are united by a single technical concept aimed at achieving the same technical result - the possibility of obtaining a keratin mono product with high environmental friendliness of production. The technical result is achieved using identical technical means: acid-peroxide treatment, which allows you to clean the original keratin-containing raw materials from non-keratin components and carry out their disinfection, as well as a series of peroxide-alkaline and acid treatments, during which both the degreasing of the starting materials take place, so and processes of gentle stepwise solubilization of fibrous keratin due to cascade cleavage of intermolecular disulfide and peptide bonds, are responsible for the quaternary structure of the biopolymer, the bioactive substance to a condition which is a keratin monoproduct undisturbed triple helix molecule structure.

The analyzed sources did not find information about the possibility of obtaining a single product with high environmental friendliness of its production using the selected set of sequential operations, accompanied by new temperature and time modes, as well as the choice of new concentrations of processing ingredients, which allows us to conclude that this technical solution meets the eligibility criteria.

The method is as follows.

As the initial raw material can be used tow of sheep wool, fur tow, hair of reindeer, feather of a bird, horned hoofed raw materials and other secondary keratin-containing resources.

Depending on the type of raw materials used, the temperature and time modes of the processes are selected, as well as the initial concentration of the ingredients used (within the specified ranges).

The initial keratin-containing material (raw material) is soaked for 4-6 hours in a solution containing 1.0-7% hydrochloric acid and 0.1-0.3% hydrogen peroxide with a liquid ratio of LC 12-15, followed by washing with deionized water to neutral pH values. From 1 to 4 consecutive treatment cycles are carried out, each of which is a treatment of a keratin-containing semi-finished product in a solution containing 0.05-2.5% sodium hydroxide and 0.1-1.0% hydrogen peroxide, for 8-12 hours. at a temperature of 28-32 ° C with an FA from 6 to 10, precipitation of the main component (keratin) from the reaction mixture for 0.5-1.0 hours using 7-10% hydrochloric acid and washing the precipitate with deionized water to neutral pH values . Rinsing the precipitate with deionized water to neutral pH values eliminates the need for dialysis and, therefore, increases the manufacturability of production.

At the end of the treatment cycles, the product purified from non-keratinic impurities is redissolved in a 0.1-1.0% sodium hydroxide solution for 4-6 hours, stirring periodically, homogenized to a particle size of 180-220 microns and filtered, and then stabilize its pH to 6, 7-7.3 using a 0.1-1.0% sodium hydroxide solution and adjust the solids content to 3.0-15.0% using the same solution. As a result, a single product is obtained containing 95-98% keratin, into which a preservative is added before packaging.

To obtain a dry form of keratin monoproduct at the end of processing cycles, (including, as in the preparation of the liquid fraction, exposure to the semifinished product with sodium hydroxide and hydrogen peroxide, purification with hydrochloric acid and washing), the precipitate purified from impurities is redissolved in 0.1-1 , A 0% solution of sodium hydroxide, keeping it for 4-6 hours with periodic stirring, add a preservative and the resulting product volume is poured into cuvettes to a layer thickness of 1-2 cm. Then the product is subjected to lyophilization (sublimation drying), using stepwise dehydration in the range of cryoscopic temperatures from -30 to -60 ° C for 24-36 hours, bringing the moisture content in the product to 0.5-5.0%.

After drying (which can be done using, for example, a vacuum sublimation unit UVS-80M), the product is gradually heated to a temperature of 10-20 ° C and crushed (for example, using ball mills) to a powdery state with a particle size of 1-3 mm, and then packaged.

Example 1 (obtaining keratin monoproduct according to the first embodiment).

1. Soaking 1 kg of the initial keratin-containing raw material (tow of sheep’s wool) in a working solution containing 3.0% hydrochloric acid and 0.2% hydrogen peroxide for 5 hours at a liquid coefficient (LC) of 1:15 at 25 ° FROM.

2. Rinsing with deionized water to neutral pH values.

3. A double cycle of processing a keratin-containing semi-finished product by exposing it to a solution containing 1.0% sodium hydroxide and 0.3% hydrogen peroxide at LC 8 for 9 hours at 30 ° C, followed by precipitation of the main component (solubilized keratin) from the reaction mixture using 8% hydrochloric acid for 0.5 hours and washing the precipitate with deionized water to neutral pH values.

4. Reconstitution of monoproduct purified from impurities (97% keratin) in a 0.5% sodium hydroxide solution for 5 hours with periodic stirring.

5. Homogenization of the finished monoproduct to a particle size of 200 microns, filtering.

6. Bringing the mass fraction of solids in the finished single product to 5% and stabilizing the pH to 7.25 using a 0.5% sodium hydroxide solution.

7. Adding a preservative.

8. Bottling and labeling.

Example 2 (obtaining keratin monoproduct according to the second option).

1. Soaking 1 kg of the original keratin-containing raw materials (crushed feather) in a working solution containing 5.0% hydrochloric acid and 0.3% hydrogen peroxide for 6 hours at a liquid ratio (LC) of 1:12 at 25 ° C .

2. Rinsing with deionized water to neutral pH values.

3. Three-time treatment of the keratin-containing semi-finished product by exposure to it with a solution containing 1.5% sodium hydroxide and 0.5% hydrogen peroxide at LC 8 for 9 hours at 30 ° C, purification of the main component (solubilized keratin), its deposition from the reaction mixture using 8% hydrochloric acid for 0.5 hours and washing the precipitate with deionized water to neutral pH values.

4. Reconstitution of the monoproduct purified from impurities (98% keratin) in a 0.5% sodium hydroxide solution for 5 hours with periodic stirring.

5. Adding a preservative.

6. Pouring into cuvettes with a layer thickness of 1-2 cm.

7. Freeze-drying for 30 hours to a temperature of -40 ° C in the thickness of the material and the content of the mass fraction of moisture in the product of 5.0%

8. Raising the temperature of the single product to 20 ° C.

9. Grinding it (in a ball mill) to a particle size of 1-3 mm.

10. Packing and labeling.

Thus, the improvement of technological processes made it possible to increase the solubility of the initial keratin-containing raw materials and to ensure the yield of native (biologically active) keratin from 50-70 by a known method to 95-98 wt. % of the proposed and, accordingly, the mass fraction of solids in the single product of 5-15 wt. %, i.e. to provide the possibility of obtaining a single product with high environmental friendliness of its production.

This method can be used to obtain both powdered and liquid high-quality keratin-containing substances intended for use in veterinary medicine, medicine, cosmetology, biotechnology, feed production and the food industry.

Claims (2)

1. A method of obtaining a keratin monoproduct, which consists in the fact that the initial keratin-containing material is treated for 4-6 hours with a solution containing 1.0-7% hydrochloric acid and 0.1-0.3% hydrogen peroxide at a liquid coefficient (LC) 12-15 followed by washing with deionized water to neutral pH values, after which 1 to 4 consecutive treatment cycles are carried out, providing for exposure of the keratin-containing semi-finished product for 8-12 hours at a temperature of 28-32 ° С with a solution containing 0.05-2 5% sodium hydroxide and 0.1-1.0% p hydrogen oxide at LC from 6 to 10, purification of the semi-finished product by precipitation of keratin from the reaction mixture for 0.5-1.0 hours with 7-10% hydrochloric acid and washing of precipitated keratin with deionized water to neutral pH values, after completion of the treatment cycles The product purified from non-keratinic impurities is redissolved in a 0.1-1.0% sodium hydroxide solution for 4-6 hours, stirring periodically, homogenized to a particle size of 180-220 microns and filtered, and then stabilize its pH to 6.7-7 3 using 0.1-1.0% sodium hydroxide solution and up to lead the solids content to 3.0-15.0% using the same solution, obtaining a single product containing 95-98% keratin, to which a preservative is added before packing. 2. A method of obtaining a keratin monoproduct, which consists in the fact that the initial keratin-containing material is treated for 4-6 hours with a solution containing 1.0-7% hydrochloric acid and 0.1-0.3% hydrogen peroxide with a liquid coefficient (LC) 12-15 followed by washing with deionized water to neutral pH values, after which 1 to 4 consecutive treatment cycles are carried out, providing for exposure of the keratin-containing semi-finished product for 8-12 hours at a temperature of 28-32 ° С with a solution containing 0.05-2 5% sodium hydroxide and 0.1-1.0% p hydrogen oxide at LC from 6 to 10, purification of the semi-finished product by precipitation of keratin from the reaction mixture for 0.5-1.0 hours with 7-10% hydrochloric acid and washing of precipitated keratin with deionized water to neutral pH values, after completion of the treatment cycles the product purified from impurities is redissolved in a 0.1-1.0% sodium hydroxide solution for 4-6 hours with periodic stirring, resulting in a single product containing 95-98% keratin, to which a preservative is added, and the resulting volume is poured into cuvettes to a layer thickness of 1-2 cm and lyophilized, with stepwise dehydration in the range of cryoscopic temperatures from -30 to - 60 ° C for 24-36 hours, bringing the moisture content in the single product to 0.5-5.0%, after which it is gradually heated to a temperature of 10 -20 ° C and crushed to a powder state with a particle size of 1-3 mm, and then packaged.