A method of obtaining a collagen containing material

 

(57) Abstract:

The essence of the invention: redoubling tannery waste prepared collagen solution, of tanned leather waste paste with a particle size of solids of 0.2-0.6 mm Solution and the paste is mixed for 1-5 hours at a temperature of not higher than 15°C until a homogeneous mass having a 0.1 to 2 wt. % nedubrovo collagen, 0.3 to 10 wt.% tanned collagen and pH of 2.6 to 5.0. The mass is filtered to the size of the constituent particles of 0.2-0.6 mm, cooled to a temperature of 0-5°C, add a crosslinking agent in the amount of 0.15-7.0 wt.% and homogenize the mixture at a temperature not exceeding 5°C. Produce freezing, in which the temperature of the mixture reduced from minus 14 to minus 75°C for 0.1 to 2.0 hours and kept in a frozen state at a temperature of from minus 2 to minus 20°C for 4-24 hours Later produce defrosting and the extract obtained polymer material in air at room temperature in a moist condition without load within 6-12 h, heating to 85-105°C, cooling to room temperature, treatment of alkali-salt solution at pH 9-10 for 10-20 min and the drying to a residual moisture content of 30-40% . Then the material is subjected to hot pressing and subsequent vyd vergnet additional leather processing. 1 C.p. f-crystals.

The invention relates to methods of producing high molecular weight products from collagen containing materials and can be used in light industry in the manufacture of leather imitation material used for the manufacture of leather goods and shoes, and in the manufacture of finishing material used in construction, transport, furniture production.

A method of obtaining collagen containing semifinished product in the form of the collagen solution [1] . In accordance with this method the original leather raw material is subjected to mechanical and chemical processing, which get a lot with a soft collagen and partially finished collagenolytic proteins. The resulting mass is frozen at a temperature of from minus 10 to minus 30oC within 1-2 days and kept frozen mass within 1-2 days, than provide a seal fibers. After defrosting perform the final processing of the mass, providing training of the obtained semi-finished product for subsequent use.

There is a method allows to obtain collagen prefabricated only in the form of a solution and may not be used for procedurial, including grinding nedubrovo collagen containing raw material, preparation of collagen solution, homogenization, introduction to the obtained collagen mass of a crosslinking agent, homogenization, freezing, keeping in a frozen state at a temperature of from minus 2 to minus 20aboutWith the release and extraction of the resulting material [2].

This method allows to obtain a collagen containing material in the form valocordinum membranes or spongy layers for application in medicine and cannot be used to produce leather imitation materials.

The aim of the invention is to provide a collagen containing prefabricated polymer structures with high physical-mechanical properties.

For this purpose, the quality of raw hides used nedobity tannery waste, of which prepare the collagen solution, and tanned leather waste, of which prepare the paste with a particle size of solids is not more than 0.6 mm, the solution and the paste is mixed for 1 to 5 hours at a temperature not exceeding 15aboutTo obtain a homogeneous mass having a 0.1 to 2 wt. % nedubrovo collagen, 0.3 to 10 wt.% tanned collagen and pH of 2.6-5. The mass is filtered to razmera in the amount of 0.15-7.0 wt.% and homogenize the mixture at a temperature of not higher than 5aboutC. and Then produce a freeze, in which the temperature of the mixture reduced to a temperature range from minus 14 to minus 75aboutC for 0.1 to 2 hours and kept in a frozen state at a temperature of from minus 2 to minus 20aboutC for 4-24 hours Final processing after thawing produced by extracts obtained polymerized material in air at room temperature in a moist condition without load within 6-12 h post-heat until 35-105aboutC for from 1 min to 1 h, cooling to room temperature, the treatment of alkali-salt solution with a pH of 9-10 in 10-20 min, pressed to a residual moisture content of 30-40%, hot pressing and subsequent exposure to air without load within 12-24 hours

To the resulting intermediate product had a leather imitation view, it is possible to conduct additional leather processing, which, given the properties of the obtained semi-finished product is as follows: aged in air, the material is washed with water at 50-60aboutTo achieve the pH of the slice of material 4,2-4,4, squeeze handle at a temperature of 50aboutWith neutralizing emulsion that includes pasta VNIIG, acetate or formate, sodium and dispersal is 50oC dye when the consumption of the last 1-5% by weight of semi-finished greasing solution emulsion at the rate of fat 8-10% by weight of semi-finished product (in terms of 100% fat), press, doublenaut solution of a tanning agent containing 4-10% tanning resins, 1-5% resistant to electrolytes synthetic fat, 4-10% synthetic tanning agent, 2-6% of the extract of Mimosa and 1-4% neutralizing substances, squeezed to a moisture content of 30-40% , maintain the material in the air within 12-24 hours, after which produce a circular centrifuge with moisture at a temperature of 50aboutC. the resulting material is subjected to finishing processing.

In the process of implementation of the proposed method at the stage of mixing of the solution based on redoubling tannery waste and pastes on the basis of the tanned leather waste only offer the particle size of the paste (0.2-0.6 mm) and the proposed parameters of the mixing process (temperature and time) provide the required for further processing of the homogeneity of the mixture. Introducing into the mixture a cross-linking agent makes it reactive. The amount of cross-linking agent is available in a fairly wide range, and determines a wide range of properties and appearance of the obtained material.

When the amount of crosslinking agent in accordance with the lower limit of 0.15 wt. % ) will result in a very soft, gentle sponge. At the maximum proposed amount of crosslinking agent will be more dense mA its appearance is connected and the choice of the particle mixture (0.2-0.6 mm). Larger particles result in a coarse granular material, as they allow the process of homogenization only for a very limited time because of the stratification of the mass of the large particles. The resulting mass is distributed on the substrate layer, the thickness of which depends on the required qualities of the resulting product. The substrate can be used pallet, the endless belt form.

When freezing is first made by deep cooling, in which a chemical reaction is practically absent, and are formed only ice crystals, the size of which depends on the speed of freezing (at higher speeds to freeze the crystals are smaller). Ice crystals in the subsequent determine the presence of pores in the material, the dimensions of which depend on the size of the crystals.

The proposed mode freeze is set for the previously agreed upon mixture and allows you to get on its basis material with a wide range of porosity, which can be obtained with many types of the final product. If the shutter speed is in a frozen state within 4-24 hours at a temperature of from minus 2 to minus 20aboutWith chemical reaction occurs, the speed of the CT concentration of the reactants.

The proposed freeze mode set based on the properties of the proposed mixture, provides the passage of the polymerization reaction as much as possible, which further defines the qualities of the final produced product.

The resulting polymer material after defrost is washed to remove residual unreacted and are not included in the structure of the material substances. Exposure of the material in the wet state on a flat surface with no load at room temperature provides relaxation and subsequent heating, leading to the folding of the protein, which has not entered into reaction, makes the resulting material is capable of further leather processing and increases the strength of the resulting material. The selected heating mode is optimal when processing the proposed method. Leaching of alkali-salt solution will neutralize the acetic acid remaining in the material as a result of chemical exposure on raw hides at the initial stage of its processing.

The proposed limits of acidity of the solution set of conditions optimum speed of the neutralization process and exceptions destructive influence on the structure of the material. impact on the appearance and properties of the final product. After pressing the semi-finished product is kept on the air without load within 12-24 hours After this material may be folded and sent to the warehouse for storage or subjected to further processing, making him koreabridge species. This processing has the distinctive modes from generally accepted in the leather processing in connection with the characteristics of the treated intermediate product.

P R I m e R 1. The hide of cattle (cattle) or Goleva scraps AWG obtained when contribuye of the hide, washed in running tap water for 0.5-1 teaspoon Crushed ice 20 kg of the hide of cattle in a meat grinder with the diameter of the holes of the lattice of 0.16-2 mm Crushed raw materials are treated at room conditions for 4 hours 5-10% solution of sodium chloride, washed with water, treated with pepsin 0,03-0,05 units of activity/ml in volume ratio of 3-4 and temperature 20-25aboutC for 2-3 days.

Then the hide was processed with sodium hydroxide solution of 0.1 to 1.0 H for at least 24 h at a temperature of 15-20aboutC, washed with running water and freeze at temperatures below minus 30aboutWith at least 1 day and then defroster. Fibrous particles of collagen after devastati is the target of acetic acid. The resulting solution has a pH of 2.5 to 4.0, characteristic viscosity 10-20 DL/g, the denaturation temperature of 35-40aboutC. Chrome leather shavings in the amount of 120 kg is mixed with water and ground to a particle size of not more than 0.6 mm, the dry matter content in the obtained paste 1-10%.

A solution of collagen and pasta are mixed and homogenized at a temperature not exceeding 15aboutC for 2-3 h, filtered in filter presses with a cell size of 0.2-0.6 mm and cooled to a temperature of 0-5aboutTo add a crosslinking agent, such as glutaric aldehyde, in the amount of 0.5-0.75 wt.%. The mixture is again homogenized, spread evenly 10-12 mm on a bearing surface and freeze at the temperature from minus 60 to minus 75aboutC for 15-25 minutes Frozen material is maintained at a temperature from minus 14 to minus 16aboutC for 6-8 hours the Material is thawed and kept in air without load 12 h, and then heated to 85-105aboutC, cooled to room temperature, treated with alkali-salt solution with a pH of 9-10 for 10-20 minutes, wring out until a residual moisture content of 30-40%, is subjected to hot pressing and kept in air without load 12 to 24 hours

For imparting T on dyeing and greasing operations per unit irrigation type, where perform the following operations:

first Strait water temperature 50-60aboutWith up to pH slice of cake mix 4,2-4,4, centrifuge;

the second Strait at a temperature of 50aboutWith neutralizing emulsion that includes pasta VNIIG, acetate or formate, sodium and dispersant NF, taken in the amount of 1-2 0,5-1 and 0.4 to 1.2, respectively, by weight of the semifinished product, centrifuge;

the third Strait at a temperature of 50aboutWith a solution of dye consumption dye 1-5% by weight of the material;

fourth Strait solution fat emulsion at the rate of fat 8-10% by weight of semi-finished product (in terms of 100% fat), centrifuge;

fifth Strait solution of the tanning agent containing 4-10% tanning resins, 1-5% resistant to electrolytes synthetic fat, 4-10% synthetic tanning agent, 2-6% of the extract of Mimosa, 1-4% neutralizing substances, pressed to a moisture content of 30-40%.

Next is the aging of the material 12-24 h, cyclic spin with moisture at a temperature of 50aboutWith, staking marciline operations. Separate operations include impregnation, hot pressing, the application of non-pigmented primer, pigmented primer coating paint and a pinning layer. After the material passes hot pressing, aging and postopshemale for the manufacture of various products (bags, belts and so on), has a high gas and moisture permeability, elasticity, suitable for the manufacture of various parts of the shoes.

P R I m m e R 2. A solution of collagen is prepared according to example 1.

Chrome leather shavings in the amount of 300 kg is mixed with water and ground to a particle size of 0.4-0.5 mm, Get the pasta with a dry matter content of 6-9%.

A solution of collagen and pasta are mixed and homogenized at a temperature not exceeding 15aboutC for 3-5 h, filtered, cooled to a temperature of 0-5aboutTo add glutaric aldehyde in the amount of 1.3-1.5 wt.%. The resulting mixture is homogenized, spread a uniform layer thickness of 25 to 28 mm on a bearing surface and freeze at the temperature from minus 14 to minus 20aboutwith over 1,7-2,0 including Frozen material is maintained at a temperature from minus 2 to minus 7aboutC for 22-24 hours Then the material is thawed, kept in air without load 10-12 h, heated to a temperature of 85-105aboutC, cooled to room temperature, treated with alkali-salt solution at pH 9-10 for 15-20 minutes, wring out until a residual moisture content of 30-40%, is subjected to hot pressing and kept in air without nagruzke aging within 20-24 h produce cyclic spin with moisture at a temperature of 50aboutAnd finishing processing, including impregnation, hot pressing, applying a pinning layer, hot pressing and aging. The resulting material has a thickness of 3.5-5.5 mm, has a high insulation properties, and has good insulating properties. This material is suitable for residential buildings, aircraft interiors and cars, for the manufacture of parts of footwear.

The described method allows to utilize waste of raw hides and derive leather imitation material, which can find wide scope of use, cheap to manufacture and has the main disadvantage inherent in synthetic leather imitation materials, namely air leakage.

Specified in the description and the claims modes characterizing the proposed method, allow a fairly wide range to vary the properties of the obtained material and its appearance.

1. A method of OBTAINING a COLLAGEN MATERIAL comprising a grinding nedubrovo collagen containing raw material, preparation of collagen solution, homogenization, introduction to the obtained collagen mass of a crosslinking agent, homogenization, freeze trichosis fact, that collagen solution is mixed with a paste with a particle size of solids 0.2 - 0.6 mm, made from tanned leather waste, within 1 to 5 hours at a temperature not exceeding 15oTo obtain a homogeneous mass having a 0.1 to 2 wt.% nedubrovo collagen, 0.3 to 1.0 wt.% tanned collagen and pH of 2.6 to 5.0, the mass is filtered to the size of the constituent particles of 0.2 - 0.6 mm and cooled to 0 to 5oWith a cross-linking agent is administered in an amount of 0.15 - 7.0 wt.%, homogenization is carried out at a temperature of not higher than 5oWith the freezing is carried out at a temperature (-14) - (-75)oC for 0.1 to 2 hours, keeping frozen carried out for 4 to 24 h after thawing derived collagen material kept in air at room temperature in a wet condition within 6 to 12 hours, heated to 85 - 105oC, cooled to room temperature, treated with alkali-salt solution at pH 9 to 10 over 10 to 20 min, the extraction is carried out to a residual moisture content of 30 - 40%, then the material is subjected to hot pressing and subsequent exposure to air for 12 - 24 hours

2. The method according to p. 1, characterized in that the material obtained is subjected to additional processing, including washing with water at 50 - 60oWith dye at the rate of 1 to 5% by weight of the material, greasing solution emulsion at the rate of fat 8 - 10% by weight of material, in terms of 100% fat, centrifuge, retanning solution of a tanning agent containing 4 to 10% tanning resins, 1 to 5% resistant to electrolytes synthetic fat, 4 to 10% synthetic tanning agent, 2.0 to 6.0% of extract of Mimosa and 1.0 to 4.0% neutralizing substances, pressed to a moisture content of 30 - 40%, the aging of the material on the air for 12 - 24 h and cyclic wringing wet when 50oC.

 

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