CN109337586B - Method for producing oxhide gelatin by acid process - Google Patents

Method for producing oxhide gelatin by acid process Download PDF

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CN109337586B
CN109337586B CN201811442555.6A CN201811442555A CN109337586B CN 109337586 B CN109337586 B CN 109337586B CN 201811442555 A CN201811442555 A CN 201811442555A CN 109337586 B CN109337586 B CN 109337586B
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gelatin
acid
solution
cowhide
oxhide
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CN109337586A (en
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陈庆成
张格�
潘美针
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Shandong Hengxin Biotechnology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09HPREPARATION OF GLUE OR GELATINE
    • C09H3/00Isolation of glue or gelatine from raw materials, e.g. by extracting, by heating

Abstract

The invention discloses a method for producing oxhide gelatin by an acid method, and belongs to the technical field of gelatin processing. According to the method, the cowhide is subjected to two-stage acid leaching, the first stage is hydrochloric acid soaking, the second stage is mixed organic acid soaking, the two-stage acid leaching greatly improves the extraction rate of gelatin, the extraction rate can reach 87%, the gelatin is frozen at the soaking interval, the gelatin is enhanced in gel strength and viscosity through the freeze-thaw action, and the gel strength and viscosity of the prepared cowhide gelatin can reach 431g and 5.9 mPa.

Description

Method for producing oxhide gelatin by acid process
Technical Field
The invention relates to a method for producing oxhide gelatin by an acid method, and belongs to the technical field of gelatin processing.
Background
Gelatin (Gelatin) is a high polymer of high molecular polypeptides obtained by purifying and primarily hydrolyzing collagen contained in animal skin, bone, cartilage, ligament, and muscle membrane, and is also called animal Gelatin and fat glue. The gelatin finished product is a colorless or light yellow, transparent or semitransparent and hard amorphous substance, and the white matter quantity is better. The gelatin is insoluble in cold water, but can slowly absorb water to swell and soften, and the gelatin can absorb 5-10 times of water by weight. Gelatin belongs to a macromolecular hydrophilic colloid, is a low-calorie health food with higher nutritive value, can be used for making candy additives, frozen food additives and the like, and is an indispensable raw material in the aspects of photographic films, X-ray films, aviation films, artificial board adhesives, belt adhesives, rubber products, cotton cloth, papermaking and the like in industry.
In the prior art, five methods of producing gelatin mainly comprise an alkaline method, an acid salt method, a salt-alkaline method and an enzymatic method, the most common production methods in industrial production at present are the alkaline method and the acid method, and although the alkaline method occupies a large market, the extraction rate of the acid method process is high and the production period is short, so that the gelatin is widely applied. However, the acid treatment process is simple, but is easy to cause environmental pollution. In addition, excessive acid action can cause abnormal breakage of covalent bonds of collagen molecules, destroy the integrity of collagen subunits and further affect the quality of finished gelatin, so that the dosage of acid and the soaking time need to be strictly controlled to prepare good-quality gelatin.
Disclosure of Invention
Aiming at the problems, the invention provides a method for producing oxhide gelatin by an acid method, which comprises the steps of carrying out acid leaching on oxhide in two stages, wherein the first stage is hydrochloric acid soaking, and the second stage is mixed organic acid soaking, the gelatin extraction rate is improved by the two-stage acid leaching, freezing is carried out at the soaking interval, and the gelatin is enhanced in gel strength and viscosity by freeze thawing, and the method is simple and has less acid consumption compared with the existing process.
The invention provides a method for producing oxhide gelatin by an acid method, which comprises the following steps:
(1) pretreating cow leather: soaking fresh cowhide with fur in sodium sulfide solution with mass fraction of 0.4-0.8%, unhairing, cutting the cowhide into small pieces with size no greater than 5mm × 5mm, soaking in sodium chloride solution with mass fraction of 1.2-2.0% at 40-50 deg.C for 3-6 hr, and washing with water to remove sodium chloride;
(2) adding the cowhide treated in the step (1) into a hydrochloric acid aqueous solution with the mass fraction of 1-2% for soaking for 1-3 h;
(3) cleaning the cowhide obtained in the step (2) until the pH value of water after washing is 6.0-7.0, and freezing to-2-5 ℃;
(4) adding the frozen cowhide into an organic acid aqueous solution for leaching, slowly heating to 45-60 ℃, preserving heat for 1.5-2h, cooling to-5-0 ℃, maintaining for 0.5-1.0h, continuously heating to 45-60 ℃, and leaching for 1.5-2h to obtain a leaching solution;
(5) and (3) filtering: adding 0.5-0.6% W/V (g/mL, the same below) of active carbon or diatomite into the leaching solution obtained in the step (4), stirring for 2.5-3.5h, and filtering to obtain a dilute glue solution;
(6) and (3) filtering and concentrating: concentrating the dilute glue solution by an ultrafiltration membrane to obtain 25-30 wt% of ultrafiltration concentrated solution, concentrating the ultrafiltration concentrated solution by a nanofiltration membrane to obtain 55-65 wt% of nanofiltration concentrated solution, and performing spray drying and crushing on the nanofiltration concentrated solution to obtain a gelatin product.
In one embodiment of the present invention, the weight ratio of the cow hide to the aqueous hydrochloric acid solution in the step (2) is 1: 3-5, and the soaking temperature is 55-60 ℃.
In one embodiment of the present invention, the organic acid aqueous solution in step (3) contains 2 to 4 mass% of acetic acid and 1 to 3 mass% of lactic acid, and the weight ratio of cow hide to organic acid aqueous solution is 1: 5-6.
In one embodiment of the invention, the pressure for ultrafiltration membrane concentration is 0.5-0.8 MPa, and the pressure for nanofiltration membrane concentration is 0.6-0.8 MPa.
In one embodiment of the present invention, the concentration of acetic acid is 4%.
In one embodiment of the present invention, the concentration of lactic acid is 2%.
The invention has the following technical effects:
(1) the method ensures that the cowhide is subjected to acid leaching in two stages, the first stage is hydrochloric acid soaking, the second stage is mixed organic acid soaking, and the acid leaching in two stages greatly improves the extraction rate of gelatin, so that the extraction rate can reach 87%;
(2) and freezing is carried out at the soaking interval, the gel strength and viscosity of the gelatin are enhanced through the freeze-thaw action, and the gel strength and viscosity of the prepared cowhide gelatin can reach 431g and 5.9 mPa.s.
Detailed Description
And (3) measuring the gel strength: taking 6.67g of gelatin obtained in the extraction, adding 70mL of water, standing at about 20 ℃ for 2h to make the gelatin absorb water and expand, then placing in a water bath at 60 ℃ for 15min to dissolve the gelatin into uniform liquid, and adding water to prepare a glue solution with the mass percentage concentration of 6.67%; covering, placing for 1-4 h, stirring and heating in a water bath at 65 +/-2 ℃ for 15min to uniformly dissolve the sample, placing for 15min at room temperature, horizontally placing the frozen bottle in a constant-temperature water bath at 10 +/-0.1 ℃, sealing with a rubber plug, keeping the temperature for 17 +/-1 h, quickly moving out the frozen bottle, wiping the outer wall, and placing on a test board of a frozen instrument for testing to obtain the gel strength of the gelatin.
And (3) viscosity measurement: : preparing 100mL of glue solution with the mass concentration of 6.67% from the extracted gelatin in a triangular flask, cooling the glue solution to about 61 ℃, starting a super constant-temperature water bath to ensure that the temperature of the glue solution flowing through a viscometer jacket is 60 +/-0.1 ℃, blocking the tail end of a capillary tube of a Boehringer viscometer to prevent air or bubbles from entering, and quickly pouring the glue solution into a viscosity tube until the glue solution exceeds the upper scale mark by 2-3 cm. And (3) inserting a thermometer into the viscometer, adjusting the level of the glue solution to the upper scale mark when the temperature is stabilized at 60 +/-0.1 ℃, starting timing when the tail end of the capillary is released, stopping timing when the level of the glue solution reaches the lower scale mark, and recording the time as t seconds.
By the viscosity calculation formula: n-1.005 At-1.005B/t, the viscosity of the glue solution is 6.5 mPa.s, which reaches the standard of medicinal gelatin, wherein n-glue solution viscosity, mPa.s, t-flow time, s; a, B-viscometer constants.
Gelatin extraction rate MGelatin/MRaw materials×100%。
Example 1
A method for producing oxhide gelatin by an acid method comprises the following steps:
(1) pretreating cow leather: soaking fresh cowhide with fur in 0.5% sodium sulfide solution, unhairing, cutting the cowhide into small pieces no larger than 5mm × 5mm, soaking in 1.2% sodium chloride solution at 40 deg.C for 6 hr, and washing with water to remove sodium chloride;
(2) adding the cowhide treated in the step (1) into a hydrochloric acid aqueous solution with the mass fraction of 2% for soaking, wherein the weight ratio of the cowhide to the hydrochloric acid aqueous solution is 1: 3, the soaking temperature is 55 ℃, and the soaking time is 1.5 h;
(3) cleaning the cowhide obtained in the step (2) until the pH value of water after washing is 6.5, and freezing to-2 ℃;
(4) leaching the frozen cow leather in an aqueous solution containing 2% acetic acid and 2% lactic acid, wherein the weight ratio of the cow leather to the aqueous solution of organic acid is 1: slowly heating to 48 ℃, keeping the temperature for 2h, cooling to 0 ℃, keeping the temperature for 0.5h, and continuously heating to
Leaching for 1.5h at 60 ℃ to obtain a leaching solution;
(5) and (3) filtering: adding 0.6% W/V active carbon or diatomite into the leaching liquor obtained in the step (4), stirring for 2.5h, and filtering to obtain a dilute glue solution;
(6) and (3) filtering and concentrating: concentrating the dilute glue solution by an ultrafiltration membrane to obtain 25 wt% of ultrafiltration concentrated solution, concentrating the ultrafiltration concentrated solution by a nanofiltration membrane to obtain 55 wt% of nanofiltration concentrated solution, and performing spray drying and crushing on the nanofiltration concentrated solution to obtain a gelatin product.
Example 2
A method for producing oxhide gelatin by an acid method comprises the following steps:
(1) pretreating cow leather: soaking fresh cowhide with fur in 0.6% sodium sulfide solution, unhairing, cutting the cowhide into small pieces no larger than 5mm × 5mm, soaking in 1.5% sodium chloride solution at 45 deg.C for 5.5 hr, and washing with water to remove sodium chloride;
(2) and (3) soaking the treated cow leather in a 1.5% hydrochloric acid aqueous solution, wherein the weight ratio of the cow leather to the hydrochloric acid aqueous solution is 1: 4, the soaking temperature is 55 ℃, and the soaking time is 1.5 h;
(3) cleaning the cowhide obtained in the step (2) until the pH value of water after washing is 6.0, and freezing to-5 ℃;
(4) leaching the frozen cow leather in an aqueous solution containing 3% acetic acid and 2% lactic acid, wherein the weight ratio of the cow leather to the aqueous solution of organic acid is 1: 6, slowly heating to 50 ℃, keeping the temperature for 2h, cooling to 0 ℃, keeping the temperature for 0.5h, and continuously heating to
Leaching for 1.5h at 60 ℃ to obtain a leaching solution;
(5) and (3) filtering: adding 0.5% W/V active carbon or diatomite into the leaching solution obtained in the step (4), stirring for 3.5h, and filtering to obtain a dilute glue solution;
(6) and (3) filtering and concentrating: concentrating the dilute glue solution by an ultrafiltration membrane to obtain 30 wt% of ultrafiltration concentrated solution, concentrating the ultrafiltration concentrated solution by a nanofiltration membrane to obtain 65 wt% of nanofiltration concentrated solution, performing spray drying on the nanofiltration concentrated solution, and crushing to obtain the gelatin product.
Example 3
A method for producing oxhide gelatin by an acid method comprises the following steps:
(1) pretreating cow leather: soaking fresh cowhide with fur in 0.5% sodium sulfide solution, unhairing, cutting the cowhide into small pieces no larger than 5mm × 5mm, soaking in 1.2% sodium chloride solution at 40 deg.C for 6 hr, and washing with water to remove sodium chloride;
(2) (2) soaking the treated cow leather in a 1% hydrochloric acid aqueous solution, wherein the weight ratio of the cow leather to the hydrochloric acid aqueous solution is 1: 5, soaking at 60 ℃ for 2 h;
(3) cleaning the cowhide obtained in the step (2) until the pH value of water after washing is 7.0, and freezing to-2 ℃;
(4) leaching the frozen cow leather in an aqueous solution containing 4% acetic acid and 2% lactic acid, wherein the weight ratio of the cow leather to the aqueous solution of organic acid is 1: slowly heating to 60 deg.C, keeping the temperature for 2h, cooling to-2 deg.C, maintaining for 0.5h, and continuously heating to
Leaching for 1.5h at 50 ℃ to obtain a leaching solution;
(5) and (3) filtering: adding 0.6% W/V active carbon or diatomite into the leaching liquor obtained in the step (4), stirring for 3h, and filtering to obtain a dilute glue solution;
(6) and (3) filtering and concentrating: concentrating the dilute glue solution by an ultrafiltration membrane to obtain 25 wt% of ultrafiltration concentrated solution, concentrating the ultrafiltration concentrated solution by a nanofiltration membrane to obtain 65 wt% of nanofiltration concentrated solution, and performing spray drying and crushing on the nanofiltration concentrated solution to obtain a gelatin product.
Comparative example 1
The hydrochloric acid water in the step (2) is changed into clear water, and the gelatin is prepared under the same conditions as in the example 3.
Comparative example 2
The freezing operation in step (3) was omitted, and gelatin was prepared under the same conditions as in example 3.
Comparative example 3
And (4) leaching at constant temperature for 4 hours in the step (4), and preparing the gelatin under the same conditions as in the example 3.
The prepared gelatin was subjected to a performance test, and the results are shown in table 1:
table 1 properties of the gelatin products prepared according to the invention
Figure BDA0001885021780000041
Figure BDA0001885021780000051
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. A method for producing oxhide gelatin by an acid process, the method comprising the steps of:
(1) pretreating cow leather: soaking fresh cowhide with fur in sodium sulfide solution with mass fraction of 0.4-0.8%, unhairing, cutting the cowhide into small pieces with size no greater than 5mm × 5mm, soaking in sodium chloride solution with mass fraction of 1.2-2.0% at 40-50 deg.C for 3-6 hr, and washing with water to remove sodium chloride;
(2) adding the cowhide treated in the step (1) into a hydrochloric acid aqueous solution with the mass fraction of 1-2% for soaking for 1-3 h;
(3) cleaning the cowhide obtained in the step (2) until the pH value of water after washing is 6.0-7.0, and freezing to-2-5 ℃;
(4) adding the frozen cowhide into an organic acid aqueous solution for leaching, slowly heating to 45-60 ℃, preserving heat for 1.5-2h, cooling to-5-0 ℃, maintaining for 0.5-1.0h, continuously heating to 45-60 ℃, and leaching for 1.5-2h to obtain a leaching solution;
(5) and (3) filtering: adding 0.5-0.6% g/mL of active carbon or diatomite into the leaching solution obtained in the step (4), stirring for 2.5-3.5h, and filtering to obtain a dilute glue solution;
(6) and (3) filtering and concentrating: concentrating the dilute glue solution by an ultrafiltration membrane to obtain 25-30 wt% of ultrafiltration concentrated solution, concentrating the ultrafiltration concentrated solution by a nanofiltration membrane to obtain 55-65 wt% of nanofiltration concentrated solution, and performing spray drying and crushing on the nanofiltration concentrated solution to obtain a gelatin product.
2. The method for producing the oxhide gelatin by the acid process according to claim 1, wherein the weight ratio of the oxhide to the hydrochloric acid aqueous solution in the step (2) is 1: 3-5, and the soaking temperature is 55-60 ℃.
3. The method for producing oxhide gelatin by acid process according to claim 1 or 2, wherein the organic acid aqueous solution in step (3) contains 2-4% by weight of acetic acid and 1-3% by weight of lactic acid, and the weight ratio of oxhide to organic acid aqueous solution is 1: 5-6.
4. The method for producing the oxhide gelatin by the acid method according to claim 1 or 2, wherein the concentration pressure of the ultrafiltration membrane is 0.5-0.8 MPa, and the concentration pressure of the nanofiltration membrane is 0.6-0.8 MPa.
5. The method for acid production of oxhide gelatin according to claim 3 wherein the concentration of acetic acid is 4%.
6. The method for producing oxhide gelatin by acid process according to claim 3 wherein the concentration of lactic acid is 2%.
7. Gelatin produced by the method of any one of claims 1 to 6 for the acid production of gelatin.
8. An artificial board adhesive, a belt adhesive, a rubber article, cotton or paper comprising the gelatin of claim 7.
9. Use of the gelatine of claim 7 in the field of adhesives.
10. Use of an acid process according to any one of claims 1 to 6 for the production of gelatin in the field of gelatin processing.
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CN104327748A (en) * 2014-10-27 2015-02-04 浙江吉达生物科技有限公司 Separation and concentration equipment and separation and concentration method for gelatin
CN108203566A (en) * 2016-12-20 2018-06-26 湖南尔康明胶有限公司 The technique that a kind of alkaline process prepares pharmagel
CN108203567A (en) * 2016-12-20 2018-06-26 湖南尔康明胶有限公司 The technique that a kind of acid system prepares pharmagel

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104327748A (en) * 2014-10-27 2015-02-04 浙江吉达生物科技有限公司 Separation and concentration equipment and separation and concentration method for gelatin
CN108203566A (en) * 2016-12-20 2018-06-26 湖南尔康明胶有限公司 The technique that a kind of alkaline process prepares pharmagel
CN108203567A (en) * 2016-12-20 2018-06-26 湖南尔康明胶有限公司 The technique that a kind of acid system prepares pharmagel

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