Method for preparing collagen aggregate and collagen from chromium-containing tanned leather wastes by combined acid-enzyme controlled degradation technology

Patent metadata

Field	Value
Publication number	US-10919952-B2
Application number	US-201916290859-A
Country	US
Kind code	B2
Filing date	Mar 2, 2019
Priority date	Apr 9, 2018
Publication date	Feb 16, 2021
Grant date	Feb 16, 2021

Abstract

A method for preparing a collagen from a chromium-containing tanned leather waste is disclosed. The method includes acid dechromation, obtaining a collagen aggregate, and converting the collagen aggregate to the collagen. The method also includes a reaction in a supercritical carbon dioxide reactor.

First claim

What is claimed is:

1. A method for preparing a collagen from a chromium-containing tanned leather waste comprising:
(1) acid dechromation: immersing the chromium-containing tanned leather waste in a 1.0-5.0 mol/L hydrochloric acid solution for 0.5-3 hours; washing the chromium-containing tanned leather waste with water for 3-5 times to pH=5-7; placing the chromium-containing tanned leather waste in a 0.1-1.0 mol/L oxalic acid solution, the weight of the oxalic acid solution being 20-50 times of the dry weight of the chromium-containing tanned leather waste; transferring the mixture of the chromium-containing tanned leather waste and the oxalic acid solution to a homogenizer; stirring the mixture in the homogenizer at 30-50° C. for 5-48 hours; centrifuging the mixture at a speed of 5000-20000×g and collecting a first precipitate; dispersing the first precipitate in 0.1-1.0 mol/L sodium oxalate solution, the weight of the sodium oxalate solution being 20-50 times of the dry weight of the chromium-containing tanned leather waste; stirring the mixture of the first precipitate and the sodium oxalate solution at 30-50° C. for 24-120 hours; and centrifuging the mixture at a speed of 5000-20000×g and collecting a second precipitate;
(2) placing the second precipitate in a 0.1-1.0 mol/L acetic acid-citric acid solution, the weight of the acetic acid-citric acid solution being 20-50 times of the dry weight of the chromium-containing tanned leather waste; transferring the mixture of the second precipitate and the acetic acid-citric acid solution to the homogenizer and stirring the mixture; adding a first 0.1-1.0 mol/L sodium hydroxide solution to the mixture to pH=7.0-7.5; adding 1.0 mol/L ammonium sulfate solution to the mixture and salting out for 10-24 hours; centrifuging the mixture at a speed of 5000-20000×g for 15-30 minutes and collecting a third precipitate; dispersing the third precipitate in a first 0.1-1.0 mol/L acetic acid solution, the weight of the acetic acid solution being 20-50 times of the dry weight of the chromium-containing tanned leather waste; dialyzing in distilled water for 10-48 hours and lyophilizing to obtain a collagen aggregate, and
(3) cutting the collagen aggregate; placing the collagen aggregate in a second 0.1-1.0 mol/L acetic acid solution, the weight of the acetic acid solution being 20-50 times of the dry weight of the collagen aggregate; adding a pepsin to the mixture of collagen aggregate and acetic acid solution, the weight of the pepsin being 0.5%-2% of the weight of the collagen aggregate; reacting the mixture in a supercritical carbon dioxide reactor at 40-42° C. and 80-100 atmospheres for 5-24 hours; adding a second 0.1-1.0 mol/L sodium hydroxide solution to the mixture to pH=7.0-7.5; adding a 1.0-1.5 mol/L sodium chloride solution and salting out for 10-24 hours; centrifuging the mixture at a speed of 5000-20000×g for 15-30 minutes and collecting a fourth precipitate; dispersing the fourth precipitate in a 0.1-0.5 mol/L acetic acid solution; dialyzing in distilled water for 10-48 hours and lyophilizing to obtain the collagen.

2. The method of claim 1 , wherein the chromium-containing tanned leather waste is from a cutting or trimming of cowhide, sheepskin, or pigskin.

3. The method of claim 1 , wherein the acetic acid-citric acid solution in step (2) has a ratio of acetic acid and citric acid of 2:1 to 20:1.

4. The method of claim 1 , wherein the collagen is used in wood adhesive, protein filler, paper, and recycled leather.

Assignees

• Wang Xuechuan
• Hou Mengdi
• Liu Xinhua
• Liang Chengyuan
• Yue Ouyang
• Zheng Manhui
• Zhu Xing
• Han Qingxin
• Li Ji
• Zhang Huijie
• Qiang Taotao
• Univ Shaanxi Science & Tech

Inventors

• Wang Xuechuan
• Hou Mengdi
• Liu Xinhua
• Liang Chengyuan
• Yue Ouyang
• Zheng Manhui
• Zhu Xing
• Han Qingxin
• Li Ji
• Zhang Huijie
• Qiang Taotao

Classifications

• C07K14/78 Primary

  Connective tissue peptides, e.g. collagen, elastin, laminin, fibronectin, vitronectin or cold insoluble globulin [CIG] · CPC title

• Y02P20/54

  using solvents, e.g. supercritical solvents or ionic liquids · CPC title

• C12P21/06 Primary

  produced by the hydrolysis of a peptide bond, e.g. hydrolysate products (preparing foodstuffs by protein hydrolysis A23J3/00) · CPC title