Preparation method of chitosan-protocatechuic acid graft copolymer film

A technology of graft copolymer and protocatechuic acid, which is applied in the field of preparation of chitosan-protocatechuic acid graft copolymer film, can solve unfavorable large-scale production application, low mechanical strength of plastic wrap, and antioxidant activity Low-level problems, to achieve the effect of simple and easy operation in the film-making process, improved mechanical properties and physical and chemical properties, and low transparency

Inactive Publication Date: 2016-12-14
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The basic principle is to use the modifier 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) to help the carboxyl group on the protocatechuic acid molecule and the amino group of chitosan Form amide bonds between them, do not actually participate in the reaction, and the intermediates are easy to be washed or dialyzed. EDC / N-hydroxysuccinimide (NHS) is selected as the cross-linking agent to modify chitosan to promote amide and The formation of esters, the synthesis conditions are mild, easy to operate, the cross-linking agent is non-toxic and has no residue, and it can also significantly improve the grafting efficiency and grafting rate of chitosan, and significantly improve the chitosan-protocatechuic acid grafting The physical and mechanical properties of the copolymer film to solve the problems of low mechanical strength, poor barrier property, low antioxidant activity, and unfavorable for large-scale production and application in the existing patented plastic wrap, so as to improve the performance of chitosan and expand its use in The scope of application in food storage and preservation

Method used

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  • Preparation method of chitosan-protocatechuic acid graft copolymer film
  • Preparation method of chitosan-protocatechuic acid graft copolymer film
  • Preparation method of chitosan-protocatechuic acid graft copolymer film

Examples

Experimental program
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Effect test

Embodiment 1

[0031] The preparation process of chitosan-protocatechuic acid graft copolymer film:

[0032] (1) Take by weighing 1.22g chitosan and be dissolved in 25mL 0.5% acetic acid solution, stir magnetically until completely dissolving, obtain chitosan solution; Take by weighing 5.8g protocatechuic acid and dissolve in 5mL dehydrated alcohol, obtain protocatechuic acid Catechin solution;

[0033] (2) Add 7.2g of EDC, protocatechuic acid solution, and 4.3g of NHS into a 20mL MES buffer reactor in sequence, and control the pH range to 6; then place it in an ice-water bath, and react with magnetic stirring for 1h;

[0034] (3) Add the fully dissolved chitosan solution into the reactor, and react for 24 hours at room temperature and normal pressure;

[0035] (4) Put the reaction solution into a dialysis bag, dialyze with tap water for 48 hours, and then dialyze with deionized water for 24 hours. After the dialysate is freeze-dried, the chitosan-protocatechuic acid graft copolymer is obta...

Embodiment 2

[0044] The preparation process of chitosan-protocatechuic acid graft copolymer film:

[0045] (1) Take by weighing 1.22g chitosan and be dissolved in 25mL 0.5% acetic acid solution, stir magnetically until completely dissolving, obtain chitosan solution; Take by weighing 5.8g protocatechuic acid and dissolve in 5mL dehydrated alcohol, obtain protocatechuic acid Catechin solution;

[0046] (2) Add 7.2g of EDC, protocatechuic acid solution, and 4.3g of NHS into a 20mL MES buffer reactor in sequence, and control the pH range to 5.5; then place it in an ice-water bath, and react with magnetic stirring for 1h;

[0047] (3) Add the fully dissolved chitosan solution into the reactor, and react for 12 hours at 20°C;

[0048] (4) Put the reaction solution into a dialysis bag, dialyze with tap water for 48 hours, and then dialyze with deionized water for 24 hours. After the dialysate is freeze-dried, the chitosan-protocatechuic acid graft copolymer is obtained, which is a purple-red sa...

Embodiment 3

[0057] The preparation process of chitosan-protocatechuic acid graft copolymer film:

[0058] (1) Take by weighing 1.22g chitosan and be dissolved in 25mL 0.5% acetic acid solution, stir magnetically until completely dissolving, obtain chitosan solution; Take by weighing 5.8g protocatechuic acid and dissolve in 5mL dehydrated alcohol, obtain protocatechuic acid Catechin solution;

[0059] (2) Add 7.2g of EDC, protocatechuic acid solution, and 4.3g of NHS into a 20mL MES buffer reactor in sequence, and control the pH range to 5; then place it in an ice-water bath, and react with magnetic stirring for 0.5h;

[0060] (3) Add the fully dissolved chitosan solution into the reactor, and react for 6 hours at room temperature and normal pressure;

[0061] (4) Put the reaction solution into a dialysis bag, dialyze with tap water for 48 hours, and then dialyze with deionized water for 24 hours. After the dialysate is freeze-dried, the chitosan-protocatechuic acid graft copolymer is obt...

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Abstract

The invention provides a preparation method of a chitosan-protocatechuic acid graft copolymer film. The preparation method comprises the following steps: using chitosan and protocatechuic acid molecules as reaction substrates, using EDC / NHS as a crosslinking agent, synthesizing a chitosan-protocatechuic acid graft copolymer, and performing freeze drying to prepare a film forming solution with the proper concentration; removing bubbles, drying, soaking till the film forming solution is neutral, and performing film uncovering to finally obtain the chitosan-protocatechuic acid graft copolymer film. The preparation method is low in investment, and is suitable for use in large-scale production. The chitosan-protocatechuic acid graft copolymer film prepared by the preparation method is significantly improved in mechanical properties and physical and chemical properties, is low in water content, good in water resistance, low in transparency and high in tensile strength, has relatively high antioxidant activity, provides a very good way for artificially synthesizing a novel food fresh-keeping film, widens the application range of a chitosan film in food storage and food fresh keeping, improves the value of chitosan, and improves economic benefits of a food processing enterprise.

Description

technical field [0001] The invention belongs to the technical field of film material preparation, in particular to a preparation method of a chitosan-protocatechuic acid graft copolymer film with antioxidant activity. Background technique [0002] With the continuous development of society and science and technology, people realize that issues such as environmental protection and food safety are particularly important. Traditional inert packaging materials are widely used because of their good barrier properties, high strength, and good flexibility. However, plastic wraps made of polyethylene (PE), polyvinyl chloride (PVC) and other chemical polymer materials as basic raw materials will produce a large amount of "three wastes" in the production process, causing great damage to the environment. In addition, when it is used in the packaging of oil-containing foods, some harmful substances (flexible agents) in it will migrate, causing food safety hazards. Paper has disadvantag...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08B37/08C08L5/08C08K5/053B65D65/38
CPCC08J5/18B65D65/38C08B37/003C08J2305/08C08K5/053C08L2201/08C08L2203/16C08L5/08
Inventor 刘俊金昌海孟晨光
Owner YANGZHOU UNIV
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