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Method for preparing chitosan oligosaccharide modified biodegradable composite

A technology of biodegradation and composite materials, which is applied in the field of preparation of biodegradable composite materials, can solve the problems of chitosan oligosaccharides being incapable of melting, poor compatibility, etc., to improve molding performance, reduce crystallinity, and have broad application prospects Effect

Active Publication Date: 2013-08-21
SHENYANG POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention provides a kind of preparation method of chitosan oligosaccharide modified biodegradable composite material, the purpose is to carry out graft copolymerization by chitosan oligosaccharide to prepare chitosan graft PCL copolymer overcomes the shortcomings of chitosan oligosaccharides that cannot be melted and has poor compatibility with polymer materials, and then melt blends it with LDPE and PCL to enhance the biodegradability of LDPE and improve the mechanical properties of LDPE. At the same time, the compound Material is biodegradable

Method used

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  • Method for preparing chitosan oligosaccharide modified biodegradable composite

Examples

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Effect test

preparation example Construction

[0044] ① Preparation of polycaprolactone (PCL)

[0045] After the three-necked flask was blown with nitrogen to remove impurities such as moisture and oxygen in the flask, ε-caprolactone was added, stannous octoate was put into dry pyridine to prepare a pyridine solution with a mass concentration of 20%, and under nitrogen protection, the Add 20% pyridine solution dropwise to the above-mentioned three-necked flask, stir and react in an oil bath at 120°C for 26 hours, then stop the reaction; precipitate the reacted product with methanol, and dry the white powder in vacuum at 40°C to obtain desired polycaprolactone;

[0046] ②Chitooligosaccharide grafted polycaprolactone thermoplastic material and polycaprolactone blend membrane preparation

[0047] Dry the purchased industrial low-density polyethylene (LDPE) at 100°C for more than 6 hours in a blast dryer, PHCSO-g-PCL (chitooligosaccharide grafted polycaprolactone thermoplastic material obtained in step (1)) and PCL (The poly...

Embodiment 1

[0059] 1. Preparation of chitooligosaccharide grafted polycaprolactone thermoplastic material

[0060] (1) Preparation of N-phthalylated chitooligosaccharides

[0061] The chitosan oligosaccharide purchased was dried in a vacuum oven for 48 hours to remove the adsorbed water on its surface, and then stored in a desiccator for subsequent use.

[0062] Add 1g of chitosan oligosaccharide, 2g of phthalic anhydride and 30ml of N, N-dimethylformamide into a three-necked flask in sequence, and react for 7 hours in an oil bath at 90°C, then pour the reaction solution into ice water for sedimentation , the precipitate was repeatedly washed with ethanol for 3 times and acetone for 3 times, filtered, and then placed in a 45°C oven to dry to constant weight to obtain a brown powder product N-phthalylated chitooligosaccharide reaction intermediate body with a yield of 67.85%.

[0063] (2) Preparation of N-phthalylated chitooligosaccharide grafted polycaprolactone

[0064] Dissolve the ...

Embodiment 2

[0076] 1. Preparation of chitosan oligosaccharide grafted polycaprolactone thermoplastic material, the molar ratio of stannous octoate to ε-caprolactone monomer in step (1) is 1%, N-phthalylated chitosan oligosaccharide and ε -The proportioning ratio of caprolactone is 1: 15 (g / mL), and all the other conditions are the same as in Example 1;

[0077] 2. Preparation of Chitooligosaccharide Modified Biodegradable Composite Materials

[0078] ① Preparation of polycaprolactone (PCL) (the molar ratio of stannous octoate to ε-caprolactone monomer is 0.05%, and the preparation conditions are the same as in Example 1).

[0079] ②Chitooligosaccharide grafted polycaprolactone thermoplastic material and polycaprolactone blend membrane preparation

[0080] LDPE was dried in a blast dryer at 100°C for more than 6 hours, and PHCSO-g-PCL and PCL were dried in a vacuum oven at 50°C for more than 6 hours.

[0081] Accurately weigh 4g chitosan oligosaccharide grafted polycaprolactone thermop...

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Abstract

The invention mainly relates to a method for preparing a chitosan oligosaccharide modified biodegradable composite. The method comprises the steps of: firstly, with N,N-dimethyl formamide as a solvent, protecting amino of chitosan oligosaccharide by using phthalic anhydride to prepare a N-methyl o-acyl chitosan oligosaccharide reaction intermediate; secondly, dropwise adding pyridine solution of stannous octoate under protection of nitrogen, initiating an epsilon-caprolactone monomer to carry out ring opening polymerization so that polycaprolactone is grafted on hydroxyl of N-methyl o-acyl chitosan oligosaccharide, so as to generate a chitooligo saccharide-grafted polycaprolactone thermoplastic material; and finally melting and blending LDPE (low-density polyethylene), chitooligo saccharide-grafted caprolactone and polycaprolactone to prepare the biodegradable composite. The blended composite has biological degradability, and is free of poison and wide in application range; deterioration of an ecological environment is effectively improved; and the situations of energy crisis and petroleum resource shortage are solved.

Description

technical field [0001] The invention relates to the fields of chemical industry, materials and biomedicine, and specifically refers to firstly synthesizing a chitosan oligosaccharide graft copolymer, and then melting the chitosan oligosaccharide graft copolymer with other medical or synthetic polymer materials by using traditional material forming processing methods. Blending method to prepare biodegradable composite materials. Background technique [0002] Most polymers are derived from petroleum, a non-renewable energy source. The topic of using natural polymers as component raw materials and synthetic polymers to prepare biodegradable sheets, pellets and membrane materials has been listed as the focus of research in the field of biodegradation by many countries in the world. Low-density polyethylene (also known as high-pressure polyethylene, LDPE), LDPE has been widely used in life. LDPE has good molding processability and is suitable for many thermoplastic molding pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/04C08L23/06C08G63/08C08B37/08
Inventor 李凤红张欣蕊王立岩陈延明李红艺孙勇张文晶
Owner SHENYANG POLYTECHNIC UNIV
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