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Preparation method of high-molecular-weight aliphatic polyester

A technology of aliphatic polyester and high molecular weight, applied in the field of preparation of aliphatic polyester, can solve the problems of small molecular weight of aliphatic polyester products, difficulty in industrialization, harsh process conditions, etc., achieve high product yield and reduce pollution , the effect of mild process operating conditions

Active Publication Date: 2011-01-05
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a method for preparing high-molecular-weight aliphatic polyester, so as to overcome the disadvantages of low yield, low molecular weight of aliphatic polyester products, harsh process conditions, and difficulty in industrialization in existing methods.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 73.0 grams (0.5mol) of dimethyl succinate and 34.1 grams (0.55mol) of ethylene glycol respectively in the reaction device with heating, stirring and temperature controller, wherein dimethyl succinate and ethylene glycol The molar ratio is 1: 1.1, 0.02 grams of p-toluenesulfonic acid, 0.02 grams of zinc acetate, stirred and heated up under nitrogen atmosphere, controlled reaction temperature 170 ℃ under normal pressure, reacted for 5 hours, then heated up, controlled vacuum 300Pa, reaction temperature 210 °C, the reaction was continued for 6 hours to obtain 81.8 grams of polyethylene succinate. After testing, the weight average molecular weight Mw value of the product is 53.5k, and the molecular weight distribution Mw / Mn value is 2.2.

Embodiment 2

[0021] Add 50.5 grams (0.25mol) of diethyl adipate and 27.0 grams (0.3mol) of butanediol respectively in the reaction device with heating, stirring and temperature controller, wherein diethyl adipate and butanediol The molar ratio is 1:1.2, 0.05 grams of p-toluenesulfonic acid, 0.1 grams of titanate, 0.05 grams of antimony trioxide, stirring and heating up under nitrogen atmosphere, controlling the reaction temperature at 180 °C under normal pressure, reacting for 3 hours, and then heating up , control vacuum 30Pa, reaction temperature 240 ℃, continue to react for 6 hours, obtain polybutylene adipate 59.6 grams. After testing, the weight average molecular weight Mw value of the product is 216.2k, and the molecular weight distribution Mw / Mn value is 1.9.

Embodiment 3

[0023] Add 73.0 grams (0.5mol) of dimethyl succinate and 40.9 grams (0.5mol) of butanediol respectively in the reaction device with heating, stirring and temperature controller, wherein dimethyl succinate and butanediol The molar ratio of p-toluenesulfonic acid is 1:1, 0.1 g of p-toluenesulfonic acid, 0.1 g of germanic acid ester, stirring and heating up under nitrogen atmosphere, controlling the reaction temperature at 180°C under normal pressure, reacting for 3 hours, then heating up, controlling the vacuum 30Pa, the reaction temperature At 230°C, the reaction was continued for 4 hours to obtain 87.7 g of polybutylene succinate. After testing, the weight average molecular weight Mw value of the product is 197.0k, and the molecular weight distribution Mw / Mn value is 2.0.

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Abstract

The invention discloses a preparation method of high-molecular-weight aliphatic polyester, comprising the following steps of: using monomer aliphatic diacid diester and aliphatic diol as reaction materials; reacting the reaction materials and a catalyst in a nitrogen atmosphere for 1-5 hours under the condition of normal pressure and temperature of 160-200 DEG C; and reacting for 1-6 hours under the conditions of absolute pressure of 30-300Pa and temperature of 190-240 DEG C to obtain the high-molecular-weight aliphatic polyester as an objective product of the invention. The obtained high-molecular-weight aliphatic polyester has weight average molecular weight Mw value of 50-250k and a molecular weight distribution Mw / Mn value of 1.9-2.2. Compared with the prior art, the invention has theadvantages of few by-products, high product yield, mild operation condition, low device cost and stable product quality and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of aliphatic polyester, in particular to a method for preparing high-molecular-weight aliphatic polyester through transesterification of aliphatic diacid and aliphatic diol. Background technique [0002] Aliphatic polyester is an important polymer material, especially as a biodegradable material, which is easily decomposed and metabolized by various microorganisms in nature or enzymes in animals and plants. At the same time, it has good mechanical properties and can fundamentally solve white pollution. It is one of the effective ways to solve the problem, and it has a very wide range of applications in the fields of packaging, tableware, medical supplies, agricultural films, slow-release materials and biomedical materials. [0003] In the prior art, US Pat. No. 5,310,782A discloses a method for preparing aliphatic polyester by polycondensation of aliphatic diacid and aliphatic diol, but the molecular weight...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/78
Inventor 吴梓新李铮高惠敏王学火揭元萍张春雷
Owner SHANGHAI HUAYI GRP CO
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