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Preparation method of polybutylene succinate

A technology of polybutylene succinate and butanediol, which is applied in the field of preparation of polybutylene succinate, can solve the problems of many by-product small molecules, high corrosion of polymerized monomers, and low yield. problems, to achieve the effect of reducing product cost, increasing product yield and reducing consumption

Inactive Publication Date: 2010-11-10
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 kind of preparation method of polybutylene succinate, overcome the high corrosivity problem of polymerized monomer in the prior art on the one hand, overcome the small by-product in the prior art on the other hand The problem of many molecules and low yield can effectively reduce the production cost of polybutylene succinate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 150.0 g (1.5 mol) of succinic anhydride, 148.7 g (1.65 mol) of 1,4-butanediol, 0.1 g of benzenesulfonic acid, and 0.1 g of zinc acetate into a reactor with heating, stirring, and temperature controller , stirred and heated up under a nitrogen atmosphere, controlled the reaction temperature at 180° C. under normal pressure, and reacted for 3 hours. Add 0.05 gram of benzenesulfonic acid and 0.05 gram of zinc acetate again, heat up then, control vacuum to be absolute pressure 300Pa, 260 ℃ of reaction temperatures, continue to react for 4 hours, obtain polybutylene succinate 253.2 grams, product yield 84.8 %. After testing, its weight average molecular weight Mw value is 83.5k, molecular weight distribution Mw / Mn value is 1.9.

Embodiment 2

[0022] Add 150.0 g (1.5 mol) of succinic anhydride, 141.5 g (1.57 mol) of 1,4-butanediol, 0.1 g of benzenesulfonic acid, and tetrabutyl titanate into a reactor with heating, stirring, and temperature controller. 0.1 g of the ester was stirred and heated under nitrogen atmosphere, and the reaction temperature was controlled at 190° C. under normal pressure, and the reaction was carried out for 2 hours. Then add 0.05 g of benzenesulfonic acid and 0.05 g of tetrabutyl titanate, then raise the temperature, control the vacuum to be 30 Pa of absolute pressure, and the reaction temperature is 260 ° C, and continue to react for 3 hours to obtain 256.2 g of polybutylene succinate, the product Yield 87.9%. After testing, its weight average molecular weight Mw value is 145.5k, molecular weight distribution Mw / Mn is 1.9.

Embodiment 3

[0024] Add 150.0 g (1.5 mol) of succinic anhydride, 135.2 g (1.5 mol) of 1,4-butanediol, 0.1 g of benzenesulfonic acid, and antimony trioxide into a reactor with heating, stirring, and temperature controller. 0.2 g, 0.1 g manganese acetate, stirred and heated up under nitrogen atmosphere, controlled reaction temperature 190° C. under normal pressure, and reacted for 2 hours. Then add 0.05 g of benzenesulfonic acid, 0.1 g of antimony trioxide, and 0.05 g of manganese acetate, then raise the temperature, control the vacuum to be an absolute pressure of 30 Pa, and the reaction temperature is 280 ° C, and continue to react for 5 hours to obtain polybutylene succinate 254.2 grams, product yield 89.2%. After testing, the weight average molecular weight Mw value is 101.2k, and the molecular weight distribution Mw / Mn value is 2.0.

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Abstract

The invention discloses a preparation method of polybutylene succinate, which comprises the steps of: carrying out ring-opening polymerization on polymer monomer succinic anhydride, butanediol and catalyst under the nitrogen atmosphere, and controlling the reaction temperature to be 160-200 DEG C and the reaction time to be 1-4h; then, carrying out condensation polymerization reaction under the vacuum condition, and controlling the vacuum degree to be absolute pressure of 30-300 Pa, the reaction temperature to be 200-280 DEG C and the reaction time to be 1-6h; and finally, obtaining the target product polybutylene succinate. The detection proves that the polybutylene succinate has the weight-average molecular weight Mw reaching up to more than 100 thousand and the molecular weight distribution Mw / Mn of 1.8-2.2. Compared with the prior art, the invention reduces the byproduct water molecules by half, improves the product yield, avoids binary acid being taken as polymerization monomer, and reduces the corrosion for equipment, thus reducing the investment and maintenance cost for the fixed equipment, and being more beneficial to industrialized production.

Description

technical field [0001] The invention relates to a method for preparing polybutylene succinate, in particular to a method for preparing polybutylene succinate through ring-opening polymerization with succinic anhydride and butanediol. Background technique [0002] Polybutylene succinate 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, and has good mechanical and thermal properties , is one of the effective ways to fundamentally solve the problem of white pollution, and 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 existing technology for preparing polybutylene succinate, there is no report on the preparation method by melting ring-opening polymerization. The method reported in U.S. Patent No. 5,310,782A use...

Claims

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Application Information

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IPC IPC(8): C08G63/16C08G63/78
Inventor 吴梓新李铮陶震揭元萍张春雷
Owner SHANGHAI HUAYI GRP CO
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