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Method for preparing poly (butylene succinate) by taking dimethyl succinate as raw material

A technology of polybutylene succinate and dimethyl succinate, which is applied in the field of preparing polybutylene succinate, can solve the problems of large amount of tetrahydrofuran generated, poor catalyst selectivity, and low molecular weight of polymers, etc. Achieve high molecular weight, improve catalytic activity, and reduce catalytic activity

Active Publication Date: 2022-01-07
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem that direct esterification polycondensation method exists is that the selectivity of catalyst is poor, and the tetrahydrofuran generation amount that side reaction produces is bigger, is generally more than 10%, causes the molecular weight of polymer to be low, and the number average molecular weight of industrialized PBS is difficult to exceed one hundred thousand, and this This severely limits the application of PBS

Method used

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  • Method for preparing poly (butylene succinate) by taking dimethyl succinate as raw material
  • Method for preparing poly (butylene succinate) by taking dimethyl succinate as raw material
  • Method for preparing poly (butylene succinate) by taking dimethyl succinate as raw material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Dimethyl succinate and butanediol (wherein the mol ratio of dimethyl succinate and butanediol is 1:1.3, the quality sum of dimethyl succinate and butanediol is 35kg) is added to reaction device, then add 0.7g magnesium acetate (the quality of the transesterification catalyst is 0.005% of the total mass of dimethyl succinate and butanediol), and carry out the transesterification reaction for 3h at a negative pressure of 10kPa and at a temperature of 155°C. Then heat up to 225°C, add 1.75g ​​of tetrabutyl titanate, 0.36g of trimethyl phosphate (the amount of trimethyl phosphate is 0.5 times the amount of tetrabutyl titanate), and reduce the pressure to 20Pa The polycondensation reaction was carried out for 6 h to obtain polybutylene succinate, which was denoted as PBS1.

Embodiment 2

[0064] Embodiment 2 has carried out test 2.1, test 2.2, test 2.3 and test 2.4 altogether 4 tests.

[0065] The difference between Test 2.1 and Example 1 is only that the molar ratio of succinic acid to butanediol is 1:1.0, and finally PBS2 is obtained.

[0066] The difference between test 2.2 and embodiment 1 is only that the mol ratio of succinic acid and butanediol is 1:1.65, finally obtaining PBS3.

[0067] The difference between test 2.3 and embodiment 1 is only that the mol ratio to succinic acid and butanediol is 1:1.8, finally obtaining PBS4.

[0068] The difference between test 2.4 and embodiment 1 is only that the mol ratio to succinic acid and butanediol is 1:2.2, and finally obtains PBS5.

[0069] The present invention also tests the mechanical properties of PBS1, PBS2, PBS3, PBS4 and PBS5, and the tensile strength is tested according to GB / T 1040.2-2006 Part 2: The test conditions for molding and extruding plastics; the bending strength is tested according to GB ...

Embodiment 3

[0081] Embodiment 3 has carried out altogether 5 tests of test 3.1, test 3.2, test 3.3, test 3.4 and test 3.5.

[0082] The difference between test 3.1 and test 2.2 in embodiment 2 is only that the consumption of transesterification catalyst is 0.005% of the total mass of dimethyl succinate and butanediol, finally obtains PBS6, and the content of by-product tetrahydrofuran is 0.005% of the mass of butanediol. 4%.

[0083] The difference between test 3.2 and test 2.2 in embodiment 2 is only that the consumption of transesterification catalyst is 0.02% of the total mass of dimethyl succinate and butanediol, and finally obtains PBS7, and the content of by-product tetrahydrofuran is 0.02% of the mass of butanediol. 1%.

[0084] The difference between test 3.3 and test 2.2 in embodiment 2 is only that the consumption of transesterification catalyst is 0.03% of the total mass of dimethyl succinate and butanediol, and finally obtains PBS8, and the content of by-product tetrahydrofur...

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Abstract

The invention belongs to the field of synthesis of high polymer materials, particularly relates to a method for preparing poly (butylene succinate) by taking dimethyl succinate as a raw material, and provides the method for preparing poly (butylene succinate) by taking dimethyl succinate as the raw material. The method comprises the following steps: catalyzing dimethyl succinate and butanediol to perform transesterification reaction by using a transesterification catalyst to obtain a transesterification product; and mixing the ester exchange product with a polycondensation catalyst, and carrying out a polycondensation reaction to obtain the poly(butylene succinate). The preparation method provided by the invention can effectively reduce the generation of side reactions and the yield of a byproduct tetrahydrofuran, and the poly (butylene succinate) with higher molecular weight is obtained. Meanwhile, the raw materials are cheap and easy to obtain, so that the reaction cost is reduced.

Description

technical field [0001] The invention belongs to the synthetic field of macromolecule material, be specifically related to a kind of method that takes dimethyl succinate as raw material to prepare polybutylene succinate. Background technique [0002] Polybutylene succinate (PBS) is an important polymer material, which not only has good mechanical and mechanical properties, but also has good heat resistance; at the same time, polybutylene succinate has excellent biodegradability It can be widely used in the fields of medical supplies, agricultural films, slow-release materials, packaging, tableware and cosmetic bottles. [0003] At present, the preparation of polybutylene succinate mostly takes succinic acid and butanediol as raw materials, under the effect of catalyst, adopts direct esterification polycondensation method to prepare. The problem that direct esterification polycondensation method exists is that the selectivity of catalyst is poor, and the tetrahydrofuran gener...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/83C08G63/85C08G63/87
CPCC08G63/16C08G63/83C08G63/85C08G63/87Y02W90/10
Inventor 郑柳春刘义周天博任万成
Owner TIANJIN POLYTECHNIC UNIV
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