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Preparation method of polybutylene succinate

A technology for polybutylene succinate and monomethyl succinate, which is applied in the field of preparation of polybutylene succinate, can solve the problems of high water content of by-products and high tetrahydrofuran production, and achieves a reduction in Maintenance costs, beneficial to industrial production, and the effect of expanding the scope of application

Inactive Publication Date: 2012-10-10
TANGSHAN XUYANG CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by this invention is to provide a kind of preparation method of polybutylene succinate (PBS), utilize the preparation method provided by the invention, overcome on the one hand the water content of by-product in the prior art is many and by-product tetrahydrofuran The problem of high production capacity, while the methanol generated can be recycled to increase the added value of by-products; on the other hand, the traditional succinic acid is replaced by monomethyl succinate to prepare PBS, which effectively overcomes the impact of succinic acid on equipment. highly corrosive problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023]Weigh 52.8g of monomethyl succinate, 43.2g of 1,4-butanediol, 0.01g of calcium acetate, 0.01g of magnesium acetate and 0.01g of zinc acetate into a 250ml three-necked flask, one of which is stirred and the other is Nitrogen protection, the other port is connected to the water separator and the distillation column; start stirring, and heat the reaction system to 180°C; after 1.5 hours of reaction, the temperature is raised to 220°C by program heating (heating rate is 5°C / min); keep the temperature for 150min The reaction can be considered as finished until the output of water and methanol reaches 90wt% of the theoretical value. Lower the temperature of the system (cooling rate is 10°C / min) to 150°C, remove the water separator and condenser while continuing to pass nitrogen, connect the vacuum pump port, close the nitrogen channel valve and start vacuuming to an absolute pressure of 5000Pa, and react for 20 minutes , to remove unreacted monomers and by-products in the syst...

Embodiment 2

[0026] Weigh 52.8g of monomethyl succinate, 50.4g of 1,4-butanediol and 0.05g of calcium acetate into a 250ml three-necked flask, one of which is connected to stirring, one to nitrogen protection, and the other to water separator and Distillation column; start stirring, heat the reaction system to 150°C, and carry out negative pressure reaction at this temperature (wherein, the vacuum degree is an absolute pressure of 6000Pa). Keep the temperature and react for 240min until the output of water and methanol reaches 90wt% of the theoretical value. The reaction is considered complete. Stop vacuuming and feed nitrogen, add 0.15g of titanium dioxide and silicon dioxide composite with a titanium / silicon molar ratio of 9:1, 0.02g of lithium acetate, 0.005g of cobalt acetate, and 0.01g of triethyl phosphite; stir for 15min Ensure that the catalyst and additives are evenly dispersed in the reaction system. Stop the nitrogen flow, evacuate to an absolute pressure below 30Pa, and rapidl...

Embodiment 3

[0029] Weigh 52.8g of monomethyl succinate, 43.2g of 1,4-butanediol and 0.02g of titanium dioxide into a 250ml three-necked flask, one of which is connected to stirring, one to nitrogen protection, and the other to water separator and distillation Column; start stirring, and heat the reaction system to 150°C; after 60 minutes of reaction, raise the temperature to 220°C in a temperature program (heating rate of 5°C / min); keep the temperature for 180 minutes until the output of water and methanol reaches 90wt of the theoretical value % can be considered as the end of the reaction. Cool down the system (cooling rate is 10°C / min) to 150°C, remove the water separator and condenser while continuing to pass nitrogen, connect the vacuum pump port, close the nitrogen channel valve and start vacuuming to an absolute pressure of 6000Pa, and react for 15 minutes , to remove unreacted monomers and by-products in the system. Stop vacuuming and feed nitrogen, add 0.30g of germanium dioxide,...

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Abstract

The invention provides a preparation method of polybutylene succinate. The preparation method of the polybutylene succinate takes mono-methyl succinate and 1, 4-butanediol as monomers, adopts an efficient compound catalyst system and comprises the following steps: reacting to obtain a PBS (polybutylene succinate) oligomer first and then performing polycondensation reaction to obtain a PBS polymer with a high molecular weight and good color and luster. Through the adoption of the preparation method, on one hand, the problems that in the conventional technology that succinic acid and the 1, 4-butanediol are taken as monomers to prepare the PBS, the speed rate of esterification reaction is low, the succinic acid cannot react completely, and the amount of a generated byproduct tetrahydrofuran is high can be solved; on the other hand, the acidicity of the mono-methyl succinate is less than that of the succinic acid, so that corrosion to equipment is reduced, and thus the maintenance cost of the equipment is reduced and greater contribution is made to industrial production; in addition, a chain extender is not used, the application range of PBS degradable plastic in the field of food packaging can be further expanded.

Description

technical field [0001] The present invention relates to a kind of preparation method of polybutylene succinate (PBS), be specifically related to a kind of use monomethyl succinate and 1,4-butanediol as polymerization monomer, adopt high-efficiency composite catalyst system, A method of producing polybutylene succinate by esterification reaction, polycondensation reaction, etc. Background technique [0002] Polybutylene succinate (PBS) is a very important polymer material in aliphatic polyesters. It has excellent mechanical properties, thermal properties and biodegradability, and is a fundamental solution to the problems caused by traditional polyolefin materials. One of the effective ways to cause the "white pollution" problem, it is widely used in the fields of sheet, plate and film. [0003] So far, in the technology for preparing polybutylene succinate, there is no public report related to the preparation of PBS with monomethyl succinate and 1,4-butanediol as polymerized...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/82
Inventor 张英伟王国利孙长江潘小君
Owner TANGSHAN XUYANG CHEM IND CO LTD
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