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Preparation method of all-biological-base poly butylenes succinate (PBS)

A technology for polybutylene succinate and dimethyl succinate is applied in the field of preparing biodegradable aliphatic polyester, which can solve the problems of poor thermal stability, poor product color and low molecular weight, etc., so as to improve the molecular weight , High product yield, the effect of reducing pollution

Active Publication Date: 2012-10-24
TANGSHAN XUYANG CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the deficiencies in the prior art, the present invention provides a two-stage synthesis of biomass dimethyl succinate and 1,4-butanediol using a high-efficiency composite catalytic system through transesterification and polycondensation The process route prepares the method for PBS, using the method of the present invention can effectively solve the problems such as low molecular weight, poor product color and poor thermal stability that exist in the existing process of PBS

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1 transesterification method

[0030] Weigh 58.4g of biomass dimethyl 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, and stir one of them. One port is connected to nitrogen protection, and the other port is connected to water separator and distillation column; start stirring, and heat the reaction system to 150°C; after 10 minutes of reaction, the temperature is raised to 220°C by program heating (heating rate is 5°C / min); keep the temperature for reaction 150min until the output of methanol reaches 95wt% of the theoretical value, the transesterification reaction is considered to be over. The by-products are mainly methanol and tetrahydrofuran, and the content of tetrahydrofuran is 0.005%. In addition, there are small amounts of unreacted dimethyl succinate and 1,4-butanediol. After the transesterification reaction, lower the temperature of the system (cooli...

Embodiment 2

[0032] Embodiment 2 transesterification method

[0033] Weigh 58.4g of biomass dimethyl succinate, 50.4g of 1,4-butanediol, and 0.05g of lithium acetate into a 250ml three-necked flask, one of which is connected to stirring, one is connected to nitrogen protection, and the other is connected to water separation Start stirring and heat the reaction system to 160°C; after 30 minutes of reaction, the temperature is raised to 200°C by program heating (heating rate is 5°C / min); keep the temperature for 180 minutes until the amount of methanol output reaches the theoretical value 95wt% can be considered as the end of the transesterification reaction. The by-products are mainly methanol and tetrahydrofuran, and the content of tetrahydrofuran is 0.02%. In addition, there are small amounts of unreacted dimethyl succinate and 1,4-butanediol. After the transesterification reaction, lower the temperature of the system (cooling rate is 10°C / min) to 155°C, remove the water trap and conden...

Embodiment 3

[0035] Embodiment 3 transesterification method

[0036] Weigh 58.4g of biomass dimethyl succinate, 43.2g of 1,4-butanediol, 0.02g of calcium acetate and 0.02g of tetraisopropyl titanate into a 250ml three-necked flask, one of which is stirred and the other is stirred. Connect the nitrogen protection, the other port is connected to the water separator and the distillation column; start stirring, and heat the reaction system to 150°C; after reacting for 30 minutes, raise the temperature to 220°C by program heating (heating rate is 5°C / min); keep the temperature for 180 minutes The transesterification reaction can be considered as finished until the amount of methanol output reaches 95wt% of the theoretical value. The by-products are mainly methanol and tetrahydrofuran, wherein the content of tetrahydrofuran is 0.01%. In addition, there are small amounts of unreacted dimethyl succinate and 1,4-butanediol. After the transesterification reaction, lower the temperature of the syst...

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Abstract

The invention provides a preparation method of all-biological-base poly butylenes succinate (PBS). According to the preparation method, biological-base dimethyl succinate and 1,4-butanediol are used as polymerization monomers, an efficient composite catalyst system is adopted, and the all-biological-base PBS is prepared through an ester exchange and polycondensation two-stage polymerization process route. The biological-base PBS prepared by the method has the advantages of high molecular weight, good product color and luster, few by-products, high product yield and the like, and in addition, because chain extenders are not used, the application range of aliphatic polyester degradable plastics to the food package field can be further enlarged. In addition, compared with the existing method for preparing the PBS from petroleum bases as raw materials, the method provided by the invention also has the advantages that the production cost is low.

Description

technical field [0001] The invention belongs to the technical field of preparing biodegradable aliphatic polyesters, in particular to a kind of polymerized monomers using biomass dimethyl succinate and 1,4-butanediol, adopting a high-efficiency composite catalyst system, through transesterification A method for preparing all-bio-based polybutylene succinate with high molecular weight and good product color through two-stage polymerization process route of polycondensation and polycondensation. Background technique [0002] PBS has a high melting point, and has good mechanical properties and biodegradability. Among aliphatic polyesters, PBS has excellent comprehensive properties and can be compared with traditional polyolefin materials. It is the most promising material to replace traditional polyolefin plastics. However, compared with polyolefin plastics, there is still a certain gap between PBS and polyolefin plastics, such as low molecular weight and poor product color, et...

Claims

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Application Information

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IPC IPC(8): C08G63/16C08G63/78
Inventor 张英伟王国利张新志孙长江
Owner TANGSHAN XUYANG CHEM IND CO LTD
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