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Preparation method of biodegradable polybutylene succinate

The technology of polybutylene succinate and succinate is applied in the field of preparation of biodegradable polybutylene succinate, and can solve the problems of poor product color and thermal stability, low product molecular weight and side reactions. Many problems, to achieve the effect of improving the appearance and color of the product, high product yield, and increasing molecular weight

Active Publication Date: 2012-10-10
沧州旭阳化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using the method of the invention can effectively solve the problems of many side reactions, low product molecular weight, poor product color and thermal stability, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Weigh 58.4g of dimethyl succinate, 43.2g of 1,4-butanediol, 0.01g of manganese acetate, and 0.01g of zinc acetate into a 250ml three-necked flask. Connect the water separator and the distillation column; start stirring, and heat the reaction system to 150°C; after 10 minutes of reaction, raise the temperature to 175°C in a programmed temperature rise mode (heating rate is 5°C / min); keep the temperature for 120 minutes until the output of methanol reaches 95wt% of theoretical value promptly considers that transesterification reaction finishes. The by-products are mainly methanol and tetrahydrofuran, wherein the content of tetrahydrofuran is 0.1%. 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 10°C / min) to 155°C, remove the water separator and condenser while continuing to pass nitrogen, connect the vacuum pump port, close the nitrogen chann...

Embodiment 2

[0032] Weigh 58.4g of monomethyl succinate, 50.4g of 1,4-butanediol, 0.02g of isopropyl titanate and 0.02g of magnesium acetate into a 250ml three-necked flask, one of which is stirred and the other is protected by nitrogen gas. The other port is connected to the water separator and the distillation column; start stirring, and heat the reaction system to 160°C; after 20 minutes of reaction, the temperature is raised to 185°C by means of a temperature program (heating rate of 5°C / min); keep the temperature for 120 minutes until the by-product methanol When the liquid output with water reaches 95wt% of the theoretical value, the reaction is considered to be over. The by-products are mainly methanol, water and tetrahydrofuran, wherein the content of tetrahydrofuran is 0.2%. In addition, there are small amounts of unreacted monomethyl succinate and 1,4-butanediol. Cool down the system (cooling rate 10°C / min) to 155°C, remove the water separator and condenser while continuing to p...

Embodiment 3

[0035] Weigh 58.4g of dimethyl succinate, 43.2g of 1,4-butanediol, 0.01g of isopropyl titanate and 0.02g of calcium acetate into a 250ml three-necked flask, one of which is stirred and the other is protected by nitrogen , the other port is connected to the 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 200°C by program heating (heating rate is 5°C / min); keep the temperature for 80 minutes until the methanol comes out When the liquid amount reaches 95wt% of the theoretical value, the transesterification reaction is considered to be over. The by-products are mainly methanol and tetrahydrofuran, wherein the content of tetrahydrofuran is 0.15%. 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 10°C / min) to 155°C, remove the water separator and con...

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Abstract

The invention provides a preparation method of biodegradable polybutylene succinate (PBS). The preparation method of the biodegradable polybutylene succinate takes a succinate compound and 1, 4-butanediol as polymerizing monomers, adopts an efficient compound catalyst system and comprises the following steps: performing transesterification reaction to obtain a PBS (polybutylene succinate) oligomer first and then performing melting polycondensation reaction to obtain a PBS polymer with a high molecular weight and good color and luster. By the preparation method, PBS degradable plastic with excellent color and luster and a high molecular weight can be prepared without using a chain extender, and meanwhile industrial production can be realized.

Description

technical field [0001] The invention belongs to the technical field of preparing biodegradable aliphatic polyester by condensation polymerization, and particularly relates to a kind of succinate compound and 1,4-butanediol as polymerization monomers, adopting a high-efficiency composite catalytic system, through ester A method for preparing biodegradable polybutylene succinate (PBS) with high molecular weight and good product color through two-stage process route of exchange and polycondensation reaction. Background technique [0002] Among biodegradable aliphatic polyesters, polybutylene succinate (PBS) has excellent comprehensive performance and biodegradability, comparable to traditional polyolefin materials, and is the most promising alternative to traditional polyolefin plastics However, compared with polyolefin plastics, PBS still has certain gaps and problems, such as low molecular weight and poor product color, etc., which seriously restrict the wider application ran...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/82
Inventor 张英伟王国利张新志孙长江
Owner 沧州旭阳化工有限公司
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