Method for producing poly(butylene succinate) with lipase as catalyst

A polybutylene succinate and diethyl succinate technology, which is applied in the field of polybutylene succinate production, can solve problems such as difficult removal, rejection of medical materials, unsatisfactory environmental and material effects, etc. , to achieve the effect of no metal residue, large output and low energy consumption

Active Publication Date: 2010-12-08
山东秋水化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the residual metal is difficult to remove due to the strong interaction between the metal and the ester, resulting in unfavorable effects on the environment and material disposal, which limits the application range of polymer materials, and may also become a factor of rejection of medical materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] A kind of method that uses lipase as catalyst to produce polybutylene succinate (PBS), its production step is:

[0014] In the first step, 0.5 parts of enzyme, 17 parts of diethyl succinate, 8 parts of butanediol, and 0.1 part of water are mixed according to the mass ratio at a temperature of 50 ° C: normal pressure for 2 hours, and then stirred at a pressure of 4 mmHg React for 1 hour; then return to normal pressure, and react for another 2 hours; this process is repeated 3 times;

[0015] The second step is to return to normal pressure, add 30 parts of toluene and 0.1 part of water, and stir and react at 50 ° C for 4 hours;

[0016] The 3rd step, vacuum distillation 2 hours, solvent recovery;

[0017] In the fourth step, add 15 parts of chloroform, dissolve and filter, and add 60 parts of methanol to the filtrate for purification to obtain polybutylene succinate (PBS). The filter residue is enzyme, which can be reused repeatedly.

[0018] Under these conditions, po...

Embodiment 2

[0020] A kind of method that uses lipase as catalyst to produce polybutylene succinate (PBS), its production step is:

[0021] In the first step, 1 part of enzyme, 16 parts of diethyl succinate, 7 parts of butanediol, and 3.0 parts of water are reacted at a temperature of 70 ° C for 3.5 hours at normal pressure, and then stirred under a pressure of 17 mmHg React for 1.5 hours, then return to normal pressure, and react for another 3.5 hours; this process is repeated 4 times;

[0022] In the second step, return to normal pressure, add 45.5 parts of cyclohexane and 3.0 parts of water, and stir and react at 70°C for 23 hours;

[0023] The 3rd step, vacuum distillation 3 hours, solvent recovery;

[0024] In the fourth step, add 17.5 parts of chloroform, dissolve and filter, and add 70 parts of methanol to the filtrate for purification to obtain polybutylene succinate (PBS). The filter residue is enzyme, which can be reused repeatedly.

[0025] Under these conditions, polybutylen...

Embodiment 3

[0027] A kind of method that uses lipase as catalyst to produce polybutylene succinate (PBS), its production step is:

[0028] In the first step, 5 parts of enzyme, 18 parts of diethyl succinate, 9 parts of butanediol, and 5.0 parts of water are reacted at a temperature of 90°C for 5 hours at normal pressure, and then stirred at a pressure of 40mmHg according to the mass ratio React for 2 hours, then return to normal pressure, and react for 5 hours; this process is repeated 5 times;

[0029] In the second step, return to normal pressure, add 100 parts of n-hexane and 5.0 parts of water, and stir and react at 90°C for 48 hours;

[0030] The 3rd step, vacuum distillation 5 hours, solvent recovery;

[0031] In the fourth step, add 20 parts of chloroform, dissolve and filter, and add 80 parts of methanol to the filtrate for purification to obtain polybutylene succinate (PBS). The filter residue is enzyme, which can be reused repeatedly.

[0032] Under these conditions, polybuty...

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PUM

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Abstract

The invention relates to a method for producing poly (butylene succinate) (PBS) with lipase as a catalyst. The steps comprises: step (1) 0.05 portion to 10 portions of enzyme, 10 portions to 20 portions of diethyl succinate, 5 portions to 10 portions of butanediol and 0.1 portion to 5.0 portions of water (by weight percentage) react at the temperature of 50 DEG C to 90 DEG C under normal pressurefor 2 hours to 5 hours, then react for 1 hour to 3 hours under the pressure of 4 mmHg to 40mmHg and then for 2 hours to 5 hours when the pressure is resumed to normal; and the process is repeated 3 times to 5 times; step (2) 30 portions to 100 portions of alkane or benzene ring solvent and 0.1 portion to 5.0 portions of water are added and reaction lasts 4 hours to 48 hours at the temperature of 50 DEG C to 90 DEG C when stirring is conducted; step (3) reduced pressure distillation is conducted for 2 hours to 5 hours and the solvent is recovered; and step (4) 15 portions to 20 portions of chloroform are added and dissolves, filtration is conducted and the filtrate is added with 60 portions to 80 portions of methanol and purified, thus obtaining the poly (butylene succinate) (PBS); and thefilter residue is enzyme and can be reused. The method is characterized by economy, low consumption, high output, no metal residue and environmental protection.

Description

technical field [0001] The invention belongs to the technical field of polybutylene succinate (PBS) production, and in particular relates to a method for producing polybutylene succinate (PBS) by using lipase as a catalyst. Background technique [0002] Polybutylene succinate (PBS) is an important biodegradable aliphatic polyester in various forms. It has good biocompatibility and biodegradability, because of its good mechanical strength and various melting points, it is suitable for Replaces many general purpose thermoplastics. Polybutylene succinate (PBS) is generally chemically synthesized, that is, commercial products of high molecular weight aliphatic polyester materials are synthesized by organometallic catalysts at a reaction temperature of ≥190°C. However, the residual metals are difficult to remove due to the strong interaction between metals and esters, resulting in unfavorable effects on the environment and material disposal, which limits the application range of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/82C08G63/16
Inventor 张敏杨金明
Owner 山东秋水化学科技有限公司
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