Preparation method of poly(butylene succinate)

A technology of polybutylene succinate and butanediol, which is applied in the field of biodegradable polyester preparation, can solve the problems of increased equipment cost and energy consumption, can not meet industrial applications well, and can improve molecular weight and Material properties, the effect of reducing energy consumption and organic solvent consumption, and reducing production costs

Active Publication Date: 2014-04-09
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing lipase-catalyzed synthesis of PBS needs to be carried out continuously under high vacuum conditions in order to remove by-product water or alcohols, which greatly increases equipment costs and energy consumption
Moreover, the average molecular weight of the product of the current enzymatic synthesis of PBS is only 10,000-38,000 Da, which cannot well meet the needs of industrial applications.

Method used

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  • Preparation method of poly(butylene succinate)
  • Preparation method of poly(butylene succinate)
  • Preparation method of poly(butylene succinate)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1, take diethyl succinate as acyl donor to prepare polybutylene succinate (reaction mode such as figure 1 shown)

[0027] (1) Add 30 parts of diethyl succinate, 35 parts of 1,4-butanediol and 100 parts of toluene respectively into the reaction flask, heat to 80°C and keep stirring, add 10 parts of lipase preparation Novozym43510, under normal pressure After 24 hours of solution polymerization, the enzyme preparation was removed by filtration (recyclable), and the filtrate was rotary evaporated at 35°C to remove the solvent (recyclable) to obtain a white prepolymer.

[0028] (2) Take 70 parts of the white prepolymer, add it to the reaction bottle, heat to 100°C and keep stirring, add lipase preparation Novozym 4355 parts after the prepolymer is melted, and stop the reaction after 40 hours of bulk polymerization under melting conditions; Add 100 parts of chloroform to dissolve the reaction mixture, filter and recover the enzyme preparation, slowly add the filt...

Embodiment 2

[0030] Embodiment 2, using dimethyl succinate as an acyl donor to prepare polybutylene succinate

[0031] (1) Add 35 parts of dimethyl succinate, 35 parts of 1,4-butanediol and 110 parts of toluene respectively into the reaction flask, heat to 80°C and keep stirring, add 12 parts of lipase preparation Novozym43512, under normal pressure After 24 hours of solution polymerization, the enzyme preparation was removed by filtration (recyclable), and the filtrate was rotary evaporated at 35°C to remove the solvent (recyclable) to obtain a white prepolymer.

[0032] (2) Take 70 parts of the white prepolymer, add it to the reaction bottle, heat to 100°C and keep stirring, add lipase preparation Novozym 4355 parts after the prepolymer is melted, and stop the reaction after 48 hours of bulk polymerization under melting conditions; Add 100 parts of chloroform to dissolve the reaction mixture, filter and recover the enzyme preparation, slowly add the filtrate dropwise to 500 parts of meth...

Embodiment 3

[0034] Embodiment 3, take succinic acid as acyl donor to prepare polybutylene succinate

[0035] (1) Add 30 parts of succinic acid, 36 parts of 1,4-butanediol and 200 parts of diphenyl ether into the reaction flask, heat to 65°C and keep stirring, add lipase preparation Novozym4355 parts, under normal pressure After solution polymerization for 24 hours, remove the enzyme preparation by filtration (recyclable), and spin the filtrate at 70°C to remove the solvent (recyclable), and obtain a white prepolymer;

[0036] (2) Take 70 parts of the white prepolymer, add it to the reaction bottle, heat to 85°C and keep stirring, add lipase preparation Novozym4355 parts after the prepolymer is melted, and stop the reaction after 48 hours of bulk polymerization under melting conditions; Add 100 parts of chloroform to dissolve the reaction mixture, filter and recover the enzyme preparation, slowly add the filtrate dropwise to 500 parts of methanol, filter the obtained white solid, and dry i...

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Abstract

The invention discloses a preparation method of poly(butylene succinate). The preparation method comprises the following steps: (1), under catalytic action of lipase, polymerizing an acyl donor and 1,4-butanediol through liquor to obtain a prepolymer, wherein the acryl donor is at least one of succinic acid, dimethyl succinate and diethyl succinate; (2), under the catalytic action of the lipase, polymerizing the prepolymer by virtue of a main body to obtain poly(butylene succinate). The invention provides the preparation method of poly(butylene succinate) with high molecular weight. Compared with the existing technology of synthesizing polyesters in an enzymatic manner, under the condition that material ingredients are the same, the method disclosed by the invention can be used for greatly reducing consumption of energy and dosage of the organic solvent in the processing process, and improving the molecular weight and material performance of a product. Moreover, the method can be used for overcoming a bottleneck of short-chain aliphatic monomer polymerization in an enzymatic manner, obtaining a high molecular product which can be put into practical application; meanwhile, the production cost is lowered by virtue of normal-pressure polymerization, and a basis is provided for industrially producing the polyesters by virtue of an enzyme process.

Description

technical field [0001] The invention relates to a preparation method of polybutylene succinate, belonging to the technical field of preparation methods of biodegradable polyester. Background technique [0002] The problem of global white pollution is becoming more and more serious, and biodegradable plastics have attracted more and more attention. Aliphatic polyester polymer materials have good biocompatibility and degradation performance, and have become the main development direction of biodegradable plastics. Among them, polybutylene succinate (PBS) has become a new type of biodegradable plastic with the most development potential due to its good mechanical properties and heat resistance. The PBS prepared by existing chemical catalysis is difficult to remove due to the strong interaction between the metal catalyst and the polyester, which limits the application range of PBS products. Enzyme-catalyzed synthesis of PBS can solve this problem well. However, in the existin...

Claims

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Application Information

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IPC IPC(8): C12P7/62
Inventor 卢滇楠安思源任立伟林森朱晶莹刘铮
Owner TSINGHUA UNIV
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