Aliphatic polycarbonate copolyester and preparation method thereof

A polycarbonate and aliphatic technology, applied in the field of high molecular weight aliphatic polycarbonate copolyester and its preparation, can solve the problem of furandicarboxylate-aliphatic polycarbonate copolyester preparation method without patent reports, etc. problems, achieve the effects of shortening the reaction time of transesterification, reducing the amount of catalyst used, improving thermodynamic properties and processing performance

Active Publication Date: 2017-12-15
CHANGZHOU INST OF CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no domestic patent report of furandicarboxyl

Method used

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  • Aliphatic polycarbonate copolyester and preparation method thereof
  • Aliphatic polycarbonate copolyester and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Under normal pressure conditions, firstly add 1.32g titanium acetylacetonate catalyst, 140g 2,5-furandicarboxylic acid and 270g 1.3-propanediol into a 2L reactor equipped with heating and stirring system, temperature measurement system and fractionation system. Blow in nitrogen to remove the air in the reactor, raise the temperature to 140°C under a nitrogen atmosphere, and react for 5 hours to obtain a clear esterified product. Then continue to add 345g of diphenyl carbonate, and raise the temperature to 190°C for transesterification. Reflux for 4 hours to remove the by-product phenol and moisture in the reaction; then, gradually reduce the pressure of the system to 3000Pa, after a certain time of reaction, gradually increase the reaction temperature of the system to 195℃, reduce the pressure of the system to 70Pa, and terminate the polycondensation after 7h The reaction is to obtain aliphatic polycarbonate copolyester.

Embodiment 2

[0023] Under normal pressure conditions, first add the catalyst 0.64g sodium ethoxide, 156g 2,5-furandicarboxylic acid and 360g 1.4-butanediol into a 2L reactor equipped with heating and stirring system, temperature measurement system and fractionation system. Blow in nitrogen to remove the air in the reactor, raise the temperature to 160°C under a nitrogen atmosphere, and react for 5 hours to obtain a clear esterification product. Then continue to add 428g of diphenyl carbonate, and raise the temperature to 180°C for transesterification. Reflux for 3h to remove the by-product phenol and moisture in the reaction; then, gradually reduce the pressure of the system to 2000Pa, after a certain time of reaction, gradually increase the reaction temperature of the system to 200℃, reduce the pressure of the system to 80Pa, and terminate the polycondensation after 5h The reaction is to obtain aliphatic polycarbonate copolyester.

Embodiment 3

[0025] Under normal pressure conditions, first add 0.55g zinc acetylacetonate as catalyst, 156g 2,5-furandicarboxylic acid and 1.5-pentanediol into a 2L reactor equipped with heating and stirring system, temperature measurement system and fractionation system , Blow in nitrogen to remove the air in the reactor, raise the temperature to 130°C under a nitrogen atmosphere, react for 10 hours to obtain a clear esterified product, then continue to add 321g of diphenyl carbonate, and raise the temperature to 185°C for transesterification Reaction, reflux reaction for 5h, remove the by-product phenol and moisture in the reaction; then, gradually reduce the pressure of the system to 1000Pa, after a certain time of reaction, gradually increase the reaction temperature of the system to 208℃, reduce the pressure of the system to 30Pa, and after polycondensation for 10h The aliphatic polycarbonate copolyester is obtained by terminating the reaction.

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Abstract

The invention discloses a high molecular weight aliphatic polycarbonate copolyester and a preparation method thereof, and relates to a multi-step ester exchange reaction and a high-temperature high-vacuum polycondensation reaction of aliphatic polyhydric alcohols, 2,5-furandicarboxylic acid and carbonic acid aryl esters. The ester exchange reaction and the polycondensation reaction are implemented continuously, so that the ester exchange reaction time is shortened, the equipment utilization rate is improved, no extra catalyst is needed before polycondensation, and thus the experiment steps are simplified. According to the copolyester disclosed by the invention, furandicarboxylic acid polyester structure units or chain segments are introduced into aliphatic polycarbonate main chains, so that the copolyester has the biodegradation of the aliphatic polycarbonate and excellent thermodynamic and processing proprieties of the furandicarboxylic acid polyester simultaneously, defects that the aliphatic polycarbonate is low in glass-transition temperature, low in melting temperature, low in crystallization temperature and the like are overcome, and requirements of different industries are met.

Description

Technical field [0001] The invention relates to a high molecular weight aliphatic polycarbonate copolyester and a preparation method thereof, and a method for preparing a high molecular weight aliphatic polycarbonate copolyester through two-step transesterification and high temperature and high vacuum polycondensation. Background technique [0002] Aliphatic polycarbonate is an important part of polyester polymer. It is a kind of surface erosion material, which is completely biodegradable, has good physical and mechanical properties, dielectric properties and biocompatibility, and has a wide variety of materials. By changing the main chain chemical structure and introducing side chain functional groups, the polymer can have a wide range of physical, chemical and biological properties to meet different needs. However, aliphatic polycarbonate has low melting temperature, low glass transition temperature, and low crystallization temperature, which limit its large-scale application. ...

Claims

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Application Information

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IPC IPC(8): C08G63/64C08G63/78
CPCC08G63/64C08G63/78
Inventor 李会玲王红丹王兴祥彭丽君
Owner CHANGZHOU INST OF CHEM
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