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A kind of aliphatic polycarbonate copolyester and preparation method thereof

A technology of polycarbonate and copolyester, 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 report To 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: 2020-05-01
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 furandicarboxylate-aliphatic polycarbonate copolyester and its preparation method

Method used

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  • A kind of aliphatic polycarbonate copolyester and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0021] Under normal pressure conditions, at first catalyst 1.32g titanyl acetylacetonate, 140g2,5-furandicarboxylic acid and 270g1.3-propanediol were joined in a 2L reactor equipped with heating and stirring system, temperature measurement system and fractionation system, Introduce nitrogen to remove the air in the reactor, raise the temperature to 140°C under a nitrogen atmosphere, react for 5 hours, and obtain a clear esterification product, then continue to add 345g of diphenyl carbonate, raise the temperature to 190°C for transesterification , reflux reaction for 4 hours, remove the by-product phenol and moisture in the reaction; then, gradually reduce the system pressure to 3000Pa, after a certain period of reaction, gradually increase the system reaction temperature to 195 ° C, reduce the system pressure to 70Pa, polycondensation is terminated after 7 hours The reaction is to obtain aliphatic polycarbonate copolyester.

Embodiment 2

[0023] Under normal pressure conditions, at first the catalyst 0.64g sodium ethylate, 156g2,5-furandicarboxylic acid and 360g1.4-butanediol were added to a 2L reactor equipped with a heating and stirring system, a temperature measuring system and a fractionation system, Introduce nitrogen to remove the air in the reactor, raise the temperature to 160°C under 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 reaction for 3 hours, remove the by-product phenol and moisture in the reaction; then, gradually reduce the system pressure to 2000Pa, after a certain period of reaction, gradually increase the system reaction temperature to 200℃, reduce the system pressure to 80Pa, polycondensation is terminated after 5h The reaction is to obtain aliphatic polycarbonate copolyester.

Embodiment 3

[0025] Under normal pressure conditions, first add the catalyst 0.55g zinc acetylacetonate, 156g 2,5-furandicarboxylic acid and g1.5-pentanediol into a 2L reactor equipped with a heating stirring system, a temperature measuring system and a fractionation system , Introduce nitrogen to remove the air in the reactor, raise the temperature to 130°C under a nitrogen atmosphere, react for 10 hours, and obtain a clear esterification product, then continue to add 321g of diphenyl carbonate, raise the temperature to 185°C for transesterification Reaction, reflux reaction for 5 hours, remove the by-product phenol and moisture in the reaction; then, gradually reduce the system pressure to 1000Pa, after a certain period of reaction, gradually increase the system reaction temperature to 208 ° C, reduce the system pressure to 30Pa, after polycondensation for 10 hours Terminate the reaction to obtain aliphatic polycarbonate copolyester.

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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 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 can be completely biodegraded. It has good physical and mechanical properties, dielectric properties and biocompatibility, and there are many kinds. By changing the chemical structure of the main chain 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 polycarbonates have low melting temperature, low glass transition temperature, and low crystallization temperature, which limit their large-scale appli...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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