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Method for preparing polyester containing isosorbide

A technology of isosorbide polyester and isosorbide, which is applied in the field of preparation of isosorbide-containing polyester, can solve the problems of reducing the content of isosorbide in polyester, rarely using water-carrying agents, and difficult to control the activation step , to achieve the effect of increasing molecular weight, good miscibility and large molecular weight

Active Publication Date: 2013-04-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Esterification polymerization after activation of isosorbide or dibasic acid increases the preparation steps and increases the cost. In addition, the activation step of the monomer is difficult to control; isosorbide polyester directly participates in the esterification reaction, because isosorbide Structural features, often require a higher esterification temperature, not only the esterification effect is poor but also need to add diols other than isosorbide, reducing the content of isosorbide in polyester
As we all know, adding an appropriate amount of water-carrying agent in the esterification reaction of alcohol and acid will improve the esterification effect, but in the esterification reaction in which isosorbide directly participates, because the reaction system and raw materials are different from ordinary esterification reactions, it is necessary to choose It is not easy to find a suitable water-carrying agent, which is why the water-carrying agent is rarely used when isosorbide directly participates in the esterification reaction in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take equimolar isosorbide and maleic acid as raw materials, use 0.01% isosorbide mass percentage of titanium n-butoxide as polycondensation catalyst, and add water-carrying agent methyl isobutyl ketone for mixing, in which methyl isobutyl ketone and The mass ratio of the raw materials is 1:3, then the temperature is raised to 120°C for 2h, and then to 180°C, the vacuum is pumped to 1000~2000Pa, and the reaction is 1h. The relative molecular weight Mn of the obtained polyester is 2500 g / mol (relative to the polymethyl methacrylate standard).

Embodiment 2

[0026] Take equimolar isosorbide and succinic acid as raw materials, use 0.03% isosorbide mass percentage of titanium n-butoxide as polycondensation catalyst, and add water-carrying agent diisobutyl ketone for mixing. The mass ratio of diisobutyl ketone to raw material is The ratio is 1:1, then the temperature is raised to 180°C for 2h, and then to 200°C, the vacuum is pumped to 1000~2000Pa, and the reaction is 2h. The relative molecular weight Mn of the obtained polyester is 4400 g / mol.

Embodiment 3

[0028] Using equimolar isosorbide and succinic acid as raw materials, using isosorbide with a mass percentage of 0.02% titanium n-butoxide as a polycondensation catalyst, and adding water-entraining agent diisobutyl ketone for mixing, wherein the mass ratio of diisobutyl ketone to the raw material The ratio is 1:2, then the temperature is raised to 180°C for 4h, and then to 200°C, the vacuum is pumped to 1000~2000Pa, and the reaction is 4h. The relative molecular weight Mn of the obtained polyester is 7500 g / mol.

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Abstract

The invention discloses a method for preparing a polyester containing isosorbide, comprising the following steps of: carrying out dehydration reaction on raw materials including isosorbide and dicarboxylic acid which have equal molar weight under the action of a polycondensation catalyst and a water-carrying agent under normal pressure, and carrying out a vacuum polycondensation to prepare the polyester containing isosorbide, wherein the water-carrying agent comprises one or more of the methyl isopropyl ketone, ethyl isopropyl ketone, methyl isobutyl ketone, diisopropyl ketone and diisobutyl ketone. According to the method, an appropriate amount of water-carrying agent is added during the direct esterification reaction of the isosorbide and the binary acid, thus the reaction temperature is decreased greatly, and the molecular weight and the polymerization efficiency of the polyester are improved.

Description

Technical field [0001] The invention relates to a preparation method of isosorbide-containing polyester, in particular to a preparation method of isosorbide-containing polyester with higher molecular weight. Background technique [0002] As a dehydration product of sorbitol, isosorbide can be easily prepared from renewable resources such as D-glucose by hydrogenation and then acid-catalyzed dehydration. It has the advantages of abundant raw material sources, degradability and good thermal stability, and has chirality. feature. Polyesters containing isosorbide have higher viscosity and glass transition temperature, better processability, spinnability and dyeability, impact resistance and mechanical strength are further enhanced. Therefore, the polyester can be widely used in products such as bottles, heat-filled containers, films, thick plates, fibers, wires, and optical products. [0003] US6291629B1 and Okada M et al. in "J Appl Polym Sci" Volume 7, Issue 1, P57–70 "Biodegradabl...

Claims

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Application Information

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IPC IPC(8): C08G63/58C08G63/42C08G63/78
Inventor 王鑫黎元生乔凯金平
Owner CHINA PETROLEUM & CHEM CORP
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