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Preparation method of high heat resistance isosorbide type random copolyester

A technology of isosorbide type and isosorbide is applied in the field of preparation of high heat-resistant isosorbide-type random copolyester, and can solve the problems of low reaction activity of secondary hydroxyl group and poor heat resistance, etc.

Active Publication Date: 2017-06-06
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The main purpose of the present invention is to provide a kind of preparation method of novel isosorbide type random copolyester—decycling olefinic ester method, to overcome the secondary hydroxyl reactivity of isosorbide is relatively low or solve product heat resistance poor sex problem

Method used

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  • Preparation method of high heat resistance isosorbide type random copolyester
  • Preparation method of high heat resistance isosorbide type random copolyester
  • Preparation method of high heat resistance isosorbide type random copolyester

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Embodiment 1. Preparation of high heat resistance (terephthalic acid-isosorbide-ethylene glycol) random copolyester by removing ethylene carbonate

[0058] (1) Under the protection of a nitrogen atmosphere, in a 250mL reaction vessel, add 29.2g (0.2mol) isosorbide, 90.0g (1.0mol) dimethyl carbonate and 0.0066g transesterification catalyst lithium acetylacetonate, (isosorbide The molar ratio of alcohol to dimethyl carbonate is 1:5), stirred and reacted at 60°C for 2 hours, then gradually raised the temperature to 180°C, and distilled out the by-product methanol produced by the reaction. After the by-product methanol and excess dimethyl carbonate are all distilled off, the reaction is complete to obtain a prepolymer of isosorbide polycarbonate;

[0059] (2) In a 250mL reaction vessel, add 41.5g (0.25mol) of terephthalic acid and 31.0g (0.5mol) of ethylene glycol under a nitrogen atmosphere (the molar ratio of terephthalic acid to ethylene glycol is 1: 2) Start stirring a...

Embodiment 2

[0063] Embodiment 2. Preparation of high heat resistance (terephthalic acid-isosorbide-ethylene glycol) random copolyester by decarbonating ethylene ester method

[0064] (1) Under the protection of a nitrogen atmosphere, in a 250mL reaction vessel, add 29.2g (0.2mol) isosorbide, 90.0g (1.0mol) dimethyl carbonate and 0.0066g transesterification catalyst lithium acetylacetonate, (isosorbide The molar ratio of alcohol to dimethyl carbonate is 1:5), stirred and reacted at 60°C for 2 hours, then gradually raised the temperature to 180°C, and distilled out the by-product methanol produced by the reaction. After the by-product methanol and excess dimethyl carbonate are all distilled off, the reaction is complete to obtain a prepolymer of isosorbide polycarbonate;

[0065] (2) In a 500mL reaction vessel, add 49.8g (0.3mol) of terephthalic acid and 37.2g (0.6mol) of ethylene glycol under a nitrogen atmosphere (the molar ratio of terephthalic acid to ethylene glycol is 1: 2) Start sti...

Embodiment 3

[0068] Embodiment 3. Decarboxylation method prepares high heat resistance (terephthalic acid-isosorbide-ethylene glycol) random copolyester

[0069] (1) Under nitrogen atmosphere protection, in the reaction container of 500mL, add 29.2g (0.2mol) isosorbide, 214.0g (1.0mol) diphenyl carbonate and 0.0066g transesterification catalyst lithium acetate, (isosorbide The molar ratio of diphenyl carbonate to diphenyl carbonate is 1:5), the stirring reaction was carried out at 60°C for 2 hours, and then the temperature was gradually raised to 200°C, and the by-product methanol produced by the reaction was distilled off. After the by-product methanol and excess diphenyl carbonate are all distilled off, the reaction is complete to obtain a prepolymer of isosorbide polycarbonate;

[0070] (2) In a 500mL reaction vessel, add 83.0g (0.5mol) of terephthalic acid and 62.0g (1.0mol) of ethylene glycol under a nitrogen atmosphere (the molar ratio of terephthalic acid to ethylene glycol is 1: 2...

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Abstract

The invention relates to a preparation method of high heat resistance isosorbide type random copolyester. As for the high heat resistance isosorbide type random copolyester, by controlling the feed molar ratio of a monomer, a short-chain alkyl carbonate structure is constructed between aromatic dibasic acid and isosorbide, and then cyclic allyl ester carbonate is removed under a certain condition to realize linkage of the aromatic dibasic acid and an isosorbide structure unit. The prepared isosorbide type random copolyester has high glass transition temperature which decides that the high heat resistance isosorbide type random copolyester has good heat resistance and is low in preparation cost and environment-friendly in preparation process. The random copolyester has the viscosity being 0.6-1.0dL / g and the glass transition temperature being 90-190 DEG C, is excellent in comprehensive performance and can be used for preparing polymer blends, polymer alloy, heat resistant vessels, bottles, films, fibers, sheets, optical products and the like.

Description

technical field [0001] The present invention relates to a kind of preparation method of high heat-resistant isosorbide type random copolyester, that is, the method of decycling olefinic ester carbonate, more specifically relates to by controlling the charging ratio of monomer, make the short chain in intermediate product After forming a ring, the olefinic ester is continuously removed from the molecular chain to prepare a high heat-resistant isosorbide random copolyester. Background technique [0002] With the depletion of petroleum resources and the deterioration of the environment, it is of urgent practical significance to develop bio-based polymer materials with renewable raw materials and environmental friendliness. Isosorbide, namely 1,4:3,6-dianhydro-D-glucitol, is derived from sorbitol through two-step dehydration. As the only sugar diol that has achieved mass industrial production, isosorbide has the advantages of abundant raw material sources, rigidity and non-toxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/42C08G64/30C08G64/38
Inventor 欧阳庆李春成刘佳健孟现明张栋张博肖耀南
Owner INST OF CHEM CHINESE ACAD OF SCI
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