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A kind of 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 resistance isosorbide type random copolyester, and can solve the problems of poor heat resistance, low secondary hydroxyl reactivity and the like

Active Publication Date: 2019-08-27
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A kind of preparation method of high heat resistance isosorbide type random copolyester
  • A kind of preparation method of high heat resistance isosorbide type random copolyester
  • A kind of preparation method of high heat resistance isosorbide type random copolyester

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Example 1. Preparation of high heat resistance (terephthalic acid-isosorbide-ethylene glycol) random copolyester by decarbonating ethylene ester method

[0058] (1) Under the protection of 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), the reaction is stirred at 60°C for 2 hours, and then the temperature is gradually raised to 180°C, and the by-product methanol produced by the reaction is evaporated. When the by-product methanol and excess dimethyl carbonate are all distilled off, that is, the reaction is complete, and a prepolymer of isosorbide polycarbonate is obtained;

[0059] (2) In a 250mL reaction vessel, add 41.5g (0.25mol) terephthalic acid and 31.0g (0.5mol) ethylene glycol (the molar ratio of terephthalic acid to ethylene glycol is 1: 2) Start stirring at 160°C, g...

Embodiment 2

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

[0064] (1) Under the protection of 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), the reaction is stirred at 60°C for 2 hours, and then the temperature is gradually raised to 180°C, and the by-product methanol produced by the reaction is evaporated. When the by-product methanol and excess dimethyl carbonate are all distilled off, that is, the reaction is complete, and a prepolymer of isosorbide polycarbonate is obtained;

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

Embodiment 3

[0068] Example 3. Preparation of high heat resistance (terephthalic acid-isosorbide-ethylene glycol) random copolyester by decarbonating ethylene ester method

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

[0070] (2) In a 500mL reaction vessel, add 83.0g (0.5mol) terephthalic acid and 62.0g (1.0mol) ethylene glycol (the molar ratio of terephthalic acid to ethylene glycol is 1: 2) Start stirring at 160°C, gradually rai...

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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 method for preparing isosorbide-type random copolyesters with high heat resistance, that is, a decyclic alkenyl carbonate method, and more specifically, to control the feed ratio of monomers to make the short chain in the intermediate product After forming a ring, the alkylene carbonate is continuously removed from the molecular chain to prepare a high heat resistance isosorbide type random copolyester. Background technique [0002] With the depletion of petroleum resources and the deteriorating environment, the development of renewable and environment-friendly bio-based polymer materials has urgent practical significance. Isosorbide (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-toxicity, and has been used to prepar...

Claims

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Application Information

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Patent Type & Authority Patents(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