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A kind of multi-block copolyester and its preparation method and the preparation method of its compound

A copolyester and multi-block technology, applied in the field of er-reacted multi-block copolyester, can solve the problem that the content of Diels-Alder bonds in the polyurethane molecular chain cannot be easily regulated, limit the adjustability of final material properties, and limit furan The number of rings and other issues can be improved to improve heat resistance, good repeatability and formability, and simple synthesis steps.

Active Publication Date: 2018-08-28
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are following two disadvantages in the disclosed method of this patent: the first, the preparation method is complicated
Second, the content of Diels-Alder bonds in the final polyurethane molecular chain cannot be easily adjusted
This greatly limits the performance tunability of the final material
[0006] At present, in the studies of Diels-Alder reaction between the furan ring and the dienophile reported in the literature, the furan ring, as the reaction site, is mostly located at the end of the polymer molecular chain or on the side chain of the molecular chain, which not only greatly limits The number of furan rings as reaction sites is limited, and the synthesis steps are relatively complicated (such as connecting the furan rings as side groups to the molecular chain)

Method used

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  • A kind of multi-block copolyester and its preparation method and the preparation method of its compound
  • A kind of multi-block copolyester and its preparation method and the preparation method of its compound
  • A kind of multi-block copolyester and its preparation method and the preparation method of its compound

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preparation example Construction

[0045] The preparation method of the multi-block copolyester that the present invention proposes comprises the following steps:

[0046] (1) Solution polymerization:

[0047] (1-1) Evenly mix dibasic alcohol and dibasic acid, wherein, the molar weight of dibasic alcohol is 1.05-1.3 times of dibasic acid molar weight, pass into inert gas protection, add catalyst, the addition amount of catalyst is two 5%-15% of the molar weight of the basic acid, the catalyst is 4-methylaminopyridine, and the stirring is started until the reactants are completely dissolved to obtain the first solution;

[0048] (1-2) In the first solution of the above-mentioned step (1-1), add dehydrating agent in 3-5 times, the addition of dehydrating agent is 100%-200% of dibasic acid molar weight, described dehydrating agent N,N'-dicyclohexylcarbodiimide, N,N'-diisopropylcarbodiimide, N-hydroxysuccinimide, N-hydroxysulfosuccinimide or 1-(3 -One or more of dimethylaminopropyl)-3-ethylcarbodiimide hydrochlor...

Embodiment 1

[0065] Add 0.4 mol of succinic acid and 0.44 mol of 2,5-furandimethanol into 500 ml of dichloromethane and mix evenly, pass through nitrogen protection, add 0.02 mol of 4-methylaminopyridine as a catalyst, and start stirring until the reactants are completely dissolved. 0.8 mol of dehydrating agent N,N-dicyclohexylcarbodiimide was added to the solution in the above step in four times, and the addition time was 0 hour, 3 hours, 6 hours and 9 hours after the reaction started, and 0.2 mol was added each time. Reaction at normal temperature, the reaction time is 12 hours. Purify to obtain hydroxyl-terminated polysuccinate 2,5-furandimethanol oligomer;

[0066] Add 0.6 mol of succinic acid and 0.66 mol of 1,4-butanediol into 500 ml of dichloromethane and mix evenly, pass through nitrogen protection, add 0.02 mol of 4-methylaminopyridine as a catalyst, and start stirring until the reactants are completely dissolved. 1.2 moles of dehydrating agent N,N-dicyclohexylcarbodiimide was ad...

Embodiment 2

[0069] Add 0.4 moles of terephthalic acid and 0.42 moles of 2,5-furandimethanol into 500 ml of dichloromethane and mix evenly, pass through nitrogen protection, add 0.06 moles of 4-methylaminopyridine as a catalyst, start stirring until the reactants are completely dissolved . Add 0.8 moles of dehydrating agent N,N'-diisopropylcarbodiimide to the solution in the above steps in four times, the addition time is 0 hour, 3 hours, 6 hours and 9 hours after the reaction starts, and add 0.2 moles each time . Reaction at normal temperature, the reaction time is 24 hours. Purify to obtain hydroxyl-terminated poly(2,5-furandimethylene terephthalate) oligomer;

[0070] Add 0.6 mol of terephthalic acid and 0.66 mol of ethylene glycol into 500 ml of dichloromethane and mix evenly, pass through nitrogen protection, add 0.09 mol of 4-methylaminopyridine as a catalyst, and start stirring until the reactants are completely dissolved. Add 1.2 moles of dehydrating agent N,N'-diisopropylcarbod...

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Abstract

The invention relates to a multi-block copolyester, a preparation method of the multi-block copolyester and a preparation method of a compound of the multi-block copolyester, especially relates to a multi-block copolyester which contains a furan ring in a molecular main chain undergoing a Diels-Alder reaction, and belongs to the technical field of polyester material preparation. The furan ring in the molecular main chain of the multi-block copolyester can undergo a Diels-Alder reaction and a reverse Diels-Alder reaction. The multi-block copolyester has excellent thermosetting resin performances and wide performance adjustability at a room temperature and has good processing molding performances of thermoplastic resin at a high temperature. The thermoplastic crosslinked polyester has a property of self-repairing micro-cracks in a wide temperature zone and can be used in fields of mulching films and packaging materials.

Description

technical field [0001] The present invention relates to a kind of multi-block copolyester and its preparation method and the preparation method of its compound, especially relate to a kind of multi-block copolyester whose main chain contains furan ring and its preparation method and its compound preparation method , particularly relates to a multi-block copolyester which contains a furan ring in the molecular main chain and can undergo Diels-Alder reaction, and belongs to the technical field of polyester material preparation. Background technique [0002] Due to its good comprehensive properties, polyester is widely used in electrical, electronic, chemical, packaging and other fields. Compared with thermoplastic resins, thermosetting resins are cross-linked between molecules to form a network structure, so they have the characteristics of high temperature resistance, high hardness, high rigidity, and good dimensional stability of products. However, due to the irreversibilit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/685C08G63/58C08L67/06C08K5/3415
CPCC08G63/58C08G63/6858C08K5/3415C08L2312/00C08L67/06
Inventor 郭宝华张旸徐军
Owner TSINGHUA UNIV
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