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Functional boron-containing polyarylene sulfide copolymer and preparation method thereof

A technology of polyarylene sulfide and copolymer, which is applied in the field of polymer synthesis, can solve problems such as interface instability and phase separation, and achieve the effects of enhancing different characteristics, expanding functional characteristics, and excellent neutron shielding performance

Active Publication Date: 2020-12-01
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the above-mentioned defects, the present invention provides a boron-containing polyarylene sulfide copolymer, which overcomes the defects of the existing composite materials such as unstable interface and phase separation after long-term use; in addition, the obtained boron-containing polyarylene sulfide copolymer It also has thermal neutron shielding properties

Method used

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  • Functional boron-containing polyarylene sulfide copolymer and preparation method thereof
  • Functional boron-containing polyarylene sulfide copolymer and preparation method thereof
  • Functional boron-containing polyarylene sulfide copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Add 19.08g (0.1mol) of 2,4-dichlorophenylboronic acid, 25.32g (0.1mol) of diphenyldichlorosilane and 20ml of N-methylpyrrolidone into a 250ml three-necked flask, and stir at 120°C under nitrogen protection React for 6 hours, then add 7.39g (0.2mol) lithium hydroxide and react for 1 hour; after the reaction, add deionized water to precipitate the product, filter, wash, and dry in vacuum at 120°C for 24 hours to obtain 33g of monomer M 1 , 90% yield.

[0048] Add 1g of sodium hydroxide, 1g of sodium formate, 1g of stannous octoate, 63.5g of sodium sulfide and 100ml of N-methylpyrrolidone into a 1L reaction kettle, dehydrate at 160°C for 3 hours, fractionate 24ml of water; the temperature of the reaction solution drops to 140°C, Add 66.15g (0.45mol) of 1,4 dichlorobenzene, M 1 18.56g (0.05mol), heat up to 200°C for 4 hours, continue to heat up to 220°C for 6 hours; after the reaction, wash with deionized water, filter, and vacuum dry at 120°C for 24 hours to obtain the h...

Embodiment 2

[0050] Add 19.0g (0.1mol) of 3,5-dichlorophenylboronic acid, 25.32g (0.1mol) of diphenyldichlorosilane and 40ml of N-cyclohexylpyrrolidone into a 250ml three-necked flask, and stir at 160°C under nitrogen protection React for 5 hours, then add 7.39g (0.1mol) lithium carbonate and react for 1 hour; after the reaction, add deionized water to precipitate the product, filter, wash, and dry in vacuum at 120°C for 24 hours to obtain the monomer M 2 33 g, 91% yield.

[0051] Add 8g of sodium bicarbonate, 8g of calcium chloride, 16g of sodium glycolate, 63.5g of sodium sulfide and 300ml of dimethyl sulfoxide into a 1L reaction kettle, dehydrate at 180°C for 1 hour, and fractionate 24ml of water; the temperature of the reaction solution drops to 100 ℃, add 100.40g (0.45mol) of 4,4'dichlorobiphenyl, M 2 18.56 g (0.05 mol), the temperature was raised to 230°C for 4 hours, and the temperature was further raised to 260°C for 2 hours. After the reaction, wash with deionized water, filte...

Embodiment 3

[0053] Add 19.08g (0.1mol) of 2,5-dichlorophenylboronic acid, 20.30g (0.10mol) of diphenyldichlorosilane and 60ml of N,N-dimethylacetamide into a 250ml three-necked flask, under nitrogen protection, Stir and react at 180°C for 4 hours, then add 7.39g (0.1mol) lithium carbonate and react for 1 hour; after the reaction, add deionized water to precipitate the product, filter, wash, and dry in vacuum at 120°C for 24 hours to obtain the monomer M 3 31 g, 86% yield.

[0054] Add 8g of sodium hydroxide, 8g of sodium formate, 16g of stannous octoate, 63.5g of sodium sulfide and 300ml of N-methylpyrrolidone into a 1L reaction kettle, dehydrate at 180°C for 1 hour, and fractionate 24ml of water; when the temperature of the reaction solution drops to 100°C, Add 66.15g (0.45mol) of 1,4 dichlorobenzene, M 3 18.56g (0.05mol), the temperature was raised to 230°C for 2 hours, and the temperature was further raised to 270°C for 4 hours. After the reaction, wash with deionized water, filter...

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Abstract

The invention relates to a high-molecular-weight polyarylene sulfide functional copolymer containing a boron element on a molecular chain, and a preparation method thereof, and belongs to the field ofpolymer synthesis. The structural formula of the boron-containing polyarylene sulfide copolymer is represented by formula I; and in the formula I, n is more than or equal to 0 and less than or equalto 100, and m is more than 0 and less than or equal to 100. According to the boron-containing polyarylene sulfide copolymer, due to the fact that the molecular chain contains the boron element, the defects that an existing composite material is unstable in interface, phase separation occurs after long-term use and the like are overcome; and in addition, the obtained boron-containing polyarylene sulfide copolymer also has thermal neutron shielding performance.

Description

technical field [0001] The invention relates to a class of high molecular weight polyarylene sulfide functional copolymers containing boron elements in molecular chains and a preparation method thereof, belonging to the field of polymer synthesis. Background technique [0002] Polyarylene sulfide, such as polyphenylene sulfide (PPS), has good mechanical properties, dimensional stability, radiation resistance, heat resistance, and chemical resistance, and is widely used in automotive, electronics, medical, aerospace and other fields . The synthesis and preparation of polyarylene sulfide develops rapidly. For example, US Patent No. 33544129 reports that sodium sulfide and dichlorobenzene are used as raw materials to synthesize high molecular weight PPS resin in polar solvents such as amine, lactam, sulfone or sulfone analogs. Chinese Patent Publication Nos. CN103087523A, CN1145375A, CN1145376A, CN1793202A also reported that sodium sulfide and p-dichlorobenzene were used as ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0254C08G75/0213
CPCC08G75/0254C08G75/0213
Inventor 严永刚焦雪菲李鹏程严大卫任浩浩张刚杨杰
Owner SICHUAN UNIV