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A two-step synthesis method of polyarylene sulfide sulfone at medium temperature

A polyarylene sulfide sulfone and a synthesis method technology are applied in the mid-temperature synthesis of polyarylene sulfide sulfone and the field of polyarylene sulfide sulfone preparation technology, which can solve problems to be improved, and achieve improved polymerization reaction efficiency and excellent heat resistance. and thermal stability and corrosion resistance

Active Publication Date: 2020-07-10
西藏睿兴新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, at present, the yield of polyarylene sulfide sulfone needs to be improved, and the heat resistance, thermal stability and corrosion resistance also need to be improved, which has become a technical problem to be solved urgently.

Method used

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  • A two-step synthesis method of polyarylene sulfide sulfone at medium temperature
  • A two-step synthesis method of polyarylene sulfide sulfone at medium temperature
  • A two-step synthesis method of polyarylene sulfide sulfone at medium temperature

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Experimental program
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Embodiment 1

[0020] In this embodiment, a medium-temperature two-step synthesis method of polyarylene sulfide sulfone includes the following steps:

[0021] a. Pretreatment of raw materials:

[0022] At room temperature, add 592.8 g of 1,3-dimethyl-2-imidazolidinone, Na 2 S·9H 2 O is 480g. Under the protection of an inert atmosphere, the raw materials are stirred evenly, then heated to 130°C, kept for 20 minutes for dehydration, and then cooled to 90°C to obtain a dehydrated mixed raw material;

[0023] b. Carry out a two-step reaction at medium temperature:

[0024] Continue to add catalyst anhydrous CH to the reactor 3 COONa is 4.1g, and another reaction monomer 4,4'-dichlorodiphenyl sulfone is 301.35g to form a reaction system, and then adopt the medium temperature two-step synthesis method of prepolymerization and polymerization to raise the temperature of the reaction system in the reactor To 125°C, stir the reaction system for pre-polymerization for 200 minutes, then rapidly rais...

Embodiment 2

[0030] This embodiment is basically the same as Embodiment 1, especially in that:

[0031] In this embodiment, a medium-temperature two-step synthesis method of polyarylene sulfide sulfone includes the following steps:

[0032] a. Carry out raw material pretreatment: this step is identical with embodiment one;

[0033] b. Carry out a two-step reaction at medium temperature:

[0034] Continue to add catalyst anhydrous CH to the reactor 3 COONa is 4.1g, and another reaction monomer 4,4'-dibromodiphenyl sulfone is 301.35g to form a reaction system, and then adopt the medium temperature two-step synthesis method of prepolymerization and polymerization to raise the temperature of the reaction system in the reactor To 125°C, stir the reaction system for pre-polymerization for 200 minutes, then rapidly raise the temperature to the polymerization reaction temperature of 160°C at a heating rate of 10°C / min, and continue the polymerization for 310 minutes to obtain the reaction produc...

Embodiment 3

[0040] This embodiment is basically the same as the previous embodiment, and the special features are:

[0041] In this embodiment, a medium-temperature two-step synthesis method of polyarylene sulfide sulfone includes the following steps:

[0042] a. Pretreatment of raw materials:

[0043]At room temperature, add 775.2 g of 1,3-dimethyl-2-imidazolidinone, Na 2 S·9H 2 O is 480g. Under the protection of an inert atmosphere, the raw materials are stirred evenly, then heated to 140°C, kept for 35min for dehydration, and then cooled to 90°C to obtain a dehydrated mixed raw material;

[0044] b. Carry out a two-step reaction at medium temperature:

[0045] Continue to add catalyst anhydrous CH to the reactor 3 COONa is 12.3g, and another reaction monomer 4,4'-dichlorodiphenyl sulfone is 430.5g to form a reaction system, and then adopt the medium-temperature two-step synthesis method of prepolymerization and polymerization to raise the temperature of the reaction system in the r...

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Abstract

The invention provides an intermediate temperate two-step synthesis method of poly(arylene sulfide sulfone). A catalyst anhydrous CH3COONa is introduced into a reaction system of sodium sulfide nonahydrate (Na2S.9H2O) and 4,4'-dihalogeno-sulfobenzide; a high-performance aprotic polar solvent 1,3-dimethyl-2-imidazolone is selected as a reaction solvent; firstly, prepolymerization is performed for 200 to 240min at 125 to 140 DEG C; then, the temperature is fast raised to be 160 to 174 DEG C for polymerization for 310 to 360min; the poly(arylene sulfide sulfone) is prepared. The product is an offwhite particulate matter; the yield is 75 percent to 80 percent; the solid residue rate at 700 DEG C is 41 percent to 42 percent. The method has the advantages that the polymerization reaction efficiency is improved; the poly(arylene sulfide sulfone) with excellent performance is synthesized at intermediate temperate.

Description

technical field [0001] The invention relates to a preparation process of polyarylene sulfide sulfone, in particular to a medium temperature synthesis method of polyarylene sulfide sulfone, which is applied in the technical field of polymer material preparation process. Background technique [0002] There are many synthesis methods of polyarylene sulfide sulfone, such as the McFarland method, sodium sulfide method, CPS ring-opening polymerization method, sulfur solution method, etc., but the only method suitable for large-scale industrial production is the sodium sulfide method. This method was first proposed by Phillips Corporation of the United States in the 1980s. At present, the countries that produce polyarylene sulfide sulfone mainly include the United States, Japan and China. The research work mainly focuses on the improvement of production process parameters, such as the choice of solvent and catalyst, the amount of solvent and catalyst, the control of synthesis time ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/23
CPCC08G75/23
Inventor 郭强曹志强刘洪
Owner 西藏睿兴新材料科技有限公司