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Polyphenyl ether thioether sulfoxide and preparation method thereof

A technology of polyphenylene ether and dihalodiphenyl sulfoxide, which is applied in the field of polyphenylene ether sulfide sulfoxide and its preparation, can solve problems such as difficult to meet, and achieve the effects of simplified process, high yield, and good solution processing performance

Active Publication Date: 2012-11-14
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In heat-resistant special engineering plastics, polyarylether has been widely used in many important fields due to its excellent performance. Commonly used polyarylethers are mainly polyarylether ketone and polyarylether sulfone. Although they have their own advantages, However, it is difficult to meet the more requirements or comprehensive performance requirements of the development of science and technology for heat-resistant special engineering plastics. Among them, high-performance polymers that integrate thermal stability, ease of processing and functionalization are heat-resistant special engineering plastics. An important direction of development

Method used

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  • Polyphenyl ether thioether sulfoxide and preparation method thereof
  • Polyphenyl ether thioether sulfoxide and preparation method thereof
  • Polyphenyl ether thioether sulfoxide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1. Raw material and its formula

[0039] 4,4′-dihydroxydiphenyl sulfide 65.4g (0.30mol)

[0040] 4,4'-Difluorodiphenylsulfoxide 71.4g (0.30mol)

[0041] Anhydrous potassium carbonate 37.1g (0.35mol)

[0042] Sodium formate 5.9g (0.086mol)

[0043] Copper powder 2.2g (0.034mol)

[0044] N,N'-Dimethylacetamide 600mL

[0045] Xylene 100mL;

[0046] 2. The process steps are as follows:

[0047] (1) Polymerization reaction

[0048] Under the protection of nitrogen, the reaction monomer 4,4'-dihydroxydiphenylsulfide, 4,4'-difluorodiphenylsulfoxide, anhydrous potassium carbonate, sodium formate, copper powder, N, Add N'-dimethylacetamide and xylene into the reaction kettle and stir, heat and dehydrate at a heating rate of 0.6°C / min, complete dehydration when the temperature reaches 140°C, and then heat up to 170°C for polymerization reaction, reaction The time is 24 hours, when the reaction finishes, stop stirring after naturally cooling to room temperature;

[0049] ...

Embodiment 2

[0055] 1. Raw material and its formula

[0056] 4,4′-dihydroxydiphenyl sulfide 64.10g (0.294mol)

[0057] 4,4'-Difluorodiphenylsulfoxide 71.4g (0.30mol)

[0058] Anhydrous sodium carbonate 37.1g (0.35mol)

[0059] Trisodium phosphate 8.2g (0.03mol)

[0060] Cuprous oxide 4.3g (0.03mol)

[0061] Sulfolane 500mL

[0062] Xylene 140mL;

[0063] 2. The process steps are as follows:

[0064] (1) Polymerization reaction

[0065] Under the protection of nitrogen, the reaction monomer 4,4'-dihydroxydiphenyl sulfide, 4,4'-difluorodiphenyl sulfoxide, anhydrous sodium carbonate, trisodium phosphate, cuprous oxide , sulfolane and xylene are added to the reaction kettle and stirred, heated and dehydrated at a heating rate of 0.5°C / min. When the temperature reaches 140°C, the dehydration is completed, and then the temperature is raised to 220°C for polymerization. The reaction time is 6 hours. Reaction finishes, stops stirring after naturally cooling to room temperature;

[0066] (...

Embodiment 3

[0069] 1. Raw material and its formula

[0070] 4,4′-dihydroxydiphenyl sulfide 64.75g (0.297mol)

[0071] 4,4'-Difluorodiphenylsulfoxide 71.4g (0.30mol)

[0072] Anhydrous sodium hydroxide 30g (0.75mol)

[0073] Sodium p-toluenesulfonate 9.7g (0.05mol)

[0074] Cuprous oxide 5.8g (0.04mol)

[0075] Hexamethylphosphoric triamide 450mL

[0076] Toluene 120mL;

[0077] 2. The process steps are as follows:

[0078] (1) Polymerization reaction

[0079] Under the protection of nitrogen, the reaction monomer 4,4'-dihydroxydiphenylsulfide, 4,4'-difluorodiphenylsulfoxide, anhydrous sodium hydroxide, sodium p-toluenesulfonate, Add cuprous oxide, hexamethylphosphoric triamide and toluene into the reaction kettle and stir, heat and dehydrate at a heating rate of 0.6°C / min, complete dehydration when the temperature reaches 130°C, and then heat up to 200°C for polymerization , the reaction time is 14 hours, when the reaction ends, stop stirring after naturally cooling to room temper...

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Abstract

The invention discloses a preparation method of polyphenyl ether thioether sulfoxide. The polyphenyl ether thioether sulfoxide comprises the following ingredients: 4,4'-dyhydroxy diphenyl sulfide and 4,4'-dihalogen diphenylsulfoxide as the reaction monomer of which the mole ratio is 1: 1.02, 1.1-2.5mole / mole of 4,4'-dyhydroxy diphenyl sulfide as the assistant, 0.1-0.5 mole / mole of 4,4'-dyhydroxy diphenyl sulfide as the catalyst, 1000-2000ml / mole of 4,4'-dyhydroxy diphenyl sulfide as the solvent, and 300-500ml / mole of 4,4'-dyhydroxy diphenyl sulfide as the azeotropy dehydrating agent. The process comprises the following steps of: (1) adding the ingredients into a reaction contain and stirring under the protection of nitrogen at the room temperature, rising the temperature, heating, and dehydrating, ending the dehydration when the temperature reaches 130-150 DEG C, subsequently rising the temperature to 170-220 DEG C and carrying out the polymerization reaction, when the reaction is ended, cooling naturally to the room temperature and stopping stirring; and (2) pouring the mixture liquid formed by the polymerization reaction into precipitating agent, precipitating and filtering so as to obtain a filter cake, washing the filter cake and drying in vacuum so as to obtain the polyphenyl ether thioether sulfoxide; and the structural formula is: (FORMULA).

Description

technical field [0001] The invention belongs to the field of heat-resistant engineering plastics, in particular to polyphenylene ether sulfoxide and a preparation method thereof. Background technique [0002] In heat-resistant special engineering plastics, polyarylether has been widely used in many important fields due to its excellent performance. Commonly used polyarylethers are mainly polyarylether ketone and polyarylether sulfone. Although they have their own advantages, However, it is difficult to meet the more requirements or comprehensive performance requirements of the development of science and technology for heat-resistant special engineering plastics. Among them, high-performance polymers that integrate thermal stability, ease of processing and functionalization are heat-resistant special engineering plastics. An important direction of development. Contents of the invention [0003] The purpose of the present invention is to overcome the deficiencies of the pri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/18
Inventor 顾爱群余自力李佐才
Owner SICHUAN UNIV
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