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Method for preparing polyphenyl ether thioether through sulfoxide reduction

A technology of polyphenylene ether and sulfide, which is applied in the field of preparation of polyphenylene ether sulfide, can solve the problems of further improvement in yield, long reaction time, and high reaction temperature, and achieve shortened production cycle, shortened reaction time, and high reaction temperature. Reduced effect

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

[0003] Patent ZL200710049609.8 discloses "a preparation method of polyphenylene ether sulfide". Ether is the raw material, and the aprotic polar solvent is the reaction medium. Under the action of the catalyst, polyphenylene ether sulfides of different molecular weight grades with an intrinsic viscosity of 0.2~0.5 dL / g are synthesized, but this method requires a certain pressure in a closed container. The reaction is carried out under the conditions (using the pressure generated by the reaction), and the reaction time is longer (4-10 hours), the reaction temperature is higher (180-350 ° C), the prepared polyphenylene ether sulfide molecular weight, thermal stability, product rate needs to be further improved

Method used

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  • Method for preparing polyphenyl ether thioether through sulfoxide reduction
  • Method for preparing polyphenyl ether thioether through sulfoxide reduction
  • Method for preparing polyphenyl ether thioether through sulfoxide reduction

Examples

Experimental program
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Effect test

Embodiment 1

[0059] 1. Preparation of poly(phenylene ether sulfide sulfoxide)

[0060] Raw material and formula

[0061] 4,4′-dihydroxydiphenyl sulfide 65.4g (0.30mol)

[0062] 4,4'-Difluorodiphenylsulfoxide 71.4g (0.30mol)

[0063] Anhydrous potassium carbonate 37.1g (0.35mol)

[0064] Sodium formate 5.9g (0.086mol)

[0065] Copper powder 2.2g (0.034mol)

[0066] N,N'-Dimethylacetamide 600mL

[0067] Xylene 100mL;

[0068] The process steps are as follows:

[0069] (1) Polymerization reaction

[0070] Under the protection of nitrogen, the reaction monomer 4,4′-dihydroxydiphenylsulfide, 4,4′-difluorodiphenylsulfoxide, anhydrous potassium carbonate, sodium formate, copper powder, Add N,N'-dimethylacetamide and xylene into the reactor 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 , the reaction time is 24 hours, when the reaction ends, stop stirring after naturally co...

Embodiment 2

[0086] 1. Preparation of poly(phenylene ether sulfide sulfoxide)

[0087] Raw material and formula

[0088] 4,4'-dihydroxydiphenyl sulfide 65.4g (0.30mol)

[0089] 4,4'-Difluorodiphenylsulfoxide 71.4g (0.30mol)

[0090] Anhydrous potassium carbonate 45.54g (0.33mol)

[0091] Sodium Benzoate 4.6g (0.032mol )

[0092] Zinc powder 1.95g (0.03mol)

[0093] N-Methylpyrrolidone 400mL

[0094] Toluene 90mL;

[0095] The process steps are as follows:

[0096] (1) Polymerization reaction

[0097] Under the protection of nitrogen, the reaction monomer 4,4'-dihydroxydiphenyl sulfide, 4,4'-difluorodiphenyl sulfoxide, anhydrous potassium carbonate, sodium benzoate, zinc powder , N-methylpyrrolidone and toluene were added to the reactor and stirred, heated and dehydrated at a heating rate of 0.5°C / min. When the temperature reached 130°C, the dehydration was completed, and then the temperature was raised to 190°C for polymerization. The reaction time was 7 Hour, when reaction finish...

Embodiment 3

[0110] 1. Preparation of poly(phenylene ether sulfide sulfoxide)

[0111] Raw material and its formula

[0112] 4,4′-dihydroxydiphenyl sulfide 64.10g (0.294mol)

[0113] 4,4'-Difluorodiphenylsulfoxide 71.4g (0.30mol)

[0114] Anhydrous sodium carbonate 37.1g (0.35mol)

[0115] Trisodium phosphate 8.2g (0.03mol)

[0116] Cuprous oxide 4.3g (0.03mol)

[0117] Sulfolane 500mL

[0118] Xylene 140mL;

[0119] The process steps are as follows:

[0120] (1) Polymerization reaction

[0121] Under the protection of nitrogen, the reaction monomer 4,4'-dihydroxydiphenylsulfide, 4,4'-difluorodiphenylsulfoxide, anhydrous sodium carbonate, trisodium phosphate, oxidation Add cuprous, sulfolane and xylene into the reaction kettle and stir, heat and dehydrate at a heating rate of 0.5°C / min, complete dehydration when the temperature reaches 140°C, then heat up to 220°C for polymerization reaction, the reaction time is 6 hours , when the reaction is over, stop stirring after naturally c...

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Abstract

The invention discloses a method for preparing polyphenyl ether thioether through sulfoxide reduction. The method adopts the following ingredients in parts by weight: 21-40 parts of polyphenyl ether thioether sulfoxide, 44-88 parts of tetrabutyl ammonium iodide, 28-60 parts of assistant, 950-1300 parts by volume of solvent, and 5-10 parts by volume of oxalyl chloride; the process comprises the following steps of: (1) adding the polyphenyl ether thioether sulfoxide, the tetrabutyl ammonium iodide, the assistant and the solvents into a reaction container and stirring under the protection of the nitrogen at the room temperature, when the polyphenyl ether thioether sulfoxide, the tetrabutyl ammonium iodide, the assistant and the solvents are completely dissolved to be mixture liquid, heating the mixture liquid till the temperature being 50-60 DEG C, adding the oxalyl chloride, and after the oxalyl chloride is added, reacting for 45-60 minutes at 50-60 DEG C, after the reaction is ended, cooling naturally to the room temperature and stopping stirring; and (2) carrying out purification to the product of the synthetic reaction.

Description

technical field [0001] The invention belongs to the field of polyphenylene ether sulfide preparation, in particular to a preparation method of polyphenylene ether sulfide. Background technique [0002] Polyphenylene ether sulfide [Poly(oxy-1,4-phenylenethio-1,4-phenylene), referred to as PPSE] is a heat-resistant high-performance polymer with both polyphenylene sulfide and polyphenylene ether structures. It can be traced back to the 1970s, mainly using nucleophilic and electrophilic substitution methods for synthesis. The synthesis operation of the electrophilic substitution method is cumbersome, often accompanied by many side reactions, and the yield is low, and the synthesized polymer often contains diphenyl disulfide bonds, which has no industrial production value. The nucleophilic substitution method needs to be carried out under high temperature or high pressure conditions, and the molecular weight of the obtained product is relatively low. [0003] Patent ZL20071004...

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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