Method for preparing polyphenylene oxide sulfide

A technology of polyphenylene ether and dihalogenated diphenyl sulfide, which is applied in the field of preparation of polyphenylene ether sulfide, can solve the problems of low melting point of PPSE, poor PPSE purity, long reaction time, etc., and achieves easy raw materials and short polymerization reaction time. , good thermal stability

Inactive Publication Date: 2007-12-26
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] As can be seen from the above technical scheme, the polymer PPSE melting point prepared by the existing nucleophilic substitution method is generally low, although the melting point of some PPSE has reached 340 ° C, but the reaction time is long (20 hours), and the productive rate is low ( 50%), some PPSEs have poor purity and have more disulfide bonds

Method used

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  • Method for preparing polyphenylene oxide sulfide
  • Method for preparing polyphenylene oxide sulfide
  • Method for preparing polyphenylene oxide sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. Raw material and its formula

[0042] Reactive monomer 4,4'-dihydroxydiphenyl sulfide (DHPS) 109g (0.5mol)

[0043] Reactive monomer 4,4'-dichlorodiphenylsulfide (DCPS) 127.5g (0.5mol)

[0044] Anhydrous Na 2 CO 3 21.2g (0.2mol)

[0045] Anhydrous K 2 CO 3 55.2g (0.4mol)

[0046] Sodium benzoate 7.5g (0.052mol)

[0047] Zinc powder 6.5g (0.1mol)

[0048] Sulfolane 200mL

[0049] Toluene 100mL

[0050] 2. Process steps

[0051] (1) Polymerization reaction

[0052] Under the protection of nitrogen at room temperature (28 ° C), the above reaction monomer 4,4'-dihydroxydiphenyl sulfide and 4,4'-dichlorodiphenyl sulfide, auxiliary agent anhydrous Na 2 CO 3 and anhydrous K 2 CO 3 , composite catalyst sodium benzoate and zinc powder, solvent sulfolane, and azeotropic dehydrating agent toluene are added to the reaction kettle equipped with agitator, thermometer, and water separator, and the temperature is raised to 140 ° C ~ 150 ° C under stirring. Azeotropic ...

Embodiment 2

[0056] 1. Raw material and its formula

[0057] Reactive monomer 4,4'-dihydroxydiphenyl sulfide (DHPS) 109g (0.5mol)

[0058] Reactive monomer 4,4'-dichlorodiphenylsulfide (DCPS) 127.5g (0.5mol)

[0059] Anhydrous Li 2 CO 3 60g (0.81mol)

[0060] Trisodium phosphate 8.2g (0.05mol)

[0061] Hydrazine hydrate 10mL (0.2mol)

[0062] Cuprous oxide 7.2g (0.05mol)

[0063] N,N'-Dimethylacetamide 250mL

[0064] Chlorobenzene 100mL

[0065] 2. Process steps

[0066] (1) Polymerization reaction

[0067] Under the protection of nitrogen at room temperature (25 ° C), the above reaction monomer 4,4'-dihydroxydiphenyl sulfide and 4,4'-dichlorodiphenyl sulfide, auxiliary agent anhydrous Li 2 CO 3 , the composite catalyst trisodium phosphate, hydrazine hydrate and cuprous oxide, the solvent N, N'-dimethylacetamide, and the azeotropic dehydrating agent chlorobenzene are added to the reaction kettle equipped with a stirrer, a thermometer and a water separator. Under stirring, heat ...

Embodiment 3

[0071] 1. Raw material and its formula

[0072] Reactive monomer 4,4'-dihydroxydiphenyl sulfide (DHPS) 109g (0.5mol)

[0073] Reactive monomer 4,4'-dichlorodiphenylsulfide (DCPS) 127.5g (0.5mol)

[0074] KOH 72.8g (1.3mol)

[0075] Sodium acetate 10g (0.12mol)

[0076] Hydrosulfite 5.2g (0.03mol)

[0077] N,N'-Dimethylformamide 350mL

[0078] Xylene 200mL

[0079] 2. Process steps

[0080] (1) Polymerization reaction

[0081] Under nitrogen protection at room temperature (21 ° C), the above reaction monomer 4,4'-dihydroxydiphenyl sulfide and 4,4'-dichlorodiphenyl sulfide, auxiliary agent KOH, composite catalyst sodium acetate and sodium hydrochloride , the solvent N, N'-dimethylformamide, and the azeotropic dehydrating agent xylene are added to a reaction kettle equipped with a stirrer, a thermometer, and a water separator, and the temperature is raised to 140°C to 150°C under stirring to azeotropically reflux, Azeotropic reflux for 4 hours (moisture and azeotropic deh...

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Abstract

This invention discloses a method for preparing poly (phenylene sulfide). The raw materials include: monomers 4, 4'-dihydroxyl diphenyl sulfide (DHPS) and 4, 4'-dihalogen diphenyl sulfide at a mol. ratio of 1:1; additive 1.1-2.6 mol. /mol. DHPS; composite catalyst 0.22-1.08 mol./mol. DHPS; solvent 400-700 mL/mol. DHPS; azeotropic dehydrating agent 200-400 mL/mol. DHPS. The method comprises: (1) adding the above raw material into a reactor under nitrogen protection, stirring, heating to 140-150 deg.C until azeotropic refluxing, sealing the reactor when water and the azeotropic dehydrating agent are completely distilled out, heating to 180-350 deg.C, and polymerizing for 4-10 h; (2) precipitating the solution, filtering, washing, purifying and vacuum-drying to obtain poly(phenylene sulfide).

Description

technical field [0001] The invention belongs to the field of polyphenylene ether sulfide, in particular to a preparation method of polyphenylene ether sulfide. Background technique [0002] Polyphenylene ether sulfide [Poly(oxy-1,4-phenylenethio-1,4-phenylene), PPSE for short] is a high temperature resistant polymer material with a wide range of uses. Regarding the preparation method of polyphenylene ether sulfide, there are nucleophilic substitution method and electrophilic substitution method. The synthesis operation of electrophilic substitution method is relatively cumbersome, the reaction is often accompanied by many side reactions, and the yield is low. The synthesized polymer PPSE often contains Diphenyl disulfide bond, low melting point, low molecular weight (only PPSE synthesized by Japanese scholar Eishun Tsuchida in 1993 with a multi-step method has a high molecular weight). Belong to the prior art scheme of nucleophilic substitution method as follows: [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08G65/40C08G75/0227
Inventor 顾爱群余自力李玉宝
Owner SICHUAN UNIV
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