Improved synthesis method of polyphenylene sulfide

A polyphenylene sulfide and synthesis method technology, applied in the field of engineering plastics, can solve problems such as difficulties in actual production and application, slow polymerization reaction speed, high content of low polymer chains, etc., to achieve favorable mechanical properties, improve performance, and increase weight-average molecular weight Effect

Inactive Publication Date: 2015-07-01
CHANGZHOU UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0008] In summary, the current methods reported in the literature can produce polyphenylene sulfide, but there are many problems such as slow polymerization reaction speed, low degree of polymerization (most chain molecular weights are less than 80,000), difficulty in industrialization, and high content of low polymer chains. Defects bring great difficulties to actual production and application

Method used

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  • Improved synthesis method of polyphenylene sulfide
  • Improved synthesis method of polyphenylene sulfide
  • Improved synthesis method of polyphenylene sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016]

[0017] At room temperature, add 14.6g (0.1mol) of p-dichlorobenzene, sodium sulfide hydrate (0.1mol), CuCl (99mg, 1mmol), and NMP (120ml) into the autoclave, and heat it to about 150°C to 160°C. The reaction is initiated, and the internal temperature can reach up to 220°C (reaction exotherm), keep at 180°C for 2 hours, heat up to 260-280°C for 2 hours, cool to room temperature, filter, wash the filter cake with NMP (20ml×2), water Washing until the conductivity remains unchanged, drying, the weight yield is 94.2%, the product has a molecular weight of 80,000-100,000 accounting for 78.5% (weight ratio, the same below), and the weight average molecular weight is 89,300.

[0018] Using the same method, using CuBr, CuI, and CuOAc as raw materials, the yield and molecular weight distribution obtained are shown in Table 1.

[0019] Table 1 Effect of different copper salts on the reaction results

[0020]

[0021] The experimental results show that: a variety of coppe...

Embodiment 2

[0023] Adopt the mode of embodiment 1, change the sodium sulfide (number of moles constant) with different water content, the results are shown in Table 2.

[0024] Table 2 Effect of water content in sodium sulfide on reaction results

[0025]

[0026] The research results show that: sodium sulfide with different water content can get more ideal results.

Embodiment 3

[0028] At room temperature, add CuCl (99 mg, 1 mol), cis-cyclohexanediamine (125.4 mg, 1.1 mmol), and NMP (5 mL) into a round bottom flask and heat to 80 ° C. After 30 min of incubation, the solution is transferred to the reaction kettle 14.6g (0.1mol) of p-dichlorobenzene, 7.8g (0.1mol) of sodium sulfide, and NMP (115ml) were added to the kettle, and the reaction was initiated by heating to about 150°C to 160°C. 220°C (exothermic reaction), keep warm at 180°C for 2 hours, heat up to 260-280°C and keep warm for 2 hours, cool to room temperature, filter, wash the filter cake with NMP (20ml×2), wash with water until the conductivity remains unchanged, and dry Drying, the yield is 94.3%, the part with molecular weight of 80,000-100,000 in the product accounts for 84.1%, and the weight average molecular weight is 93,700.

[0029] Using the same method, tetramethylethylenediamine, N,N'-dimethylethylenediamine, trans-cyclohexanediamine, triphenylphosphine, 2,2'-bis(diphenylphosphine...

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Abstract

The invention discloses an improved synthesis method of polyphenylene sulfide, and belongs to the field of engineering plastics. The improved synthesis method comprises the following step: with p-dichlorobenzene and sodium sulfide as raw materials, preparing polyphenylene sulfide with high molecular weight and narrow molecular weight distribution under the catalysis of univalent copper ions or complexes of the univalent copper ions. The polymerization product disclosed by the invention is high in yield and few in low polymers, and has good industrialized application prospect.

Description

technical field [0001] The invention relates to an improved synthesis method of polyphenylene sulfide, which belongs to the field of engineering plastics. Background technique [0002] Polyphenylene sulfide (PPS) is a special engineering plastic with excellent performance. It has the advantages of high mechanical strength, high temperature resistance, corrosion resistance, and good insulation performance. It has a wide range of applications in the fields of automobiles, military industry, and medicine. Its structural formula is as follows: [0003] [0004] The synthesis methods reported in the literature mainly include the following: such as self-condensation of halothiophenate, melt polymerization of p-halodiphenyl and sulfur, electrophilic reaction of sulfur and benzene, solution polycondensation of alkali metal sulfide and p-dihalobenzene (sodium sulfide method), solution polycondensation of sulfur and p-dichlorobenzene (sulfur solution method), polymerization of dip...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08G75/0213C08G75/0254
Inventor 樊白白张进胡睿王瑶瑶王利群刘建武马晓明沈介发丁瑞仪吴雨豪张跃严生虎辜顺林
Owner CHANGZHOU UNIV
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