Method for preparing polyphenylene sulfide from benzene and sulfur

A technology of polyphenylene sulfide and polyphenylene sulfide resin, which is applied in the production process of polyphenylene sulfide, can solve the problems of high crystallinity of polyphenylene sulfide, difficulty in processing, limitation of application field and use range, etc., and achieve washing The effect of less frequency, improved production efficiency, and expanded application field and use range

Active Publication Date: 2018-12-07
四川中科兴业高新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problem that the above-mentioned existing polyphenylene sulfide is not easy to be processed into films or fibers due to its high crystallinity, resulting in the limitation of its application field and scope of use. Method for preparing polyphenylene sulfide

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  • Method for preparing polyphenylene sulfide from benzene and sulfur
  • Method for preparing polyphenylene sulfide from benzene and sulfur

Examples

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Embodiment 1

[0032] A method for preparing polyphenylene sulfide with benzene and sulfur as raw materials, comprising the following steps:

[0033] (1) Add 1 mol of 1,2,4-trichlorobenzene and 0.04 mol of nano-copper oxide into the reactor in sequence, start stirring, then add 1 mol of sulfur, and continue stirring until a uniform suspension is formed in the reactor;

[0034] (2) Add 0.51mol benzene to the suspension formed in step (1), adjust the temperature in the reactor to 80°C at a heating rate of 5-6°C / min, and react at a constant temperature for 1.5h;

[0035] (3) Adjust the temperature in the reactor to 130°C at a heating rate of 5-6°C / min, and react at a constant temperature for 4 hours;

[0036] (4) Adjust the temperature in the reactor to be lower than 40°C, send the materials in the reactor to a centrifuge for solid-liquid separation to obtain crude polyphenylene sulfide resin, and send the separated liquid to the mother liquor temporary storage tank for recycling use;

[0037...

Embodiment 2

[0039] A method for preparing polyphenylene sulfide with benzene and sulfur as raw materials, comprising the following steps:

[0040] (1) Add 1 mol of 1,2,4-trichlorobenzene and 0.03 mol of nano-aluminum chloride to the reactor in sequence, start stirring, then add 1 mol of sulfur, and continue stirring until a uniform suspension is formed in the reactor;

[0041] (2) Add 0.51mol benzene to the suspension formed in step (1), adjust the temperature in the reactor to 90°C at a heating rate of 5-6°C / min, and react at a constant temperature for 1.5h;

[0042] (3) Adjust the temperature in the reactor to 150°C at a heating rate of 5-6°C / min, and react at a constant temperature for 4 hours;

[0043] (4) Adjust the temperature in the reactor to be lower than 40°C, send the materials in the reactor to a centrifuge for solid-liquid separation to obtain crude polyphenylene sulfide resin, and send the separated liquid to the mother liquor temporary storage tank for recycling use;

[0...

Embodiment 3

[0046]A method for preparing polyphenylene sulfide with benzene and sulfur as raw materials, comprising the following steps:

[0047] (1) Add 1mol 1,2,4-trichlorobenzene and 0.05mol nano-copper iodide to the reaction kettle in turn, start stirring, then add 1mol sulfur, and continue stirring until a uniform suspension is formed in the reaction kettle;

[0048] (2) Add 0.52mol of benzene to the suspension formed in step (1), adjust the temperature in the reactor to 95°C at a heating rate of 5-6°C / min, and react at a constant temperature for 1.5h;

[0049] (3) Adjust the temperature in the reactor to 160°C at a heating rate of 5-6°C / min, and react at a constant temperature for 4 hours;

[0050] (4) Adjust the temperature in the reactor to be lower than 40°C, send the materials in the reactor to a centrifuge for solid-liquid separation to obtain crude polyphenylene sulfide resin, and send the separated liquid to the mother liquor temporary storage tank for recycling use;

[005...

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Abstract

The invention discloses a method for preparing polyphenylene sulfide from benzene and sulfur. The method comprises the following steps: (1) sequentially adding a solvent and an inorganic salt catalystinto a reaction kettle, starting to stir, adding sulfur, continuously stirring until uniform suspension liquid is formed in the reaction kettle; (2) adding benzene into the suspension liquid, adjusting the temperature in the reaction kettle to 60-100 DEG C, and reacting at a constant temperature for 0.5-1.5 hours; (3) adjusting the temperature in the reaction kettle to 120-170 DEG C, and reactingat a constant temperature for 2-6 hours; (4) adjusting the temperature in the reaction kettle to be lower than 40 DEG C, and carrying out solid-liquid separation, so as to obtain a polyphenylene sulfide resin crude product; and (5) washing and drying the polyphenylene sulfide resin crude product, so as to obtain the polyphenylene sulfide resin. According to the method, amorphous polyphenylene sulfide resin is synthesized through the reaction of benzene and sulfur, so that the problem that existing polyphenylene sulfide is difficult to be processed into a film or a fiber due to the high crystallization degree is solved; and production purify is high, the solvent is easy to recycle, the production cost is low, and the ''three wastes'' are remarkably reduced.

Description

technical field [0001] The invention belongs to the technical field of polyphenylene sulfide production technology, and in particular relates to a method for preparing polyphenylene sulfide by using benzene and sulfur as raw materials. Background technique [0002] The full name of polyphenylene sulfide is polyphenylene sulfide, which is a thermoplastic resin with phenylthio groups in the main chain of the molecule. The unstretched fiber has a large amorphous region (the crystallinity is about 5%). The fiber crystallizes during stretching, and the crystallinity can reach 60-80%. The synthesis methods of polyphenylene sulfide mainly include sodium sulfide method, sulfur solution method, hydrogen sulfide method, oxidation polymerization method, p-halogenated thiophenol polycondensation method, etc. The polyphenylene sulfide synthesized by these methods has excellent thermal properties and electrical properties. Performance, short-term resistance to 260°C, and long-term use at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0263
CPCC08G75/0209C08G75/025C08G75/0263
Inventor 刘洪范志永李玉凤尹振泉陈云余雷胡小冬
Owner 四川中科兴业高新材料有限公司
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