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Method for synthesizing fiber-grade polyphenylene sulfide through adding composite accelerant in intermediate stage

A composite accelerator and polyphenylene sulfide technology, applied in the field of polymer materials, can solve the problems of affecting product quality, prolonging production steps, low molecular weight, etc., and achieve the effects of simplifying the production process, improving production efficiency, and high reaction rate

Active Publication Date: 2014-02-26
ZHUHAI CHANGXIAN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The raw materials of the above methods are easy to obtain, but it is difficult to obtain high-molecular-weight PPS resins that meet the requirements of use by ordinary processes
Even if synthesized under high temperature and high pressure conditions, there is still the defect that it is difficult to synthesize high molecular weight PPS, and due to the low molecular weight and high dispersion, it needs to be purified, thermal oxygen cross-linking and other subsequent treatment processes to meet the use requirements.
In this way, it not only prolongs the production steps and increases the cost, but also makes the color of the product darker, affecting the appearance of the product
[0007] To sum up, the existing PPS production technology usually has complex synthesis process and high requirements on process conditions, the growth of PPS molecular chain is not easy in the later stage of polymerization reaction, it is difficult to synthesize PPS with high molecular weight (weight average molecular weight above 40,000), and the product color Deep, unstable quality and other issues

Method used

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  • Method for synthesizing fiber-grade polyphenylene sulfide through adding composite accelerant in intermediate stage
  • Method for synthesizing fiber-grade polyphenylene sulfide through adding composite accelerant in intermediate stage

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Low temperature section: In a 10-liter reactor, add Na 2 S·3H 2 O1000g, catalyst 380g and N-methylpyrrolidone 4200g for dehydration reaction; after dehydration, add p-dichlorobenzene 1200g, fill with nitrogen, airtight, prepolymerize at 220°C for 3h at low temperature.

[0028] Middle temperature section: raise the temperature to 231°C, add 200g of composite accelerator using the differential pressure method, control the pressure in the reactor within the range of 0.40-0.9mpa, and react for 1.5h.

[0029] High-temperature section: Finally, the temperature is raised to 265°C for 3 hours, and the pressure in the reactor remains unchanged in the range of 0.40-0.9mpa.

[0030] The catalyst mentioned above is lithium chloride.

[0031] The above composite accelerator is formed by mixing p-dichlorobenzene, trichlorobenzene and N-methylpyrrolidone in a weight ratio of 0.8:0.5:100.

[0032] The finally obtained polyphenylene sulfide particles are uniform, with a particle siz...

Embodiment 2

[0034] Low temperature section: In a 10-liter reactor, add Na 2 S·3H 2 O1000g, catalyst 400g and N-methylpyrrolidone 3200g for dehydration reaction; after dehydration, add p-dichlorobenzene 1250g, fill with nitrogen, airtight, pre-polymerize at 200°C for 2h at low temperature.

[0035] Middle temperature section: raise the temperature to 240°C, add 250g of composite accelerator using the pressure difference method, control the pressure in the reactor within the range of 0.50-0.9mpa, and react for 1h.

[0036] High-temperature section: Finally, the temperature is raised to 255°C for 3 hours, and the pressure in the reactor remains unchanged within the range of 0.50-0.9mpa.

[0037] The catalyst mentioned above is lithium chloride.

[0038] The above-mentioned composite accelerator is formed by mixing lithium chloride, p-dichlorobenzene, m-dichlorobenzene and N-methylpyrrolidone in a weight ratio of 15:12:5:300.

[0039] The finally obtained polyphenylene sulfide particles ar...

Embodiment 3

[0041] Low temperature section: In a 10-liter reactor, add Na 2 S·3H 2 O1000g, catalyst 400g and N-methylpyrrolidone 3200g for dehydration reaction; after dehydration, add p-dichlorobenzene 1250g, fill with nitrogen, airtight, pre-polymerize at 200°C for 2h at low temperature.

[0042] Middle temperature section: raise the temperature to 240°C, add 250g of composite accelerator using the pressure difference method, control the pressure in the reactor within the range of 0.50-0.9mpa, and react for 1h.

[0043] High-temperature section: Finally, the temperature is raised to 255°C for 3 hours, and the pressure in the reactor remains unchanged within the range of 0.50-0.9mpa.

[0044] The catalyst mentioned above is lithium chloride.

[0045] The above-mentioned composite accelerator is formed by mixing lithium chloride, p-dichlorobenzene, m-dichlorobenzene and trichlorobenzene, and N-methylpyrrolidone in a weight ratio of 7:6:3:200.

[0046] The finally obtained polyphenylene ...

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Abstract

The invention discloses a method for synthesizing fiber-grade polyphenylene sulfide through adding a composite accelerant in an intermediate stage. The method comprises the step: with p-dichlorobenzene and waterish sodium sulfide as reaction raw materials, synthesizing polyphenylene sulfide through polycondensation, wherein the composite accelerant is added in the intermediate stage of the reaction and is formed by mixing the four components: lithium chloride, p-dichlorobenzene, trichlorobenzene and / or m-dichlorobenzene and N-methylpyrrolidone. Compared with the prior art, the method disclosed by the invention is simple in process and low in production cost, and the synthesized polyphenylene sulfide is high in molecular weight, good in appearance and favorable in quality.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a method for adding a composite accelerator to synthesize fiber-grade polyphenylene sulfide in the middle section. Background technique [0002] Polyphenylene sulfide is a new polymer material, its English abbreviation is PPS. PPS has excellent heat resistance, flame retardancy, corrosion resistance and balanced mechanical and electrical properties, so it is widely used in electronics, automobiles, machinery and chemical fields. [0003] At present, the relatively mature synthesis methods of polyphenylene sulfide commonly used at home and abroad generally use p-dichlorobenzene and hydrous sodium sulfide as reaction raw materials, and synthesize polyphenylene sulfide through steps such as dehydration and polycondensation. The reaction equation is as follows: [0004] [0005] [0006] The raw materials of the above-mentioned method are easy to obtain, but it is di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08G75/0254
Inventor 杨伟明周鸿文张德明叶维雪
Owner ZHUHAI CHANGXIAN CHEM TECH
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