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Synthetic method of polyarylene sulfide resin

A technology of polyarylene sulfide and synthesis method, applied in the field of polymer materials, can solve problems such as large solvent loss, and achieve the effects of reducing solvent loss, low production cost and high economy

Active Publication Date: 2021-03-30
ZHEJIANG UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In order to solve the problem of large solvent loss in the existing industrial synthesis of polyarylene sulfide, the present invention provides a synthesis method of polyarylene sulfide, which fundamentally reduces the loss of solvent NMP, and at the same time the alkali metal produced in the reaction process Carboxylate can also play a role in promoting polymerization

Method used

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  • Synthetic method of polyarylene sulfide resin
  • Synthetic method of polyarylene sulfide resin

Examples

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Embodiment 1

[0041] Dehydration: In a 1000L reactor, add 1000mol of sodium hydrosulfide, NaOH / sodium hydrosulfide (mol / mol)=1.01, NMP / sodium hydrosulfide (mol / mol)=2.5, at a stirring speed of 200rpm and under nitrogen protection, At a speed of 1.5°C / min, the temperature was raised to 200°C for dehydration, 124.4Kg of aqueous solution (water content 94.2%) was removed, and then the temperature was lowered to 110°C.

[0042] Polymerization: continue to add p-dichlorobenzene (PDCB) and solvent NMP to the reactor, and in the final reaction system, PDCB / sodium hydrosulfide (mol / mol)=1.02, and NMP / sodium hydrosulfide (mol / mol)=3.5. Raise the temperature to 220°C at a rate of 2°C / min, and add acetic acid after keeping the temperature for 1 hour. The amount added is 0.005mol / 1mol sodium hydrosulfide. Then the temperature was raised to 270°C at a rate of 1°C / min, and kept for 2 hours; then cooled to 240°C at 1°C / min, kept for 0.5h, and finally cooled to 150°C at 2°C / min to obtain polyarylene sulfide ...

Embodiment 2～6

[0046] On the basis of Example 1, the type, timing and amount of organic monobasic acid were changed, as shown in Table 1 below. The properties of the polyphenylene sulfide prepared in each example are also listed in Table 1 below.

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Abstract

The invention discloses a synthetic method of polyarylene sulfide resin, which comprises: 1, adding a sulfur source, an alkaline substance and Nmethylpyrrolidone to a reaction kettle, heating to a temperature of 180-210 DEG C, and carrying out a dehydration reaction to obtain an intermediate product; 2, continuously adding a dihalogenated aromatic compound and N-methylpyrrolidone into the reactionkettle, adding organic monobasic acid, carrying out condensation polymerization at 210-280 DEG C to obtain polyarylene sulfide slurry, and carrying out post-treatment to obtain polyarylene sulfide resin, wherein the structural general formula of the organic monobasic acid is R-COOH, and in the formula, R is selected from hydrogen or alkyl with the carbon number of 1-4. According to the synthesismethod provided by the invention, the loss of the solvent NMP is fundamentally reduced, and meanwhile, the alkali metal carboxylate generated in the reaction process can also play a role in promotingpolymerization. The method is simple in process, low in production cost and high in economy.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a synthesis method of polyarylene sulfide resin. Background technique [0002] Polyarylene sulfide refers to a class of polymers in which the main chain structure of the polymer molecule is alternately connected with sulfur and aryl structures. Due to the particularity of the composition of such polymers and the rigidity of their molecular structures, they generally have excellent high temperature resistance, corrosion resistance, radiation resistance, flame retardancy, balanced mechanical properties, excellent dimensional stability, and excellent electrical properties, etc. Advantages, are widely used as structural polymer materials. Such as: polyarylene sulfide resin can be used as high-performance composite material matrix resin, can be made into special fibers, etc.; can be widely used as special engineering plastics after filling and modification; at the same time...

Claims

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Application Information

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IPC IPC(8): C08G75/0259C08G75/0209
CPCC08G75/0259C08G75/0209
Inventor 周贵阳陈志荣尹红杨郑邓杭军缪建峰李沃源
Owner ZHEJIANG UNIV
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