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S-containing polymer and preparation method thereof

A technology of polymer and polymer solution, applied in the field of preparation of sulfur-containing polymers, can solve the problems of long reaction period, general efficiency, complicated process, etc., achieve excellent melt processing stability, improve solvent recovery rate, reduce halogen The effect of content

Active Publication Date: 2022-02-08
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In industrial production, the current main method of polyarylene sulfide production is: using sodium sulfide and dihalogenated aromatic compounds to carry out solution polycondensation under high temperature and pressure, such as Philips company using sodium sulfide and p-dichlorobenzene in nitrogen in a polar solvent Pressurized reaction preparation in NMP (US 33544129), this method energy consumption is big, and reaction cycle is long; , using a tank reactor, the efficiency is general, its solvent and catalyst recovery rate are low, and its product has not been subjected to post-end capping treatment, and the product processing stability is not good; Chinese patent CN1143652A reports that sulfur is used as a raw material in a polar solvent to pressurize The synthesis of tough polyphenylene sulfide resin requires the use of a reducing agent in the reaction process, the process is relatively complicated, there are many reaction by-products, the product is not easy to purify, and the solvent is also recovered by dehydration and rectification, which consumes a lot of energy. Uneconomical

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  • S-containing polymer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0055] (1) Wafer 50GCECL 2 , 50 g sodium carbonate, 400 g of solvent isoquinoline and 178 g of sodium sulfur sulfide are added to the pre-reaction kettle, under nitrogen protection, dehydrated at a temperature of 220 ° C, resulting in dehydrated pre-reactive solution, constant temperature; 147 g of dichloro Benzene and 100 g of solvent isoquinoline is added to the premixer, and after the dicase is dissolved, the pre-pressure metering pump is separately supplied to the monomeric solution in the pre-transmixer and the premixer reactor. (Number of modules: 50 groups), the feed molar ratio of the monomer solution in the pre-reactive solution and the premixer is 1: 1.01 (S monomer: dihalogenated monomer), the feed speed is 40g / min At the temperature of 260 ° C, the contract 1400s is polyeded to obtain a sulfur-containing compound solution having a certain molecular weight and molecular weight distribution;

[0056] (2) The obtained sulfur-containing compound solution is then sent to ...

Embodiment 2

[0061] (1) 30 g of lithium chloride, 5 g sodium hydroxide, 350 g of solvent N-methylpyrrolidone and 117 g of sodium hydrogenated sodium hydrogenide were added to the pre-reaction kettle, under nitrogen protection, dehydrated at a temperature of 200 ° C for 1 h, after dehydration The pre-reactive solution, constant temperature; 287 g of 4'-dichlorophenyl sulfone and 100 g solvent N-methylpyrrolidone is added to the premixer, and after the dielectric monomer is dissolved, the high-pressure metering pump will be pre-rely. The monomer solution in the solution and the premixer is sent into a tandem type microchannel reactor (number of modules: 40 groups), the feed molar ratio of the monomer solution in the pre-reactive solution and the premixer is 1: 1.02 ( S monomer: dihalogenated monomer), the feed speed is 50 g / min, the polyline 1100s, the temperature is 190 ° C, that is, a sulfur compound solution having a certain molecular weight and molecular weight distribution;

[0062] (2) T...

Embodiment 3

[0066](1) 50 g of sodium acetate, 45 g of potassium carbonate, 350 g of sodium, and 117 g of sodium hydrogen sulfonate, and sodium hydrogen sulfide, under nitrogen protection, dehydration reaction at a temperature of 195 ° C for 1 h, to obtain dehydration Solution, constant temperature; 218 g of 4, 4'-difluorobenzophenone and 100 g of solvent N-methylpyrrolidone are added to the premixer, and after the dielectric monomer is dissolved, the pre-reactive solution is used. And the monomer solution in the premixer is sent into a tandem type microchannel reactor (number of modules: 80 groups), the feed molar ratio of the monomer solution in the pre-reactive solution and the premixer is 1: 0.99 (s The monomer: dihalogenated monomer), the feed rate is 350 g / min, the polyline 1800s, the temperature is 240 ° C, i.e., a sulfur compound solution having a certain molecular weight and molecular weight distribution;

[0067] (2) The obtained sulfur compound solution is then sent to another in ...

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Abstract

The invention relates to a preparation method of a sulfur-containing polymer, and belongs to the field of polymer synthesis. According to the preparation method of the S-containing polymer, the preparation method comprises the following steps: 1) carrying out blending reaction on raw materials such as a sulfur-containing monomer and a dihalogenated monomer by adopting a tandem micro-channel reactor to obtain a sulfur-containing polymer solution; 2) feeding the sulfur-containing polymer solution obtained in the step 1) into another group of parallel micro-channel reactors, and reacting with an end group control agent solution at 240-280 DEG C to prepare a sulfur-containing polymer mixed solution; and (3) purifying to obtain a product, namely the S-containing polymer. The micro-channel reactor is introduced into the preparation process of the S-containing polymer for the first time, and the polymer with narrow molecular weight distribution can be prepared; besides, by controlling the feeding amount and feeding speed of the sulfur-containing monomer and the dihalogenated monomer and the number of reaction modules of the microchannel reactor, the reaction ratio and the molecular weight and molecular weight distribution of the sulfur-containing polymer can be controlled.

Description

Technical field [0001] The present invention relates to a method of preparing a sulfur-containing polymer, belonging to the field of polymer synthesis. Background technique [0002] Sulfur-containing compound polyaryl sulfide such as polyphenylene sulfide, polyphenylene sulfide, polyphenylene sulfide due to its high temperature, corrosion resistance, excellent electrical energy, mechanical properties, and dimensional stability, and is widely used in automobiles , Aerospace and electronic technology. In industrial production, the main method of current polyaryl sulfide production is: a solution polycondensation of sodium sulfide and dihalogenated aromatic compounds, such as philips, sodium sulfide and dichlorobenzene in nitrogen in a polar solvent Preparation (US 33544129) in NMP (US 33544129), this method can be large, the reaction cycle is long; CN1793202A Deyang Technology Co., Ltd. uses a pressurized synthetic polyphenylene sulfide resin with sodium sulfide and dichlorobenzene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0254C08G75/0281
CPCC08G75/0254C08G75/0281Y02E60/10
Inventor 不公告发明人
Owner SICHUAN UNIV
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