Preparation method of sodium sulfide reaction precursor in polyphenylene sulfide production

A technology of polyphenylene sulfide and sodium sulfide, applied in chemical instruments and methods, sulfur compounds, inorganic chemistry, etc., can solve the problems of unfavorable polyphenylene sulfide product quality, unfavorable polycondensation reaction, and time-consuming, etc., and achieve remarkable results Economic and environmental protection value, conducive to popularization, and the effect of reducing energy consumption of the process

Active Publication Date: 2020-01-17
YIBIN TIANYUAN GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method mainly utilizes adding NMP to the sodium sulfide system, and adopts the method of heating to remove crystallization water by forming an azeotrope between NMP and water. However, this method consumes a lot of energy and takes a lot of time. The time is very long, usually at least 4 to 6 hours. Practice has proved that if the dehydration time is shortened, it is not conducive to the polycondensation reaction, and the quality of the polyphenylene sulfide product cannot be guaranteed.

Method used

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  • Preparation method of sodium sulfide reaction precursor in polyphenylene sulfide production
  • Preparation method of sodium sulfide reaction precursor in polyphenylene sulfide production
  • Preparation method of sodium sulfide reaction precursor in polyphenylene sulfide production

Examples

Experimental program
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Effect test

Embodiment 1

[0030] In a 25L pre-reaction kettle, add sodium sulfide trihydrate, NMP (N-methylpyrrolidone), sodium hydroxide and sodium acetate into the pre-reaction kettle at a molar ratio of 1:5:0.02:0.02, and then add A certain amount of deionized water, control the addition of deionized water to ensure that the mol ratio of sodium sulfide to water (including crystal water and free water) in the system is 1:10, open the pre-reactor to stir before heating up, and open the nitrogen to the pre-reaction tank simultaneously. The gas phase space of the reaction kettle is replaced, the replacement time is 10 minutes, and then the temperature of the system is raised to 150°C by electric heating, and the temperature is maintained until the complete reaction forms a stable ternary complex. It takes 30 minutes to obtain the aqueous sodium sulfide reaction Precursors (i.e. intermediates).

[0031] Continue to use heat conduction oil to raise the temperature of the pre-reactor to 190°C, and use a vacu...

Embodiment 2

[0037] In a 25L pre-reaction kettle, add sodium sulfide nonahydrate and formamide into the pre-reaction kettle at a molar ratio of 1:10, then add a certain amount of deionized water, and control the amount of deionized water added to ensure that the system The molar ratio of sodium sulfide to water (including crystal water and free water) is 1:20. Before the temperature rises, the pre-reactor is turned on for stirring, and at the same time, nitrogen is turned on to replace the gas phase space of the pre-reactor. The replacement time is 10 minutes, and then electric heating is used. The method is to raise the temperature of the system to 180°C, and maintain this temperature until the complete reaction forms a stable ternary complex. It takes 40 minutes to obtain a water-containing sodium sulfide reaction precursor (ie, an intermediate).

[0038] Continue to use heat transfer oil to raise the temperature of the pre-reactor to 208°C, and use a vacuum pump to control the vacuum of ...

Embodiment 3

[0041] In a 25L pre-reaction kettle, add sodium sulfide pentahydrate, 2-pyrrolidone, and sodium hydroxide into the pre-reaction kettle in a molar ratio of 1:8:0.02, and then add a certain amount of ion-free water to control the ion-free The amount of water added ensures that the molar ratio of sodium sulfide to water (including crystal water and free water) in the system is 1:15. Before the temperature rises, the pre-reactor is opened to stir, and nitrogen is opened to replace the gas phase space of the pre-reactor. After 10 minutes, the temperature of the system was raised to 160°C by means of electric heating, and the temperature was maintained until the complete reaction formed a stable ternary complex. It took 30 minutes to obtain the aqueous sodium sulfide reaction precursor (ie intermediate).

[0042] Continue to use heat transfer oil to raise the temperature of the pre-reactor to 200°C, and use a vacuum pump to control the vacuum of the system to 0.095MPa, and then remov...

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Abstract

The invention relates to a production method of polyphenylene sulfide and specifically discloses a preparation method of a sodium sulfide reaction precursor in polyphenylene sulfide production. The preparation method comprises the following steps: (A) dissolution, proportionally adding raw materials into a pre-reaction kettle, wherein the raw materials include a sodium sulfide polyhydrate and an entrainer, and the entrainer is an amide compound; adding water into the system to ensure that the molar ratio of Na2S to H2O is 1 to (10 to 20); eliminating oxygen in the pre-reaction kettle; then, heating the mixture to 150-180 DEG C, and maintaining the temperature for at least 30min to obtain an intermediate; (B) dehydration: distilling to remove redundant water in the intermediate to obtain the sodium sulfide reaction precursor. The preparation method disclosed by the invention has the following advantages: 1) the preparation time of the sodium sulfide reaction precursor can be shortened from 4-6h to 2-3h, and the process energy consumption is correspondingly lowered by 50% or more, thereby creating remarkable economic and environmental value; 2) the scheme is easy to implement and promotes industrial popularization.

Description

technical field [0001] The invention relates to a synthesis process of polymer material resin, in particular to a synthesis process of polyphenylene sulfide. Background technique [0002] There are three main synthetic routes for polyphenylene sulfide, sodium sulfide method, sulfur solution method, and oxidative polymerization method. The most widely used technology for industrial synthesis is the sodium sulfide method. [0003] At present, the process of synthesizing polyphenylene sulfide by sodium sulfide method is all prepared by dehydration and polycondensation of p-dichlorobenzene and sodium sulfide as raw materials. The main steps are as follows: [0004] (1) dehydrating sodium sulfide to obtain sodium sulfide reaction precursor; [0005] (2) In the polymerization kettle, the reaction precursor of sodium sulfide reacts with p-dichlorobenzene (p-DCB) to obtain the polyphenylene sulfide product. [0006] Among them, due to the strong water absorption of sodium sulfide...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/0254C01B17/38
CPCC01B17/38C08G75/0254
Inventor 谢濠江罗云颜华孙永贵李军严国银
Owner YIBIN TIANYUAN GRP CO LTD
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