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Dehydration process for polyphenyl thioether resin synthesis solvent system

A polyphenylene sulfide resin and solvent technology, which is applied in the field of resin synthesis of polymer materials, can solve the problems of large initial investment, large recovery loss, and long recovery cycle, and achieve the goals of increasing reaction speed, saving costs, and improving production efficiency Effect

Active Publication Date: 2013-03-13
SICHUAN DEYANG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can reduce the initial input amount of solvent by 20-30%, reduce the amount of dehydration liquid by about 70%, wherein the content of solvent is also reduced from more than 65% to 5-15%; the energy consumption is reduced by about 25%, effectively reducing the initial NMP The input amount, recovery workload and energy consumption greatly reduce the loss in solvent recovery, thereby effectively reducing the production cost of the final product by about 5%, overcoming the large initial input amount of solvent in the background technology, long recovery period and large recovery loss, etc. Disadvantages, although a 25% reduction in energy consumption is introduced therein, but the cost is still very high compared to the prior art of the present invention

Method used

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  • Dehydration process for polyphenyl thioether resin synthesis solvent system
  • Dehydration process for polyphenyl thioether resin synthesis solvent system
  • Dehydration process for polyphenyl thioether resin synthesis solvent system

Examples

Experimental program
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Effect test

Embodiment 1～4

[0028] In the sodium sulfide dehydration treatment stage, in order to make the raw material Na in the solvent system 2 S:NMP:NaOH:H 2 The mol ratio between O is 1.0: 3.9: 0.02, is that the Na in the formula is ≥ 66.0%wt purity 2 S. 3 h 2 O solid excess 1% is added in common reactor, under the pressure is -0.9Mpa, is heated to 80 ℃, makes Na 2 After the S is fully dissolved, adjust the vacuum degree to 0.75Mpa and then raise the temperature to 150°C, keep the temperature, the pressure is -0.75Mpa, and the stirring speed is 300rpm; dehydration treatment until the water content in the sodium sulfide solution is 1.0mol / molNa 2 After S, after using a quick moisture analyzer to detect the moisture content therein, Na 2S: p-dichlorobenzene (p-DCB) molar ratio of 1:1.5 is added to p-dichlorobenzene for temperature rise polymerization to complete the polymerization reaction of polyphenylene sulfide; the amount of nitrogen and energy consumption in this dehydration process are onl...

example 5～8

[0030] In the sodium sulfide dehydration treatment stage, in order to make the raw material Na in the solvent system 2 S:NMP:NaOH:H 2 The molar ratio between O is 1.0: 3.9: 0.02: 1.5, is that the Na in the formula is ≥ 66.0%wt with purity 2 S. 3 h 2 O solid excess 1% is added in common reactor, under the pressure is -0.92Mpa, is heated to 80 ℃, makes Na 2 After S is fully dissolved, adjust the vacuum degree to -0.73Mpa and then raise the temperature to 150°C, keep the temperature, pressure at -0.73Mpa, stirring speed at 300rpm; dehydration treatment until the water content in the sodium sulfide solution is 1.0mol / molNa 2 After S, after using a quick moisture analyzer to detect the moisture content therein, Na 2 S: p-dichlorobenzene (p-DCB) molar ratio of 1:0.98 is added to p-dichlorobenzene for temperature-rising polymerization to complete the polymerization of polyphenylene sulfide; the amount of nitrogen and energy consumption in this dehydration process are only nitro...

example 8～11

[0032] In the sodium sulfide dehydration treatment stage, in order to make the raw material Na in the solvent system 2 S:NMP:NaOH:H 2 The molar ratio between O is 1.0: 3.9: 0.02: 1.5, is that the Na in the formula is ≥ 66.0%wt with purity 2 S. 3 h 2 O solid excess 1% is added in the common reactor, under pressure is 0.97Mpa, is heated to 80 ℃, makes Na 2 After S is fully dissolved, adjust the vacuum degree to -0.72Mpa and then raise the temperature to 150°C, keep the temperature, pressure at -0.72Mpa, stirring speed at 300rpm; dehydration treatment until the water content in the sodium sulfide solution is 1.0mol / molNa 2 After S, after using a quick moisture analyzer to detect the moisture content therein, Na 2 S: p-dichlorobenzene (p-DCB) with a molar ratio of 1:1.05 is added to p-dichlorobenzene for temperature-rising polymerization to complete the polymerization of polyphenylene sulfide; the amount of nitrogen and energy consumption in this dehydration process are only...

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Abstract

The invention discloses a dehydration process for a polyphenyl thioether resin synthesis solvent system. According to the dehydration process, in a process flow that sodium sulfide and p-dichlorobenzene are taken as raw materials, N-methyl-2-pyrrolidone is taken as a solvent, and polyphenyl thioether resin is produced through condensation polymerization, the purity, whiteness and particle shape of the polyphenyl thioether resin are improved by controlling the content of moisture in a synthetic system so as to meet the requirements on the application and development of polyphenyl thioether resin subsequent products; raw materials, i.e. Na2S, NMP, NaOH and H2O, are enabled to exist in the polyphenyl thioether resin synthesis solvent system in a certain molar ratio; the raw materials, such as Na2S, NMP and NaOH, in a formulation are added into an ordinary reaction kettle in a certain excessive proportion at a dehydration treatment stage; vacuum dehydration treatment is carried out on the polyphenyl thioether resin synthesis solvent system during stirring at certain temperature and pressure under the condition that air in the polyphenyl thioether resin synthesis solvent system is replaced with nitrogen; a dehydration treatment process for the polyphenyl thioether resin synthesis solvent system is completed after the moisture content of the polyphenyl thioether resin synthesis solvent system is determined by adopting a rapid moisture determinator; and meanwhile, NaOH aqueous liquid of certain temperature and concentration is required for absorbing hydrogen sulfide produced due to the fact that the sodium sulfide is unstable and pyrolyzed during dehydration, so as to protect environments from being polluted.

Description

technical field [0001] The invention belongs to the synthesis of polymer material resin, especially the field of polyphenylene sulfide resin production. Background technique [0002] High-performance polyphenylene sulfide has excellent chemical resistance and thermal stability at high temperatures, and has flame retardancy, insulation, radiation resistance and good mechanical properties. In order to explore the synthesis method of this material, researchers from all over the world have been working hard to find it. [0003] In U.S. Patent No. 4,761,468, it is described that chemical substances such as mercapto and mercapto metal salts are used to treat the polyphenylene sulfide resin after synthesizing the polyphenylene sulfide resin, thereby reducing the content of chlorine in the polyphenylene sulfide resin, and then the polyphenylene sulfide resin is processed. The sulfide resin is used in the field of electronic components through modification, and its main purpose is t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/02C08G75/0254
Inventor 李勇邓文皓龚海明周鹏韦霞张勇
Owner SICHUAN DEYANG CHEM
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