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Production method of polyphenylene sulfide resin and recovery method of rectification raffinate

A technology of polyphenylene sulfide resin and production method, which is applied in the direction of chemical recovery, etc., can solve the problems that metal salt catalysts cannot obtain qualified products, do not save production costs, and have a large melt flow index, so as to reduce environmental pollution pressure, The effect of reducing energy consumption and simple equipment

Active Publication Date: 2019-03-29
SICHUAN NIUPAISI NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the process of producing polyphenylene sulfide by the sodium sulfide method, when alkali metal chloride is used as a catalyst, it must be an industrial superior product with a purity ≥ 99%, although in the prior art, metal salt catalysts or cosolvents must be used. Recycling, but the recovery rate is not high, the general recovery rate is only 50-70%, more importantly, when the recovered metal salt catalyst is used to produce polyphenylene sulfide in actual production, the obtained polyphenylene sulfide cannot meet the standard at all, and the obtained resin The color is darker, the molecular weight is not high, and the melt flow index is relatively large (≥500g / 10min), that is, the recovered metal salt catalyst cannot obtain qualified products; therefore, the so-called recovery does not save production costs, or can only be used as Other use, and can not be reused to produce qualified polyphenylene sulfide products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 100kg of lithium chloride-containing polyphenylene sulfide solvent recovery tower kettle residual slurry and 500kg of methanol into the dilution tank respectively, dilute and disperse the viscous slurry, and add 20kg of sodium carbonate for stirring and precipitation, and the mixed solution Carry out filtration, collect filter cake and filtrate, and backwash filter cake with 10kg methanol, merge the filtrate that collects before and send into the solvent recovery finished product tower to handle; Add 0.5kg of caustic soda to adjust the pH of the solution to 6, 0.1kg of PVA0588, and 0.1kg of magnesium chloride to purify and filter the catalyst solution, and rinse the filter cake with 30kg of methanol again, send the combined liquid into an evaporator, concentrate and dry the catalyst solution to contain the catalyst 30%, as a catalyst for the next batch of polyphenylene sulfide resin synthesis.

[0035] The preparation method of polyphenylene sulfide is the disclosed...

Embodiment 2

[0038]Add 100kg of residual slurry in the polyphenylene sulfide solvent recovery tower containing lithium acetate, and 100kg of water into the dilution tank, dilute and disperse the viscous slurry, and add 100kg of potassium carbonate for stirring and precipitation, and the mixed solution is Filter, collect the filter cake and filtrate, and backwash the filter cake with 100kg of water, combine the filtrate collected before and send it to the solvent recovery finished product tower for processing; the filter cake is transferred to the neutralization tank, add 100kg of glacial acetic acid for acidification, and add 10kg of ammonia water is used to adjust the pH of the solution to 8, 10kg of PVA1700, and 10kg of magnesium nitrate to purify and filter the catalyst solution, and to wash the filter cake with 50kg of water again, and the combined liquid is sent to an evaporator, and the catalyst solution is concentrated and dried to contain 50% of the catalyst. As a catalyst for the n...

Embodiment 3

[0041] 100kg of residual slurry in the polyphenylene sulfide solvent recovery tower containing cesium chloride and 300kg of ethanol were added to the dilution tank respectively, the viscous slurry was diluted and dispersed, and 80kg of potassium carbonate was added to stir and precipitate, and the mixed solution Filter, collect the filter cake and filtrate, and backwash the filter cake with 60kg of ethanol, combine the filtrate collected before and send it to the solvent recovery finished product tower for processing; the filter cake is transferred to the neutralization tank, add 60kg industrial hydrochloric acid for acidification, and Add 1kg of caustic soda to adjust the pH of the solution=7.2, 5kg PEG-400, and 1kg calcium chloride to purify and filter the catalyst solution, and rinse the filter cake with 10kg ethanol again, and send the combined liquid into an evaporator, concentrate and dry the catalyst solution to contain 60% of the catalyst is used as a catalyst for the n...

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Abstract

The invention relates to a method for producing polyphenylene sulfide resin and a method for recycling rectification residue thereof, and belongs to the field of polymer synthesis. The invention provides a method for producing a polyphenylene sulfide resin by using a sodium sulfide-based production process with paradichlorobenzene and sodium sulfide as raw materials in the presence of an alkaline metal chloride solution with the purity of 30 wt% to 70 wt% as a catalyst, wherein the preparation method for the catalyst comprises the following steps: (1) diluting and dispersing the rectification residue obtained in the sodium sulfide-based process of producing polyphenylene sulfide with a diluent, precipitating and filtering, and collecting the filter cake and filtrate; (2) acidifying the filter cake with an industrial hydrochloric acid or glacial acetic acid to obtain a catalyst solution, then adding a pH value regulator, a flocculating agent and a negative ion remover to purify and filter the catalyst solution; and concentrating and drying the purified catalyst solution till the mass of the catalyst in the mixed solution is 30% to 70 %. The present invention produces an industrial polyphenylene sulfide resin with standard-meeting performance by using the recycled metal salt catalyst.

Description

technical field [0001] The invention relates to a production method of polyphenylene sulfide resin and a recovery method of rectification raffinate, belonging to the field of polymer synthesis. technical background: [0002] Polyphenylene sulfide is a heat-resistant high-performance polymer with high temperature resistance, corrosion resistance, excellent electrical properties, mechanical properties and dimensional stability. It is an important variety of high-performance polymer materials and has a wide range of applications in various fields of the national economy. Applications. [0003] At present, there are multiple synthetic routes for polyphenylene sulfide, but there are two routes that have been industrialized or have industrial value: one method is the industrialized Phillips route (i.e. sodium sulfide method), and the other method has industrial value The sulfur solution polycondensation route (ie sulfur solution method). [0004] At present, the first method is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/0259C08J11/00C08J11/02
CPCY02P20/584
Inventor 杨杰张刚李相达
Owner SICHUAN NIUPAISI NEW MATERIALS CO LTD