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Preparation method of polyphenylene sulfide resin with low ion precipitation

A technology of polyphenylene sulfide resin and ions, which is applied in the field of polymer material synthesis, can solve the problems such as inability to remove ions, achieve the effects of reducing the discharge of three wastes, reducing the pickling process, and maintaining microscopic stability

Active Publication Date: 2022-08-05
四川中科兴业高新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is: in order to solve the technical problem that the above-mentioned existing purification process only solves the problem of low-chlorine grade resin, but other ions cannot be removed, the present invention provides a preparation method of low-ion precipitation polyphenylene sulfide resin

Method used

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  • Preparation method of polyphenylene sulfide resin with low ion precipitation
  • Preparation method of polyphenylene sulfide resin with low ion precipitation
  • Preparation method of polyphenylene sulfide resin with low ion precipitation

Examples

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Effect test

Embodiment 1

[0038] A preparation method of low-ion precipitation polyphenylene sulfide resin, using sodium sulfide pentahydrate, sodium hydroxide, p-dichlorobenzene and lithium acetate composite catalyst as raw materials, in N-methylpyrrolidone solvent, polycondensation into low-ion precipitation The polyphenylene sulfide resin, the specific technological process comprises the following steps:

[0039] (1) dehydration of sodium sulfide: 17.5kgN-methylpyrrolidone is added in the reactor, then add sodium sulfide pentahydrate 7.6kg, sodium hydroxide 0.2kg, composite catalyst 0.64kg (the composite catalyst is barium hydroxide and lithium acetate, hydrogen The mol ratio of barium oxide and lithium acetate is 1:1), drop into the dehydration kettle successively, then feed into nitrogen protection, open stirring, and the stirring speed is controlled at 80rpm, and the temperature of the system kettle is from normal temperature with a heating rate of 1.5 ℃ / min. After warming up to 202℃ for 10min, s...

Embodiment 2

[0045] A preparation method of low-ion precipitation polyphenylene sulfide resin, using sodium sulfide, sodium hydroxide, p-dichlorobenzene and lithium acetate composite catalyst as raw materials, in N-methylpyrrolidone solvent, polycondensation into low-ion precipitation poly Phenyl sulfide resin, the concrete technological process comprises the following steps:

[0046] (1) dehydration of sodium sulfide: 17.5kgN-methylpyrrolidone is added in the reactor, then add sodium sulfide pentahydrate 7.6kg, sodium hydroxide 0.2kg, composite catalyst 0.64kg (the composite catalyst is barium hydroxide and lithium acetate, hydrogen The mol ratio of barium oxide and lithium acetate is 1:1), drop into the dehydration kettle successively, then feed into nitrogen protection, turn on stirring, the stirring speed is controlled at 80rpm, and the temperature of the system kettle is from normal temperature with a heating rate of 1.5 ℃ / min After warming up to 202℃ for 10min, stop dehydration;

[...

Embodiment 3

[0054] A preparation method of low-ion precipitation polyphenylene sulfide resin, using sodium sulfide, sodium hydroxide, p-dichlorobenzene and lithium acetate composite catalyst as raw materials, in N-methylpyrrolidone solvent, polycondensation into low-ion precipitation poly Phenyl sulfide resin, the concrete technological process comprises the following steps:

[0055] (1) dehydration of sodium sulfide: 17.5kgN-methylpyrrolidone is added in the reactor, then add sodium sulfide pentahydrate 7.6kg, sodium hydroxide 0.2kg, composite catalyst 0.64kg (the composite catalyst is barium hydroxide and lithium acetate, hydrogen The mol ratio of barium oxide and lithium acetate is 1:1), drop into the dehydration kettle successively, then feed into nitrogen protection, turn on stirring, the stirring speed is controlled at 80rpm, and the temperature of the system kettle is from normal temperature with a heating rate of 1.5 ℃ / min After warming up to 202℃ for 10min, stop dehydration;

[...

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Abstract

The invention discloses a preparation method of polyphenylene sulfide resin with low ion precipitation, relates to the field of preparation of polyphenylene sulfide resin with low anion and cation precipitation, solves the problems that the existing purification process only solves the problem of low-chlorine resin and other ions cannot be removed, and comprises the steps of sodium sulfide dehydration, paradichlorobenzene dissolution and first-stage prepolymerization. Carrying out second-stage polymerization, filtering, washing and drying, third-stage polymerization and fourth-stage polymerization, cooling to below 50 DEG C after constant temperature is finished, and separating to obtain low-ion precipitation polyphenylene sulfide resin; after the polyphenylene sulfide resin subjected to primary polymerization is washed, the activity of the water-containing resin is increased, and unstable positive ions and negative ions on end groups on the surface layer of the polyphenylene sulfide resin are removed; removing moisture, adding N-methyl pyrrolidone and a catalyst again to open the chain of the polyphenylene sulfide again, removing unstable end groups in the resin and trace anions and cations wrapped in the middle of the resin, separating out the polyphenylene sulfide, and polymerizing again through the catalyst to obtain the polyphenylene sulfide resin with high purity and low ion separation.

Description

technical field [0001] The invention relates to the technical field of polymer material synthesis, and more particularly to the technical field of preparation of polyphenylene sulfide resin with low anion and cation precipitation. Background technique [0002] Polyphenylene sulfide is a special engineering resin industrialized by Phillips in the 1960s. It has the characteristics of high temperature resistance, radiation protection, self-flame retardant, high strength and high modulus, and is widely used in automobiles, environmental protection, military industry, aerospace and other fields. At present, most domestic and foreign manufacturers continue to use the polymerization process developed by Phillips for the production of polyphenylene sulfide. During the synthesis process, many ions of the raw materials cannot be removed due to technological reasons, resulting in polyphenylene sulfide. The purity of the resin is not suitable for the use of hydrogen energy. The 21st ce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/0254C08G75/0281C08J5/04C08L81/02C08K7/14
CPCC08G75/0254C08G75/0281C08J5/043C08J2381/02C08K7/14Y02E60/50Y02E60/10
Inventor 刘洪陈云冯杰陈俊
Owner 四川中科兴业高新材料有限公司
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