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A process for purifying polysulfone resin material by critical phase change extraction

A technology of polysulfone resin and extraction method, which is applied in the field of purification of polysulfone resin materials by critical phase change extraction method, can solve the problems of difficult recycling, high ash content of products, and decline in product performance, and achieve uniform product performance and The effect of low ash content and low production cost

Active Publication Date: 2022-07-19
FUHAI (DONGYING) ADVANCED MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The disadvantages of the purification process of the above two polysulfone resins are obvious: 1. Since polysulfone materials themselves are non-hydrophilic materials, the surface tension of water is relatively high, and the water boiling method can only clean the surface layer of polysulfone materials, not In the state of full immersion, the polysulfone particles with larger particle size and the inorganic salts wrapped inside cannot be effectively removed. Therefore, it will inevitably cause the problems of high ash content, low purity, and decline in product performance; 2. Longer immersion time, production The cycle is longer and the cost increases; 3. The waste water produced is more, the recycling process is difficult and expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0036] The preparation process of the polysulfone resin solution is as follows: the mixture of phenolic substance and sulfone substance is put into the reaction kettle as raw material, acid binding agent, solvent and water-carrying agent according to the proportion, and the reaction kettle is evacuated and nitrogen purged , The nitrogen standard is high-purity nitrogen, the total time of the polymerization reaction with water above 150℃ is 12~20h, the temperature in the kettle reaches 150~220℃, and the reaction is ended when the viscosity in the kettle reaches the requirement. The known range of the viscosity of the polysulfone material polymerization solution is 4000-12000 mpa.s, all of which are suitable for the purification process of the present invention.

[0037] After the reaction is completed, the polymerization solution in the reaction kettle is cooled and diluted to 80-90° C., and then the polysulfone resin solution is purified by the process of the present invention....

Embodiment 1

[0040] The process for purifying the polysulfone resin material by the critical phase change extraction method of the present embodiment specifically includes the following steps:

[0041] Add 8.78kg of 4,4'-dichlorodiphenylsulfone, 7.35kg of bisphenol S, 5.44kg of potassium carbonate, 60kg of solvent sulfolane, 15kg of xylene with water agent into the 100L polymerization reaction kettle, and vacuumize the kettle to ≤0.08MPa Then, nitrogen was introduced to make the pressure in the kettle reach ≥ 0.01MPa. After nitrogen replacement three times, the reaction at normal pressure in the kettle was maintained. The polymerization temperature was 200°C, the polymerization time was 14h, and the polymerization stirring speed was 100r / min. When the polyethersulfone resin solution reaches the target viscosity of 8000mpa.s, the reaction ends.

[0042] After the reaction is completed, the heating temperature of the heating medium in the kettle is lowered from 200 ° C to 90 ° C, and fresh s...

Embodiment 2

[0046] The process for purifying the polysulfone resin material by the critical phase change extraction method of the present embodiment specifically includes the following steps:

[0047] 9.2kg of 4,4'-dichlorodiphenyl sulfone, 6.41kg of bisphenol A, 5.27kg of potassium carbonate, 65kg of solvent dimethylacetamide, 20kg of water agent xylene were added to the 100L polymerization reaction kettle, and the kettle was evacuated After reaching ≤0.08MPa, nitrogen was introduced to make the pressure in the kettle reach ≥0.01MPa. After three nitrogen replacements, the reaction at normal pressure in the kettle was maintained. The polymerization temperature was 164°C, the polymerization time was 12h, and the polymerization stirring speed was 200r / min. When the polysulfone resin solution reaches the target viscosity of 6500mpa.s, the reaction ends.

[0048] After the reaction, the heating temperature of the heating medium in the kettle was lowered from 164°C to 85°C, and fresh dimethyla...

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Abstract

The invention discloses a process for purifying polysulfone resin material by a critical phase change extraction method. The emulsifier-deionized water compound solution is added dropwise, and the entire dropping process is divided into at least three stages. Each stage is added dropwise at a constant speed, and the dropping amount and dropping speed are gradually increased; Stir, extract the gel-like solid phase in the upper layer of the reaction kettle, thoroughly crystallize the polysulfone resin into a solid by deionized water, then pulverize it into powder, and wash off the residual solvent. The invention has the advantages of simple and easy process, low production cost, energy saving and environmental protection, high production efficiency, high purity of the prepared target product, low ash content, narrower molecular weight distribution, uniform and stable product performance, and can be applied to various high-end fields.

Description

technical field [0001] The invention relates to the technical field of purification of polysulfone resin materials, in particular to a process for purifying polysulfone resin materials by a critical phase change extraction method. Background technique [0002] Polysulfone is a slightly amber amorphous transparent or translucent polymer, an amorphous, thermoplastic resin. Synthesis of polysulfone resins: the main raw materials are 4,4'-dichlorodiphenylsulfone, bisphenol A, bisphenol S, 4,4'-dihydroxybiphenyl, potassium carbonate or potassium bicarbonate, sodium carbonate, etc. polymerized in solvent. When the polymer solution reaches the target viscosity, the polysulfone materials need to be post-treated and purified. [0003] The purification process of polysulfone resin directly determines the performance and quality of the product. At present, the most advanced purification process of polysulfone resin is mainly the purification process of normal pressure or high pressur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/20C08G75/23
CPCC08G75/20C08G75/23Y02P20/54
Inventor 高天正王敏潘家永廖广明
Owner FUHAI (DONGYING) ADVANCED MATERIAL TECH CO LTD