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A kind of preparation method of polyethersulfone resin

A technology of polyethersulfone resin and polymer solution, applied in the field of polymer synthesis, can solve the problems of difficult polymerization reaction, dark product color, long polymerization cycle, etc. reduced effect

Active Publication Date: 2022-04-22
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the common disadvantages of the above methods are: difficult polymerization reaction, long polymerization cycle, darker product color

Method used

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  • A kind of preparation method of polyethersulfone resin
  • A kind of preparation method of polyethersulfone resin
  • A kind of preparation method of polyethersulfone resin

Examples

Experimental program
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Effect test

preparation example Construction

[0066] Preparation of chain spreaders

[0067] In a four-mouth flask with nitrogen and a reflux water separator, 18.9g of ethylene disultanol was dissolved in 200ml of butanone distilled water, fully dissolved and heated up to 65 ° C, slowly added 26.2g dicyclohexylmethane diisocyanate, the control temperature gradually warmed up to reflux, reaction 2h, cooling after the product precipitated, after filtering with acetone washed 2 times after vacuum drying, to obtain the target bispoyl compound (chain extender X). 1 37.5g, yield 83.2%. The compound was tested for a thiol equivalent of 220, and after conversion, it was learned that the number of repeating units was about 1, that is, m = 1.

[0068] By selecting different types of dithiols and diisocyanates, or adjusting the reaction molar ratios of dithitols and diisocyanates (see Table 2 for details on the preparation of chain spreaders), different structures and different thiol equivalents can be prepared, and the remaining condit...

Embodiment 1

[0072] In a four-mouth flask connected to a condensing tube, water separator, mechanical agitator and thermometer, 93 g of molecularly sieve-dewatered N, N-dimethylacetamide (moisture content 1 Pd / C catalyst 0.029g, reacted at residual temperature (about 135 °C) for 2h to give a polymer solution. Under the condition of high-intensity stirring, the polymer solution was poured into 250ml of water for precipitation, filtered and then boiled for 3 to 4 times, and dried at 180 °C in a vacuum oven for 6h to obtain a finished polyethersulfone resin product of 45.2g.

Embodiment 2

[0074] In the reactor connected to the reflux condensing device, 1195.5g of dichlorodiphenyl ether, 855.26g of potassium carbonate, 1238.96g of bisphenol S, 3749g of N, N-dimethylformamide and 1874g of toluene were added to the reactor, the air in the kettle was extracted to negative pressure, and then nitrogen was introduced to completely replace the air in the kettle; the temperature in the kettle was heated to 110 ~ 112 ° C, and the constant temperature reaction was maintained for 1 hour, and the toluene reflux was maintained until all the generated water was brought out. Toluene is then distilled, heating is stopped, and the reaction solution is cooled to room temperature (25 °C). Continue to pour 198.3 g of chain spreader X into the reactor 2 and 3.587g of copper acetylacetonate, stirred the reaction for 1h to give a polymer solution. Under high-intensity stirring conditions, the polymer solution was precipitated with 9000g methanol, and then washed with water 3 times repeate...

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Abstract

The invention relates to a preparation method of polyethersulfone resin. The method includes the following steps: mixing bisphenol S, dichloro monomer, acid-binding agent, water-carrying agent and solvent, heating under nitrogen protection to form a salt, and at the same time refluxing to separate water; distilling off the water-carrying agent and carrying out prepolymerization reaction at the same time; The chain agent and the catalyst continue to react; the polymer solution is precipitated to obtain polyethersulfone resin. By adopting the self-made dimercapto chain extender containing carbamate groups, the present invention can efficiently and rapidly complete the chain extension reaction, and obtain high molecular weight polyethersulfone resin through polymerization in a short time. Due to the improvement of the chain extension efficiency, the high boiling point polar solvent used in the conventional preparation method is avoided, and the medium and high boiling point polar solvent is used, which reduces the reaction time and reaction temperature, and the economic efficiency is significantly improved. In addition, due to the introduction of carbamate groups, the melt index of the obtained polyethersulfone resin is significantly reduced, which is beneficial to processing and molding, but will not affect the use strength of the resin itself.

Description

Technical field [0001] The present invention belongs to the field of polymer synthesis, specifically relates to a method of low temperature polymerization of polyethersulfone resin. [0002] Technical background [0003] Polyethersulfone is a kind of high-temperature special engineering plastics with aromatic ether bonds and sulfone groups in the main chain, with glass transition temperature above 220 °C, with corrosion resistance, high temperature resistance, creep resistance, impact resistance, flame retardant and other excellent properties, widely used in electronics, medical, machinery, automobiles and other fields. [0004] However, the traditional preparation method of polyethersulfone is to use high boiling point and high polarity solvents such as diphenyl sulfone and cyclobutyl sulfone to slowly polymerize at high temperatures for a long time (EP2225328A1, US20100310804A1, CN85105138A). Such methods applied to actual chemical production have many disadvantages, such as th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/23
CPCC08G75/23
Inventor 仇伟张鑫陈海波
Owner WANHUA CHEM GRP CO LTD
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