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Polysulfone preparation method

A technology for polysulfone and polymerization reaction, which is applied in the field of preparing polysulfone and can solve the problems of cumbersome reaction steps, chain scission, complicated process and the like

Active Publication Date: 2019-10-22
NINGXIA QINGYAN POLYMER MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polymerization reaction steps are cumbersome, the process is complicated, the reaction time is long, and the energy consumption is large.
The above-mentioned salt-forming reaction takes a long time, and the temperature in the reactor reaches 160°C after the salt-forming is completed. In order to ensure that the next polycondensation reaction is not too violent, the temperature must be lowered to 120°C first, and then the temperature is raised for polycondensation; in addition, the salt-forming stage produces The water needs to be taken out of the system in time to prevent the decrease of the monomer concentration and the hydrolysis side reaction of the halogen-containing monomer at high temperature, so it is usually necessary to ensure sufficient water separation time, which is usually 2.5-8.5h, and the result is from salt formation From the beginning of the reaction until the completion of polycondensation, the whole cycle takes up to 18h
And adopt single sodium hydroxide strong alkali to carry out reaction cycle long, easily cause polymer aging, chain scission phenomenon takes place

Method used

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  • Polysulfone preparation method

Examples

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Effect test

preparation example Construction

[0020] In the method for preparing polysulfone, the potassium carbonate described in step (1) is granular potassium carbonate with a particle size of 100-600 mesh.

[0021] The method for preparing polysulfone, the solid 4,4'-dichlorodiphenyl sulfone, bisphenol A, dimethylacetamide, toluene described in step (2), and the mixed drying method prepared in step (1) The feeding ratio of the material is: the parts by weight of each component are: 50 parts by weight of solid 4,4'-dichlorodiphenyl sulfone, 50 parts by weight of bisphenol A, 30 parts by weight of dimethylacetamide, 1.95-2.13 parts by weight of the mixed dried product prepared in step (1), and 15 parts by weight of toluene.

[0022] In the method for preparing polysulfone, the water separation temperature in step (2) is preferably 140°C.

[0023] In the method for preparing polysulfone, the polymerization reaction temperature in step (2) is preferably 180°C.

[0024] In the method for preparing polysulfone, the washin...

specific Embodiment

[0027] Sodium hydroxide, potassium hydroxide, and potassium carbonate were mixed and dried according to Table 1 below; then solid 4,4'-dichlorodiphenyl sulfone (DCDPS), bisphenol A (BPA), dimethylacetamide (DMAC), toluene (Tol), mixed and dried sodium hydroxide (NaOH), potassium hydroxide (KOH), potassium carbonate (K 2 CO 3 ) mixed and dried under the protection of nitrogen, water separation at 140°C for 4 hours; heating to 180°C for 4 hours of polymerization reaction; cooling to room temperature after completion of the polymerization reaction, sedimentation of the polymer into deionized water, washing at 80°C 5 times and dry, test intrinsic viscosity is as follows: the mensuration method of viscosity is to carry out viscosity measurement with Ubbelohde viscometer according to common capillary viscometry method in the present embodiment:

[0028]

[0029] It can be seen from the above comparative examples and examples that under the same reaction conditions and the same p...

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Abstract

The present invention provides a polysulfone preparation method, which comprises: (1) mixing sodium hydroxide, potassium hydroxide and potassium carbonate according to a mass ratio of 1:1:(0.25-0.45),and drying; (2) mixing a solid 4,4'-dichlorodiphenyl sulfone, bisphenol A, dimethylacetamide, toluene and the mixed dried product prepared in the step (1), carrying out water separation for 4 h undernitrogen protection at a temperature of 136-144 DEG C, heating to a temperature of 178-188 DEG C, and carrying out a polymerization reaction for 4 h; and (3) cooling to a room temperature after completing the polymerization reaction, settling the polymer in deionized water, washing, and drying. According to the present invention, the method can conveniently and rapidly produce the phenol salt, shorten the water separation time, avoid the chain breaking phenomenon, and improve the quality of the polymer product.

Description

Technical field: [0001] The invention relates to a method for preparing polysulfone, belonging to the technical field of organic chemistry. Background technique: [0002] Polysulfone has a sulfone group (-SO 2 -) and arylene group thermoplastic resin, English name Polysulfone (referred to as PSF or PSU). In the industrial synthesis of polysulfone, bisphenol A and sodium hydroxide solution are usually reacted in dimethyl sulfoxide solvent to generate bisphenol A sodium salt. After the salt-forming reaction is completed, the water-carrying agent is evaporated, and then solid is added under nitrogen protection. 4,4'-dichlorodiphenyl sulfone, start stirring, then gradually increase the temperature at 150-160°C for polycondensation reaction to generate polysulfone, and the polymerization reaction ends in about 3 hours (controlled by viscosity). This polymerization reaction step is loaded down with trivial details, and process is complicated, and reaction time is long, and energ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/23
CPCC08G75/23
Inventor 张东宝张奇
Owner NINGXIA QINGYAN POLYMER MATERIALS CO LTD