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Preparation method for reducing cyclic dimer in polysulfone resin polymer material

A technology for polymer materials and cyclic dimers, which is applied in the field of preparation of cyclic dimers, can solve the problems of adverse effects on the product quality of polysulfone materials, affecting the storage and use of polysulfone materials, and being difficult to dissolve and remove, etc. The effect of reducing the influence of cyclic dimer impurities, the preparation method is simple and convenient, and the quality is improved

Inactive Publication Date: 2019-12-03
NANJING QINGYAN POLYMER NEW MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the polysulfone material synthesized by this one-step method contains a large proportion of about (0.5wt%) cyclic dimer by-products, which adversely affects the product quality of the polysulfone material
[0004] This cyclic dimer slowly crystallizes from polysulfone solution in polar aprotic solvents such as dimethylformamide (DMF) or dimethylacetamide (DMAC), making the production of polysulfone downstream products, solvent In the process of preparing polymers, such as the casting process of ultrafiltration membranes, there are production problems of crystallization
Moreover, this cyclic dimer deposits on the wall of the polysulfone solution storage container as hard crystalline scale. Once formed, this scale is extremely difficult to dissolve, insoluble in traditional organic solvents, and difficult to dissolve and remove at a temperature of 400 ° C. Storage and use of polysulfone materials

Method used

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  • Preparation method for reducing cyclic dimer in polysulfone resin polymer material
  • Preparation method for reducing cyclic dimer in polysulfone resin polymer material
  • Preparation method for reducing cyclic dimer in polysulfone resin polymer material

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 1) First, add 33.3kg DMAC into a 150L reactor, except for DCDPS, other materials bisphenol A BPA10kg, K 2 CO 3 11.5kg and 33.3kg of Tol were all added to the reaction kettle, water was separated for 8 hours at 140°C, Tol was evaporated, and the temperature was raised to 180°C. Dissolve 10kg of DCDPS in 33.3kg of DMAC, add dropwise to the reaction solution, complete the addition in 45 minutes, keep at 180°C for 4 hours for polymerization;

[0030] 2) Post-treatment: After the reaction is completed, cool to room temperature, settle into deionized water, wash 5 times at 80°C, and dry to obtain powdered bisphenol A polysulfone product (PSU);

[0031] 3) The obtained polysulfone product was tested for intrinsic viscosity by Ubbelohde viscometer and molecular weight distribution by GPC for gel permeation chromatography, and the content of cyclic dimer was determined to be 0.015 wt%.

Embodiment 2

[0033] 1) First, add 5kg DCDPS and 33.3kg DMAC into a 150L reactor, and the remaining materials bisphenol A BPA10kg, K 2 CO 3 11.5kg and 33.3kg of Tol were all added to the reaction kettle, water was separated for 8 hours at 140°C, Tol was evaporated, and the temperature was raised to 180°C. Dissolve 5kg DCDPS in 33.3L DMAC, add it dropwise to the reaction solution, complete the addition in 45 minutes, keep at 180°C for 4 hours for polymerization;

[0034] 2) Post-treatment: After the reaction is completed, cool to room temperature, settle into deionized water, wash 5 times at 80°C, and dry to obtain powdered bisphenol A polysulfone product (PSU);

[0035] 3) The obtained polysulfone product was tested for intrinsic viscosity with Ubbelohde viscometer and molecular weight distribution with gel permeation chromatography (GPC), and the content of cyclic dimer was determined to be 0.011 wt%.

Embodiment 3

[0037] 1) First, add 33.3kg DMAC into a 150L reactor, except for DCDPS, other materials include bisphenol S 10kg, K 2 CO 3 11.5kg and 33.3kg of Tol were all added to the reaction kettle, water was separated for 8 hours at 140°C, Tol was evaporated, and the temperature was raised to 180°C. Dissolve 10kg of DCDPS in 33.3kg of DMAC, add dropwise to the reaction solution, complete the addition in 45 minutes, keep at 180°C for 4 hours for polymerization;

[0038] 2) Post-treatment: After the reaction is completed, cool to room temperature, settle into deionized water, wash 5 times at 80°C, and dry to obtain powdery polyethersulfone product (PES);

[0039] 3) The intrinsic viscosity of the obtained polysulfone product was tested by Ubbelohde viscometer and the molecular weight distribution was tested by GPC by gel permeation chromatography, and the content of cyclic dimer was determined to be 0.019 wt%.

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Abstract

The invention provides a preparation method for reducing cyclic dimer in a polysulfone resin polymer material. The preparation method comprises the steps that 4,4'-dichlorodiphenyl sulfone, a polymerized monomer and potassium carbonate are taken as raw materials, dimethylacetamide is taken as an organic solvent, and methylbenzene or xylene is taken as a water removing agent; and when reaction starts, the polymerized monomer, the potassium carbonate, the organic solvent and the water removing agent are completely added into a reaction kettle according to the reaction using amount firstly, meanwhile, the dimethylacetamide with the amount being half of the reaction using amount is added, the 4,4'-dichlorodiphenyl sulfone is not added or the 4,4'-dichlorodiphenyl sulfone with the amount beinghalf of the reaction using amount is added, water distribution is conducted for 8 hours under the condition of 140+ / -5 DEG C, Tol is steamed away, after the temperature is increased to be 180+ / -5 DEGC, the 4,4'-dichlorodiphenyl sulfone of the remaining reaction using amount is dissolved in the other half of reaction using amount of dimethylacetamide, a mixture is added into the reaction kettle dropwise and completely added within 0.5-1 hour, and the temperature is maintained at 180+ / -5 DEG C for polymerization for 4 hours. According to the preparation method, the content of the cyclic dimer in a polysulfone product can be effectively decreased.

Description

Technical field: [0001] The invention relates to a preparation method for reducing cyclic dimers in polysulfone resin polymer materials, and belongs to the technical field of polymer materials. Background technique: [0002] Polysulfone is a high molecular polymer, an amorphous, thermoplastic resin. At present, industrialized polysulfone resins mainly include bisphenol A polysulfone (PSU / PSF), polyethersulfone (PES / PESU), polyphenylsulfone / polyarylsulfone / polyphenylenesulfone (PPSU). Its characteristics are: excellent mechanical properties, high rigidity, wear resistance, high strength, etc. Due to its good characteristics, polysulfone has been widely used in medical equipment, aerospace, electronics and other high-end materials. [0003] At present, the most advanced production technology of polysulfone polymer materials is a one-step synthesis method. One-step synthesis method: main raw materials 4,4'-dichlorodiphenyl sulfone, polymerized monomer, potassium carbonate or ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/23
CPCC08G75/23
Inventor 张建民于冉张奇张东宝
Owner NANJING QINGYAN POLYMER NEW MATERIAL CO LTD
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