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Efficient preparation method of block sulfonated aromatic poly (thio) ether

A technology of sulfonated polyarylamide and aromatic ether, which is applied in the field of high-efficiency preparation of novel block sulfonated polyaryl ether, can solve the problems of complicated recycling process, large reaction liquid volume, and long reaction time, and achieve simplified equipment composition and simplified process , the effect of high molecular weight

Active Publication Date: 2009-11-18
安徽摩纳珀里科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to overcome the problems in the prior art of using a large amount of organic flammable, volatile, toxic solvents and the follow-up waste liquid recovery and treatment process, long reaction time, large reaction liquid volume and high energy consumption, etc., and provides a Novel preparation method of block sulfonated polyaryl (sulfide) ether

Method used

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  • Efficient preparation method of block sulfonated aromatic poly (thio) ether
  • Efficient preparation method of block sulfonated aromatic poly (thio) ether
  • Efficient preparation method of block sulfonated aromatic poly (thio) ether

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Effect test

Embodiment 1

[0062] Synthesis of lipophilic segment at the end of potassium phenate (taking the molecular weight of 5000g / mol as an example)

[0063] according to figure 2 In the shown reaction device, 4,4'-dichlorodiphenyl sulfone (DCDPS, 14.3580g, 50mmol), 4,4'-biphenol (BP, 10.0838g, 54.2mmol), anhydrous potassium carbonate ( K 2 CO 3 , 14.9820g, 108.4mmol), 122mL N,N-dimethylacetamide (DMAc) were mixed, heated to 180°C, and reacted for 24 hours. Stop heating and stirring, and cool to room temperature naturally. Suction filtration, the filtrate was poured into 800mL of methanol, a white powder was precipitated, filtered, washed with methanol, dried, and then vacuum-dried at 100°C for 24 hours to obtain a lipophilic fragment ending in potassium phenate, 20.4g, yield: 98%, Intrinsic viscosity: 0.22dL / g.

Embodiment 2

[0065] Synthesis of Chlorine-terminated Lipophilic Fragment (Taking a Molecular Weight of 5000g / mol as an Example)

[0066] according to figure 2 In the shown reaction device, 4,4'-dichlorodiphenylsulfone (DCDPS, 15.5641g, 54.2mmol), 4,4'-biphenyldiphenol (BP, 9.3105g, 50mmol), anhydrous potassium carbonate ( K 2 CO 3 , 13.8210g, 100mmol), 124mL N,N-dimethylacetamide (DMAc) were mixed, heated to 180°C, and reacted for 24 hours. Stop heating and stirring, and cool to room temperature naturally. Suction filtration, the filtrate was poured into 800mL methanol, a white powder was precipitated, filtered, washed with methanol, dried, and then vacuum-dried at 100°C for 24 hours to obtain a lipophilic fragment ending in potassium phenate, 20.6g, yield: 97%, Intrinsic viscosity: 0.24dL / g.

Embodiment 3

[0068] Synthesis of Hydrophilic Fragment with Potassium Phenate Tail (Taking Molecular Weight as 5000g / mol as an Example)

[0069] according to figure 2 In the shown reaction device, 3,3'-sodium disulfonate-4,4'-dichlorodiphenyl sulfone (SDCDPS, 24.5625g, 50mmol), 4,4'-biphenyldiphenol (BP, 11.0662g , 56.4mmol), anhydrous potassium carbonate (K 2 CO 3 , 15.5901g, 112.8mmol), 178mL of N-methylpyrrolidone (NMP) were mixed, heated to 180°C, and reacted for 48 hours. Stop heating and stirring, and cool to room temperature naturally. Suction filtration, the filtrate was poured into 1000mL isopropanol, white powder was precipitated, filtered, washed with isopropanol, dried, and then vacuum-dried at 100°C for 24 hours to obtain a hydrophilic fragment ending in potassium phenate, 30.1g, collected Rate: 94%, intrinsic viscosity: 0.18dL / g.

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Abstract

The invention relates to a preparation method of block sulfonated aromatic poly (thio) ether. In the invention, a sulfonated monomer, a non-sulfonated monomer and a bis (thio) phenol monomer are adopted as starting raw materials and react for 10 to 24 hours under the carbonate alkaline condition of an aprotic solvent with high boiling point with the temperature being controlled between 150 DEG C and 200 DEG C so as to effectively prepare a block sulfonated aromatic poly (thio) ether macromolecular compound. In the preparation method, a toluene organic solvent is omitted, the step of azeotropic water division is omitted, the technology is simplified, the use of a large number of organic, flammable, volatile and toxic solvents and subsequent complicated waste liquid recycling processes are avoided, the volume of reaction liquid is reduced, the reaction time is shortened, energy consumption is reduced, the cost of the production technology is reduced, and the work efficiency is increased.

Description

technical field [0001] The invention belongs to the technical field of macromolecular materials, and relates to a preparation method of sulfonated polyaryl (thio)ether polymers, more specifically, a novel high-efficiency preparation method of block sulfonated polyaryl (thio)ether. Background technique [0002] Sulfonated polyaryl (sulfide) ether can be used as film, sheet, plate, tube, fiber, coating and other structural materials for aerospace, aviation, nuclear industry, electronics industry, shipbuilding industry, automobile industry and electromechanical industry, etc. As an ideal material for membrane separation, it has a wide range of applications in membrane water treatment such as reverse osmosis, nanofiltration, ultrafiltration, microfiltration, osmotic distillation, ion exchange, electrodialysis, and proton exchange membrane fuel cells. Sulfonated polyarylene (thio)ether polymer materials contain both hydrophilic and lipophilic parts, the former provides channels f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/40C08G75/04C08G75/20C08G75/23
Inventor 张中标宋爱茹郑勇王智强汤红英王子铱刘小斌
Owner 安徽摩纳珀里科技有限公司
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