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Method for preparing irregular sulfonated poly aromatic (sulfur) ether with high efficiency

A technology for sulfonating polyaromatic sulfide and polyaromatic ether, which is applied in the field of novel and efficient preparation of random sulfonated polyaromatic ether, can solve the problems of complicated recovery process, large volume of reaction solution, long reaction time, etc., and achieves simplification Equipment composition, simplified process, high molecular weight effect

Active Publication Date: 2010-12-29
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 random sulfonated polyaryl (sulfide) ether

Method used

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  • Method for preparing irregular sulfonated poly aromatic (sulfur) ether with high efficiency
  • Method for preparing irregular sulfonated poly aromatic (sulfur) ether with high efficiency
  • Method for preparing irregular sulfonated poly aromatic (sulfur) ether with high efficiency

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Experimental program
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Embodiment 1

[0055] according to figure 2 In the shown reaction device, 3,3'-sodium disulfonate-4,4'-dichlorodiphenylsulfone (SDCDPS, 17.1938g, 35mmol), 4,4'-dichlorodiphenylsulfone (DCDPS, 18.6654 g, 65mmol), 4,4'-biphenol (BP, 18.6210g, 100mmol), anhydrous potassium carbonate (K 2 CO 3 , 27.6420g, 200mmol), 272mL N,N-dimethylacetamide (DMAc) were mixed, the reaction temperature was raised to 180°C, and the reaction was carried out for 12 hours. Stop heating and stirring, and cool to room temperature naturally. The reaction solution was slowly poured into 2L of deionized water to obtain a white fibrous polymer, soaked in 4L of deionized water for 8 hours at 80°C, repeated three times, filtered, dried, and then vacuum-dried at 100°C for 24 hours to obtain a shallow Yellow fibrous polymer (sulfonated polyethersulfone compound), 46.7 g, yield: 99%, intrinsic viscosity: 0.91 dL / g.

Embodiment 2

[0057] according to figure 2 In the shown reaction device, 3,3'-sodium disulfonate-4,4'-dichlorodiphenylsulfone (SDCDPS, 17.1938g, 35mmol), 4,4'-dichlorodiphenylsulfone (DCDPS, 18.6654 g, 65mmol), 4,4'-biphenol (BP, 18.6210g, 100mmol), anhydrous potassium carbonate (K 2 CO 3 , 27.6420g, 200mmol), 272mL of N-methylpyrrolidone (NMP) were mixed, the reaction temperature was raised to 190°C, and the reaction was carried out for 12 hours. Stop heating and stirring, and cool to room temperature naturally. The reaction solution was slowly poured into 2L of deionized water to obtain a light yellow fibrous polymer, soaked in 4L of deionized water at 80°C for 8 hours, repeated three times, filtered, dried, and then vacuum-dried at 100°C for 24 hours to obtain Yellow fibrous polymer (sulfonated polyethersulfone compound), 44.3 g, yield: 94%, intrinsic viscosity: 0.89 dL / g.

Embodiment 3

[0059] according to figure 2 In the shown reaction device, 3,3'-sodium disulfonate-4,4'-dichlorodiphenylsulfone (SDCDPS, 17.1938g, 35mmol), 4,4'-dichlorodiphenylsulfone (DCDPS, 18.6654 g, 65mmol), 4,4'-biphenol (BP, 18.6210g, 100mmol), anhydrous potassium carbonate (K 2 CO 3 , 27.6420g, 200mmol), 272mL N,N-dimethylacetamide (DMAc) were mixed, the reaction temperature was raised to 180°C, and the reaction was carried out for 24 hours. Stop heating and stirring, and cool to room temperature naturally. The reaction solution was slowly poured into 2L of deionized water to obtain a white fibrous polymer, soaked in 4L of deionized water for 8 hours at 80°C, repeated three times, filtered, dried, and then vacuum-dried at 100°C for 24 hours to obtain a shallow Yellow fibrous polymer (sulfonated polyethersulfone compound), 46.7 g, yield: 99%, intrinsic viscosity: 1.04 dL / g.

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Abstract

The invention discloses a method for preparing irregular sulfonated poly aromatic (sulfur) ether with high efficiency. The method comprises the following steps that: a sulfonated monomer, a non-sulfonated monomer and a bisphenol (bisulfide) monomer are used as initial raw materials; carbonate which is 2 to 2.25 times of the total mole number of the bisphenol (bisulfide) is used as alkali and is added into the raw materials; the mixed materials react for 10 to 24 hours in a non-protonic solvent with high boiling point; then reaction solution is slowly poured into deionized water to obtain a white fibriform polymer; subsequently, the white fibriform polymer is soaked for 5 to 10 hours under the condition that the temperature is between 60 and 80 DEG C and the process is repeated for 3 to 5 times; and the white fibriform polymer is subjected to filtering, drying and vacuum drying to obtain the irregular sulfonated poly aromatic (sulfur) ether. The preparation method does not need the addition of toluene, removes the step of water separation, simplifies the process, avoids the use of mass organic, flammable, volatile and toxic solvents and the subsequent complex process of reclaiming and processing waste liquid, reduces the volume of the reaction liquid, shortens the reaction time and reduces energy consumption so as to reduce the cost of the production process and improve the working efficiency.

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 and efficient preparation method of random 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. The polymerization of sulfonated monomers, which is widely used at present, has many advantages compared with the sulfonated polyar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/02C08G65/40C08G75/20C08G75/23
Inventor 张中标宋爱茹郑勇王智强汤红英
Owner 安徽摩纳珀里科技有限公司
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