Method for preparing aromatic nucleophilic substitution polymer under anhydrous condition

A nucleophilic substitution and polymer technology, applied in the field of preparing aromatic nucleophilic substitution polymers under novel anhydrous conditions, can solve the problems of complicated recycling process, large reaction liquid volume, long reaction time, etc., and reduce energy consumption , simplified process, high molecular weight effect

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 provide polymerization suitable for monomers with low reactivity, or relatively sensitive to water polymerization, to overcome the use of a large number of organic flammable, volatile, toxic solvents and subsequent waste liquid recovery and treatment processes in the prior art Complicated, long reaction time, large volume of reaction solution and high energy consumption, etc., under anhydrous conditions, use inorganic medium strong alkali potassium phosphate to prepare high molecular weight polyaryl (thio) ethers, esters, amines, and amides with high Molecular compounds, for the above purposes

Method used

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  • Method for preparing aromatic nucleophilic substitution polymer under anhydrous condition
  • Method for preparing aromatic nucleophilic substitution polymer under anhydrous condition
  • Method for preparing aromatic nucleophilic substitution polymer under anhydrous condition

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Experimental program
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Effect test

Embodiment 1

[0045] 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 phosphate (K 3 PO 4 , 46.6994g, 220mmol), 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), 46.8 g, yield: 99%, intrinsic viscosity: 0.98 dL / g.

Embodiment 2

[0047] 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 phosphate (K 3 PO 4 , 46.6994g, 220mmol), 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), 44.2 g, yield: 94%, intrinsic viscosity: 0.91 dL / g.

Embodiment 3

[0049] 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), 46.8 g, yield: 99%, intrinsic viscosity: 1.14 dL / g.

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Abstract

The invention relates to a method for preparing a polymer by an aromatic nucleophilic substitution reaction under an anhydrous condition. The method comprises the following steps: in an aprotic polar solvent with high boiling point, an aromatic halide and an acyl halide react with phenol, thiophenol or amine respectively by heating according to the feed ratio of the mole number of 1:1 under the existence of anhydrous potassium phosphate to obtain a corresponding macromolecular compound; and a reaction mixture is poured into deionized water after cooled to room temperature to obtain a white fibrous polymer, immersion is carried out for 5 to 10 hours under the condition of 60 DEG C to 80 DEG C and is repeated for 3 to 5 times, and then the processes of filtration, baking and vacuum drying are carried out to obtain the aromatic nucleophilic substitution polymer. The invention omits a toluene organic solvent and takes the anhydrous potassium phosphate as alkali, the alkalescence of the anhydrous potassium phosphate is equivalent to that of potassium carbonate, a sufficient alkaline condition required by the reaction is ensured, monopotassium phosphate generated by the reaction can not decompose to generate water under the reaction temperature of the invention, so the polymerization method of the invention is a novel preparation method under an absolutely anhydrous condition under the precondition of using inorganic moderately strong alkali.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a method for preparing polyaryl (sulfide) ethers, esters, amines, and amides polymers, and more specifically to a novel method for preparing aromatic nucleophilic substitution polymerization under anhydrous conditions. way of things. Background technique [0002] Aromatic nucleophilic substitution polymerization is a very efficient and widely used method to prepare a variety of polymer materials. These materials include polyaryl (sulfide) ethers, esters, amines, and amides polymer compounds, which can be used in aerospace, aviation, nuclear industry, electronics industry, shipbuilding industry, automobile industry and electromechanical industry, etc., and can also be used as ideal membrane separation materials. Material selection has a wide range of applications in membrane water treatment such as reverse osmosis, nanofiltration, ultrafiltration, microfiltration, osmotic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G85/00C08G75/23C08G65/40
Inventor 张中标王智强王子铱
Owner 安徽摩纳珀里科技有限公司
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