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Preparation method of polyarylphenyl resin by phase-transferring catalyst

A technology of phase transfer catalyst and polyarylene sulfide, which is applied in the field of preparation of polyarylene sulfide resin by phase transfer catalyst, to achieve the effects of easy recovery, stable properties and improved activity

Active Publication Date: 2008-05-14
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The phase transfer catalyst involved in the present invention prepares the method for polyarylene sulfide resin by the solution polycondensation method, so far, there is no relevant literature report in China

Method used

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  • Preparation method of polyarylphenyl resin by phase-transferring catalyst
  • Preparation method of polyarylphenyl resin by phase-transferring catalyst
  • Preparation method of polyarylphenyl resin by phase-transferring catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1. Add 400ml of N-methylpyrrolidone, 6.3g of sodium benzoate and polyethylene glycol 37.4 with a molecular weight of 4000 into the reaction kettle, stir well and add Na with a content of ≈60%.2 S·XH 2 O 100g, in N 2 Under protection, after dehydration at a temperature of 190°C, 117.6 g of p-dichlorobenzene was added and reacted at a temperature of 230°C for 5.0 hours to obtain a polyphenylene sulfide resin.

[0048] After the above reaction is completed, the solid-liquid system is separated, and the solid is washed and dried to obtain pure polyphenylene sulfide resin.

[0049] Using a-chloronaphthalene as a solvent, prepare a sample solution of about 0.40g / dl, and use an Ubbelohde viscometer at 208±0.5°C to measure the intrinsic viscosity of polyphenylene sulfide resin η=0.35.

Embodiment 2

[0050] Embodiment 2. With dimethyl sulfoxide 1000ml, lithium formate 8.4g and crown ether 15-crown-5 1.2g, add in the three-neck bottle that import tube, stirrer, thermometer and water separator are housed, after stirring Add content ≈60% Na 2 S·XH 2 O 100g, p-dichlorodiphenyl sulfone 229.6g, in N 2 Under protection, dehydration reaction was carried out at a temperature of 170° C. for 1 h. After the reaction system was dehydrated, the temperature of the system was raised to 180° C. for 6 hours to obtain a polyarylene sulfide resin.

[0051] Pour the above polyarylene sulfide sulfone resin into the precipitating agent water while it is hot, precipitate the polymer, and obtain pure polyarylene sulfide sulfone resin after washing and drying.

[0052] Using NMP as a solvent, prepare a sample solution of about 0.50g / dl, and use an Ubbelohde viscometer at 30.0±0.1°C to test the intrinsic viscosity of polyarylene sulfide sulfone resin η=0.25.

Embodiment 3

[0053] Embodiment 3. With N-cyclohexylpyrrolidone 600ml, sodium acetate 10g and quaternary ammonium chloride trioctyl dodecyl ammonium chloride 17.5g, add introduction tube, stirrer, thermometer and water separator three In the neck bottle, after stirring evenly, add 32.7g of sulfur ≈98%, 174.4g of p-difluorobenzone, in N 2 Under protection, dehydration reaction was carried out at a temperature of 120° C. for 4 h. After the reaction system was dehydrated, the temperature of the system was raised to 204° C. for 8 hours to prepare a polyarylene sulfide ketone resin.

[0054] The polyarylene sulfide ketone resin precipitate is separated from the solution, and the pure polyarylene sulfide ketone resin is obtained after washing and drying.

[0055] Use concentrated sulfuric acid as a solvent to prepare a sample solution of about 0.50g / dl, and use an Ubbelohde viscometer at 30.0±0.1°C to test the intrinsic viscosity of polyarylene sulfide ketone resin η=0.21.

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Abstract

Production of polyaryl sulfide resin by phase transferring agent is carried out by adding solvent 400-1000 proportion, catalyst 1-38 proportion and auxiliary catalyst 1-20 proportion into reactor with connecting conduct, agitator, thermometer and water distributor, agitating, adding into 60% Na2S.XH2O 100 proportion or NaHS 56 proportion or sulfacid 32.7 proportion, dihalogenated aromatic compound or dihalgenated heterocylic compound or its derivative 10-600 proportion, dewater reacting at 100-200degree for 0.5-4hrs under N2 protection, raising temperature to 150-230degree for 1-20hrs, filtering or pouring it into precipitant liquid, eluting out polymer, washing and drying to obtain purified final product.

Description

technical field [0001] The invention relates to a method for preparing polyarylene sulfide resins with a phase transfer catalyst, which belongs to the field of polymer preparation. Background technique [0002] Phase transfer catalysis (Phase transfer catalyst) overcomes the disadvantage of requiring polar aprotic solvents in heterogeneous organic synthesis, and has greatly promoted the development of organic synthesis. Phase transfer catalysis refers to the process of using a small amount of material as a carrier of a reactant to migrate the reactant to another phase through the phase interface, so that the heterogeneous reaction can proceed smoothly (Liu Zengxun, phase transfer catalyst in organic chemistry and pesticides Application in Chemistry, Anhui Chemical Industry Research Institute, 1987.12(3~7)). Solution polycondensation method to prepare polyarylene sulfide resin, the sulfur source can only reach the dispersion equilibrium in the organic solvent, and it is in a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/02C08G75/23C08G75/0213C08G75/0236C08G75/024C08G75/0254C08G75/0263
Inventor 杨杰刘春丽龙盛如
Owner SICHUAN UNIV