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Polyarylene amide sulfides polymers and preparation method thereof

A polyarylene sulfide amide and polymer technology, which is applied in the field of polymer synthesis, can solve the problems of harsh solvent purity, high toxicity of aminothiophenol, unfavorable industrial production, etc., and achieve the effect of low cost, high molecular weight and easy processing

Inactive Publication Date: 2008-07-09
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] People such as Wu Qixian had initially studied the synthesis of novel polyarylene sulfide amide resin in the 1990s, but the resin molecular weight obtained was very low and had no practical value; European Patent EP0162606A1 reported the synthesis of polyarylene sulfide amide with p-aminothiophenol, The p-aminothiophenol used is highly toxic, pollutes the environment, has strict requirements on the purity of the solvent in the polymerization reaction, complex process and high cost, which is not conducive to industrial production

Method used

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  • Polyarylene amide sulfides polymers and preparation method thereof
  • Polyarylene amide sulfides polymers and preparation method thereof
  • Polyarylene amide sulfides polymers and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Embodiment 1, with 37.2g 4,4'-diaminodiphenyl sulfone, 30g triethylamine and 200ml tetrahydrofuran, add successively in the reactor that has stirrer, thermometer, dropping funnel, add paraffin in the dropping funnel 55g of fluorobenzoyl chloride, when the temperature drops to -5°C, start to add p-fluorobenzoyl chloride dropwise, finish adding it within 1 hour, keep it for 3 hours, and react at room temperature for 6 hours, pour the above reaction solution Put it into cold water to make it precipitate, wash and filter the precipitate with boiled deionized water, remove water-soluble impurities such as p-fluorobenzoic acid and inorganic salts attached to the monomer, and reflux in methanol for 0.5 hours to further remove p-fluorobenzoic acid , filtered and recrystallized by pyridine to obtain 60.5 g of N,N'-bis(p-fluorobenzoyl)-p-diphenylsulfone diamine with a yield of 82% and a purity of 99.1%.

[0039] Add 1g of lithium chloride, 2g of ε-aminocaproic acid, 1g of potassi...

Embodiment 2

[0040] Embodiment 2, with 37.2g 3,3'-diaminodiphenyl sulfone, 30g triethylamine and 200ml tetrahydrofuran, add successively in the reactor that has stirrer, thermometer, dropping funnel, add paraffin in the dropping funnel 55g of fluorobenzoyl chloride, when the temperature drops to -5°C, start to add p-fluorobenzoyl chloride dropwise, finish adding it within 1 hour, keep it for 3 hours, then react at room temperature for 6 hours, and reduce the above reaction solution to Press and filter, wash and filter the precipitate with boiled deionized water to remove water-soluble impurities such as p-fluorobenzoic acid and inorganic salts attached to the monomer, reflux in methanol for 1 hour to further remove p-fluorobenzoic acid, and filter to obtain 60 g of N,N'-bis(p-fluorobenzoyl)-m-diphenylsulfone diamine was recrystallized from acetone, the yield was 81%, and the purity was 99.3%.

[0041] Add 5g of sodium acetate, 8g of ε-aminocaproic acid, 2g of sodium carbonate, 100g of N-me...

Embodiment 3

[0042]Example 3, add 16.2g m-phenylenediamine, 25g triethylamine and 200ml tetrahydrofuran into the reaction kettle with stirrer, thermometer and dropping funnel in turn, add 47.5g p-fluorobenzoyl chloride to the dropping funnel , when the temperature drops to -5°C, start to add p-fluorobenzoyl chloride dropwise, finish the addition within 1 hour, keep it for 3 hours, and react at room temperature for 6 hours, pour the above reaction solution into cold water to make it Precipitation, the precipitation is washed and filtered with boiling deionized water to remove water-soluble impurities such as p-fluorobenzoic acid and inorganic salts attached to the monomer, recrystallized from methanol, and filtered to obtain N,N'-bis(p-fluorobenzoyl )-m-phenylenediamine 47g, the yield is 89%, and the purity is 99.3%.

[0043] Add 1g of trisodium phosphate, 2g of triphenylphosphine, 0.1g of potassium hydroxide, 300g of N-methylpyrrolidone and 10g of xylene into the reaction kettle with nitro...

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Abstract

The invention discloses a polythiamide amides polymerized substance and a process for preparation, which is characterized in that the process comprises adding 1-5 parts auxiliary agent, 2-8 parts catalyst, 0.1-6 parts alkali or strong base-weak acid salt, 100-500 parts organic solvent and 5-30 parts entrainer into autoclaves of an in-out pipe with nitrogen gas, a water separater, a stirrer and a thermometer, adding sodium sulfide 13 parts whose content is 60% after being evenly stirred, dewatering for 0.5 to 3 hours in 160-200 DEG C under the protection of nitrogen, adding 35.2 to 49.2 parts dihalogenated aromatic amide when the reaction temperature is lowered to 80-150 DEG C, keeping for 2-10 hours in 160-230 DEG C, pouring reaction liquid into water, separating out polymers, purifying with deionized water and acetone after washing and drying, at last obtaining high molecular weight polythiamide amides polymerized substance after drying for 24 hours in 120 DEGC in 0.09 MPa vacuum degree. The inherent viscosity eta=0.1-0.86( the density is 0.1g / dL, and the measuring temperature is 30+-0.1 DEG C), the glass transition temperature Tg is 150-300 DEG C, the initial heat decomposition temperature Td is 440-480 DEG C.

Description

technical field [0001] The invention relates to a polyarylene sulfide amide polymer and a preparation method thereof, belonging to the field of polymer synthesis. Background technique [0002] Both polyarylene sulfide and polyamide are special engineering plastics with excellent performance. They both have good mechanical properties and thermal properties. In order to combine the advantages of the two polymers, the glass transition temperature and melting point of polyarylene sulfide can be increased to improve its toughness. ; Improve the corrosion resistance of polyamide and give it flame retardancy. [0003] People such as Wu Qixian had initially studied the synthesis of novel polyarylene sulfide amide resin in the 1990s, but the resin molecular weight obtained was very low and had no practical value; European Patent EP0162606A1 reported the synthesis of polyarylene sulfide amide with p-aminothiophenol, The p-aminothiophenol used is highly toxic, pollutes the environment...

Claims

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Application Information

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IPC IPC(8): C08G75/02C08G75/0227C08G75/024C08G75/0254C08G75/30
Inventor 杨杰张刚龙盛如王孝军刘静陈永荣
Owner SICHUAN UNIV
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