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Yellowing-resistant antioxidation flame-retardant semi-aromatic polyamide and preparation method thereof

A semi-aromatic polyamide, anti-oxidation technology, applied in the field of semi-aromatic polyamide and its preparation, can solve the problems of anti-oxidation, poor weather resistance, easy yellowing, easy to burn, etc.

Active Publication Date: 2017-09-01
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the resin product obtained by this method has good high temperature resistance, corrosion resistance and heat processability, but due to the high content of aliphatic linear structure in its main molecular chain, its semi-aromatic polyamide copolymer product The anti-oxidation and weather resistance are poor, and it is easy to produce yellowing; in addition, although the semi-aromatic polyamide copolymer product has the characteristics of high temperature resistance, it still has not overcome its flammability defect, so the obtained product is extremely flammable. Its vertical burning UL-94 rating is stepless

Method used

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  • Yellowing-resistant antioxidation flame-retardant semi-aromatic polyamide and preparation method thereof
  • Yellowing-resistant antioxidation flame-retardant semi-aromatic polyamide and preparation method thereof
  • Yellowing-resistant antioxidation flame-retardant semi-aromatic polyamide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] (1) Preparation and purification of thiadiazole dibenzyl sulfide dicarboxylic acid-4,4'-diaminodicyclohexylmethane salt

[0057] Add 418 kg of thiadiazole dibenzyl sulfide dicarboxylic acid, 210 kg of 4,4'-diaminodicyclohexyl methane, and 200 kg of deionized water into a reactor with mechanical stirring and reflux condenser, and react at 50°C for 0.5 h, control the pH of the solution to 6, to obtain the terephthalic acid-4,4'-diaminodicyclohexylmethane salt reaction solution; centrifuge the above reaction solution while it is hot to remove insolubles, and then transport the reaction solution To the cooling crystallization tank, perform natural cooling and crystallization; filter the precipitated thiadiazole dibenzyl sulfide dicarboxylic acid-4,4'-diaminodicyclohexylmethane salt, collect the filter cake, and rinse with a small amount of water Wash, collect the filtrate as the solvent for the next batch of materials, and dry the filter cake at 60°C under a vacuum of 0.08MPa ...

Embodiment 2

[0063] (1) Preparation and purification of 4,4'-diphenylsulfide dicarboxylic acid-4,4'-diaminodicyclohexylmethane salt

[0064] Put 274 kg of 4,4'-diphenyl sulfide dicarboxylic acid, 210 kg of 4,4'-diaminodicyclohexyl methane, and 500 kg of deionized water into a reactor with mechanical stirring and reflux condenser, and react at 100°C 1h, control the pH of the solution to 6.5 to obtain 4,4'-diphenylsulfide dicarboxylic acid-4,4'-diaminodicyclohexylmethane salt reaction solution; centrifuge the above reaction solution while hot to remove Insoluble matter, the reaction liquid is transported to the cooling crystallization tank for natural cooling and crystallization; the precipitated 4,4'-diphenylsulfide dicarboxylic acid-4,4'-diaminodicyclohexylmethane salt is filtered , Collect the filter cake and rinse with a small amount of water. Collect the filtrate as the solvent for the next batch of materials. The filter cake is dried at 80°C under a vacuum of 0.085MPa for 10 hours to obta...

Embodiment 3

[0070] (1) Preparation and purification of 4,4'-diphenylsulfide dicarboxylic acid-3,3'-dimethyl-4,4'-diaminodicyclohexylmethane salt

[0071] Add 274kg of 4,4'-diphenylsulfide dicarboxylic acid, 238kg of 3,3'-dimethyl-4,4'-diaminodicyclohexylmethane, and 2000kg of deionized water into a reflux condenser with mechanical stirring In the reactor, react at 80°C for 3h, and control the pH of the solution to 8 to obtain 4,4'-diphenyl sulfide dicarboxylic acid-3,3'-dimethyl-4,4'-diamino Dicyclohexylmethane salt reaction liquid; the above reaction liquid is centrifuged and filtered while it is hot to remove insoluble materials, and then the reaction liquid is transported to a cooling crystallization tank for natural cooling and crystallization; the precipitated 4,4'-diphenyl sulfide Ether dicarboxylic acid-3,3'-dimethyl-4,4'-diaminodicyclohexylmethane salt was filtered, the filter cake was collected, and rinsed with a small amount of water, and the filtrate was collected as the solvent f...

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Abstract

The invention discloses yellowing-resistant antioxidation flame-retardant semi-aromatic polyamide and a preparation method thereof. Semiaromatic nylon salt, nylon salt, caprolactam, catalysts and deionized water are added into a reaction kettle; nitrogen is introduced for air replacement; heating reaction is performed; the temperature is lowered; soft water is sprayed into the kettle through a spraying opening of the reaction kettle; dilution pulping and filtering are performed on the materials in the reaction kettle; then, solid oligomers are dried, and then the yellowing-resistant antioxidation flame-retardant semi-aromatic polyamide oligomer particle dry bases are obtained; the oligomer particle dry bases are added into a reaction extrusion machine; the screw rod rotating speed, the feeding speed and the temperature of each section of an extruding machine are controlled; exhaust, extrusion, particle cutting and drying are performed; the yellowing-resistant antioxidation flame-retardant semi-aromatic polyamide resin with high molecular weight is obtained. The yellowing-resistant antioxidation flame-retardant semi-aromatic polyamide has the characteristics of high temperature resistance, flame-retardant performance, antioxidation and yellowing resistance. The preparation method also has the advantages of high yield and green and environment-friendly effects.

Description

Technical field [0001] The invention belongs to the technical field of polymer materials and their synthesis, and in particular relates to a semi-aromatic polyamide which is resistant to yellowing, oxidation and flame retardant and a preparation method thereof. Background technique [0002] High temperature resistant nylon is a kind of engineering plastic with excellent performance, with good mechanical and thermal properties, but conventional high temperature resistant nylon such as PA6T not only contains high-density hydrogen bonds, which makes its melting point higher than its thermal decomposition temperature, resulting in It cannot be molded and processed, and it is also a flammable material, which limits its use in certain applications requiring flame retardancy. [0003] In order to improve its molding processability, the prior art is to introduce aliphatic polyamide molecular chain structural units into the high-temperature nylon main chain structure through the method of m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/36
CPCC08G69/36
Inventor 张刚卢杰宏杨杰严光明黄翔张美林王孝军龙盛如
Owner SICHUAN UNIV
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