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DOPO and crosslinked alkenyl polyaryletherketone containing cable material and preparation method thereof

A technology of alkenyl polyarylether ketone and alkenyl polyarylether is applied in the field of preparation containing DOPO and cross-linked alkenyl polyarylether ketone, which can solve the problem of many additives, complex preparation process requirements, and reduced ultra-thin-wall insulation Cable reliability and other issues, to achieve the effect of long-lasting flame retardant performance, good stability, high glass transition temperature

Active Publication Date: 2019-06-28
QUANGANG PETROCHEM RES INST OF FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is difficult to form a uniform blend between the above polymers, and the requirements for the preparation process are relatively complicated, and more additives are added, which reduces the reliability of ultra-thin-wall insulated cables

Method used

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  • DOPO and crosslinked alkenyl polyaryletherketone containing cable material and preparation method thereof
  • DOPO and crosslinked alkenyl polyaryletherketone containing cable material and preparation method thereof
  • DOPO and crosslinked alkenyl polyaryletherketone containing cable material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of bisphenol monomer (I) containing DOPO substituent: add 6.1060g of p-hydroxybenzaldehyde, 4.9565g of 4,4'-diaminodiphenylmethane and 90mL of ethyl acetate into a single-necked bottle, stir well, React at 40°C for 2 hours in a nitrogen atmosphere, then add 10.8085g DOPO to continue the reaction for 24 hours to terminate the reaction. The reaction solution was cooled to room temperature, filtered to obtain a solid, soaked in ethanol, rinsed, filtered, and vacuum-dried at 60°C for 24 hours to obtain a DOPO-substituted bisphenol monomer (I).

[0028]

[0029] (2) Synthesis of DOPO-containing and cross-linked alkenyl polyaryletherketone: 1.6777g (2mmol) of bisphenol monomer containing DOPO substituent (I) and 6.0521g (18mmol) of hexafluorobisphenol A were sequentially added to a three-necked flask , difluorobenzophenone 4.3640g (20mmol), toluene 80mL, DMAc100mL, at 1mL / sec N 2Flow down to 140°C for 3 hours, then raise the temperature to 170°C for 8 hour...

Embodiment 2

[0033] (1) Preparation of bisphenol monomer (II) containing DOPO substituent: add 6.1060g of p-hydroxybenzaldehyde, 2.7035g of p-phenylenediamine and 90mL of absolute ethanol into a one-mouth bottle, stir evenly, and place the mixture in a nitrogen atmosphere at 40°C React for 2h, then add 10.8085gDOPO to continue the reaction for 24h, and terminate the reaction. The reaction solution was cooled to room temperature, filtered to obtain a solid, soaked in ethanol, rinsed, filtered, and vacuum-dried at 60°C for 24 hours to obtain a DOPO-substituted bisphenol monomer (II).

[0034] (2) Synthesis of DOPO-containing and cross-linked alkenyl polyaryletherketone: 3.7438g (5mmol) of DOPO-containing bisphenol (II), 5.0434g (15mmol) of hexafluorobisphenol A, 5.0434g (15mmol) of hexafluorobisphenol A, difluoro Benzophenone 4.3640g (20mmol), toluene 80mL, DMAc100mL, in 1mL / sec N 2 Flow down to 140°C for 3 hours, then raise the temperature to 170°C for 7 hours, stop heating and naturally c...

Embodiment 3

[0037] (1) Preparation of bisphenol monomer (Ⅲ) containing DOPO substituent: add 6.1060g of p-hydroxybenzaldehyde, 5.0060g of 4,4'-diaminodiphenyl ether and 100mL of ethyl acetate into a one-mouth bottle, stir well, and nitrogen React at 50°C for 2 hours in the atmosphere, then add 10.8085g DOPO to continue the reaction for 24 hours, and terminate the reaction. The reaction solution was cooled to room temperature, filtered to obtain a solid, soaked in ethanol, rinsed, filtered, and vacuum-dried at 60°C for 24 hours to obtain a DOPO-substituted bisphenol monomer (Ⅲ).

[0038] (2) Synthesis of DOPO-containing and cross-linked alkenyl polyaryletherketone: 8.4082g (10mmol) of DOPO-containing bisphenol (Ⅲ), 3.3623g (10mmol) of hexafluorobisphenol A, difluorobisphenol A Benzophenone 4.3640g (20mmol), toluene 100mL, DMAc120mL, in 1mL / sec N 2 Flow down to 140°C for 3 hours, then raise the temperature to 170°C for 15 hours, stop heating and naturally cool down to 80°C, then add 0.3022...

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Abstract

The invention discloses a DOPO and crosslinked alkenyl polyaryletherketone-containing cable material and a preparation method thereof. The method comprises the following steps: putting a dual-component bisphenol monomer, difluorobenzophenone and K2CO3 or Na2CO3 in a molar ratio of 1:1:(1.2-3) in a solvent, reacting at 130-150 DEG C for 1-5 hours under the effect of N2 flow; reacting at 150-170 DEGC for 1-10 hours, stopping heating, and naturally cooling to 80 DEG C; and adding alkenyl-containing bisphenol and alkenyl polyaryletherketone in equal molar ratio, uniformly stirring under the effect of N2 flow, heating to 150-160 DEG C, reacting for 3-20 hours, and synthesizing the cable material containing DOPO and alkenyl polyaryletherketone. The method is simple and feasible, salt is formedwith weak base in a polymerization reaction to synthesize the DOPO and crosslinked alkenyl polyaryletherketone-containing cable material. The polymer has good thermal stability, has DOPO flame retardant performance and alkenyl high-temperature crosslinking to improve the environment stress cracking resistance and abrasion resistance, and enables resin to achieve an excellent flame retarding effectwhen being used in polyarylether ketone, polyether sulphone and other resin.

Description

technical field [0001] The invention relates to a cable material containing DOPO and cross-linked alkenyl polyaryl ether ketone, in particular to a preparation method containing DOPO and cross-linked alkenyl polyarylether ketone. Background technique [0002] As power cables are widely used, different environments have different requirements, such as high temperature resistance, low temperature resistance, oil resistance, tear resistance, flame retardancy, etc. Especially in the case of special use conditions and complex application environments, the demand for special cables is becoming more and more prominent, and higher requirements are put forward for the reliability and durability of cables. my country's high-speed railway and urban rail transit equipment are developing rapidly, and the requirements of manufacturing companies for cables used in high-speed rail and urban rail equipment are developing in the direction of ultra-thin wall, high temperature resistance, high ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/40C07F9/6574
Inventor 黄雪红丁富传凌启淡刘金玲陈登龙
Owner QUANGANG PETROCHEM RES INST OF FUJIAN NORMAL UNIV
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