Preparation method of poly(ether-ether-ketone) resin containing ferrocene/DOPO group and crosslinked alkenyl

A technology of alkenyl polyether and ferrocene is applied in the field of preparation of resin containing ferrocene/DOPO group and cross-linked alkenyl polyether ether ketone, which can solve the problem of many additives, reducing cable reliability and increasing product cost etc., to achieve the effect of high glass transition temperature

Inactive Publication Date: 2019-06-07
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 undoubtedly increases the product cost and reduces the reliability of the cable.

Method used

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  • Preparation method of poly(ether-ether-ketone) resin containing ferrocene/DOPO group and crosslinked alkenyl
  • Preparation method of poly(ether-ether-ketone) resin containing ferrocene/DOPO group and crosslinked alkenyl
  • Preparation method of poly(ether-ether-ketone) resin containing ferrocene/DOPO group and crosslinked alkenyl

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Synthesis of ferrocene and DOPO-based bisphenol monomers: 6.4854 g of DOPO-based bisphenol (I), 2.7405 g of 1,1'-ferrocenedicarboxylic acid, and 4-bisphenol Add 2.4534g of methylaminopyridine and 140mL of dichloromethane, put it into an ice bath and stir and fill with N 2 After 30 minutes, dissolve 4.166g of N,N'-dicyclohexylcarboimide in 20mL of dichloromethane, add dropwise to the above solution within 60 minutes, naturally warm to room temperature under stirring and continue to react for 24 hours, and concentrate the reaction solution , cooling, filtering, washing, and drying, and drying the precipitate in a vacuum oven at 40° C. for 10 h to obtain a product containing ferrocene and DOPO-based bisphenol (M1) monomer.

[0041] (2) Synthesis of polyether ether ketone containing ferrocene, DOPO group and cross-linked alkenyl group: In a three-necked flask, 1.1186 g (2 mmol) of bisphenol (M1) containing ferrocene and DOPO group, and 3.6512 bisphenol A g (16mmol), 3....

Embodiment 2

[0046] (1) Synthesis of monomers containing ferrocene and DOPO-based bisphenol (M2): Add 7.4840 g of DOPO-based bisphenol (II), 2.2261 g of triethylamine and 120 mL of dichloromethane in a three-necked flask, and stir to dissolve Evenly, 2.9305g of 1,1'-ferrocenedicarboxylic acid chloride was dissolved in 20mL of dichloromethane, slowly dripped into the above solution under stirring, reacted at room temperature for 24h, raised the temperature to 42-45°C, reacted for 8h, and evaporated the solvent , cooled, filtered, washed and dried, and the precipitate was dried in a vacuum oven at 40° C. for 10 h to obtain a product containing ferrocene and DOPO-based bisphenol (M2) monomer.

[0047] (2) Synthesis of polyether ether ketone containing ferrocene, DOPO group and cross-linked alkenyl: In a three-necked flask, 2.4493 g (4 mmol) of bisphenol (M2) containing ferrocene and DOPO group, hydroquinone 1.6515g (15mmol), 4.1458g (19mmol) of difluorobenzophenone, 4.1463g (30mmol) of anhydr...

Embodiment 3

[0050] (1) Synthesis of bisphenol containing ferrocene and DOPO-based monomers: Add 6.4854 g of DOPO-based bisphenol (I), 2.2261 g of triethylamine and 120 mL of dichloromethane in a three-necked flask, stir and dissolve evenly, 2.9305 Dissolve g1,1'-ferrocenedicarboxylic acid chloride in 20mL of dichloromethane, slowly drop into the above solution under stirring, react at room temperature for 24h, raise the temperature to 42-45°C, react for 8h, evaporate the solvent, cool and filter , washing and drying to obtain a product containing ferrocene and DOPO-based bisphenol (M1) monomers.

[0051] (2) Synthesis of polyetheretherketone containing ferrocene, DOPO group and crosslinked alkenyl group: 5.5929g (10mmol) of bisphenol (M1) containing ferrocene and DOPO group, hexafluorobisphenol A3.3623g (10mmol), difluorobenzophenone 4.3640g (20mmol), anhydrous potassium carbonate 6.2195g (45mmol), toluene 80mL, DMAc100mL, in 1mL / sec N 2 React at 140°C for 3 hours, then raise the tempera...

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Abstract

The invention relates to a preparation method of a poly(ether-ether-ketone) resin containing a ferrocene / DOPO group and crosslinked alkenyl. The preparation method comprises following steps: adding acompound liquid containing ferrocene, difluorobenzophenone (DFBP), and a catalyst (I) into an organic solvent (I) according to a certain mole ratio, carrying out secondary reactions under the action of N2 flow; then adding a mixed solution of allyl containing bisphenol and DFBP, raising the temperature to carry out reactions, pouring the reaction liquid into water, carrying out precipitation, filtering, and drying to obtain the poly(ether-ether-ketone) resin. A bisphenol unit containing ferrocene and a DOPO group into the poly(ether-ether-ketone) resin to overcome the problems that the productof industrial NaOH salt forming reactions can be degraded easily, the reactions are difficult to control, and alkali pollution happens. An allyl bisphenol monomer is introduced into the resin to avoid crosslinking reactions of double bonds after long time high temperature reactions. A new approach and a new method are provided for obtaining a flame retardant resin system having a strong flame retardant performance and excellent properties.

Description

technical field [0001] The invention relates to the technical field of preparation of crosslinked alkenyl polyether ether ketone resin, in particular to a preparation method of ferrocene / DOPO group and crosslinked alkenyl polyether ether ketone resin. 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 tempera...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/02
Inventor 黄雪红郑飞江生光丁富传凌启淡
Owner FUJIAN NORMAL UNIV
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