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Preparation method of 9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) side group polyaryletherketone containing ternary flame-retardant material

A technology of polyaryletherketone and flame-retardant materials, which is applied in the field of preparation of DOPO side-group polyaryletherketone containing ternary flame-retardant materials, can solve the problems of material mechanical properties decline and affect flame-retardant performance, and achieve good maintenance, The effect of good electrical insulation, good economic benefits and promotional value

Active Publication Date: 2019-05-07
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the direct addition of DOPO small molecules to the material is often accompanied by a decline in the mechanical properties of the material, and it is easy to migrate out of the polymer material, affecting its flame retardant performance.

Method used

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  • Preparation method of 9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) side group polyaryletherketone containing ternary flame-retardant material
  • Preparation method of 9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) side group polyaryletherketone containing ternary flame-retardant material
  • Preparation method of 9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) side group polyaryletherketone containing ternary flame-retardant material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] One of embodiment 1 p-fluorobenzaldehyde or p-chlorobenzaldehyde and reactant B

[0032] (1) Add p-fluorobenzaldehyde and 2-aminothiazole or p-fluorobenzaldehyde and 2-aminobenzothiazole to absolute ethanol at a molar ratio of 1:1, react at 50°C for 2 hours in a nitrogen atmosphere, and then add Continue to react with DOPO in an equimolar amount of 2-aminothiazole or 2-aminobenzothiazole for 24 hours, terminate the reaction, and obtain DOPO derivatives respectively. The synthetic route is shown in the figure.

[0033]

[0034] (2) Synthesis of polyaryletherketone containing DOPO side groups: In a three-necked flask, add 1.4014g (10mmol) of o-methoxyhydroquinone, 3.3623g (10mmol) of hexafluorobisphenol A, and difluorobiphenyl Methanone 4.3640g (20mmol), anhydrous potassium carbonate 3.3166g (24mmol), toluene 80mL, DMAc100mL, in N 2 React at 140°C for 3h under airflow, then raise the temperature to 170°C for 6h, immediately pour the reaction solution into deionized wa...

Embodiment 2

[0042] In a three-necked flask, add 0.707g (5mmol) of o-methoxyhydroquinone, 5.0434g (15mmol) of hexafluorobisphenol A, 4.3640g (20mmol) of difluorobenzophenone, and 3.3166g of anhydrous potassium carbonate. (24mmol), toluene 80mL, DMAc100mL, in N 2 React at 140°C for 3h under airflow, then raise the temperature to 170°C for 6h, immediately pour the reaction solution into deionized water for precipitation under stirring, and filter. The filtered precipitate was soaked in deionized water, soaked in running water for 24 hours, filtered, and dried in a vacuum oven at 80° C. for 10 hours to obtain methoxy-containing polyaryletherketone. GPC analysis, Mn = 20200, PDI = 1.84.

[0043] Weigh 5.0 g of methoxy-containing polyaryletherketone and dissolve it in 100 mL of dried dichloromethane. N 2 Under gas protection, in an ice-salt bath, 1.5 mL of boron tribromide solution diluted with 15 mL of dichloromethane was added dropwise. After the dropwise addition was completed within 2 ho...

Embodiment 3

[0047] In a three-necked flask, add 0.2803g (2mmol) of o-methoxyhydroquinone, 6.0521g (18mmol) of hexafluorobisphenol A, 4.3640g (20mmol) of difluorobenzophenone, and 3.3166g of anhydrous potassium carbonate. (24mmol), toluene 80mL, DMAc100mL, in N 2 React at 140°C for 3h under airflow, then raise the temperature to 170°C for 6h, immediately pour the reaction solution into deionized water for precipitation under stirring, and filter. The filtered precipitate was soaked in deionized water, soaked in running water for 24 hours, filtered, and dried in a vacuum oven at 80° C. for 10 hours to obtain methoxy-containing polyaryletherketone.

[0048] Weigh 5.0 g of methoxy-containing polyaryletherketone and dissolve it in 100 mL of dried dichloromethane. N 2 Under gas protection, in an ice-salt bath, 0.6 mL of boron tribromide solution diluted with 6 mL of dichloromethane was added dropwise. After the addition was completed within 2 hours, the temperature was naturally raised to roo...

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Abstract

The invention relates to a preparation method of a 9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) side group polyaryletherketone containing a ternary flame-retardant material. The method comprises the following steps: placing multi-component bisphenol, difluorobenzophenone and a catalyst in an organic solvent, carrying out twice temperature-control reactions, then pouring the reaction product into water, carrying out dialysis and vacuum drying on the precipitate to obtain a methoxy substituent group-containing polyaryletherketone base material; dissolving the methoxy substituent group-containing polyaryletherketone in a boron trifluoride solution, filtering the reactant, and carrying out Soxhlet extraction and drying to obtain polyaryletherketone; adding p-fluorobenzaldehyde orp-chlorobenzaldehyde and 2-aminothiazole or 2-aminobenzothiazole into a solvent to carry out a reaction to obtain a 2DOPO group-containing thiazole derivative or DOPO group-containing benzothiazole derivative; and placing hydroxyl substituent group-containing polyaryletherketone, the DOPO side group-containing thiazole derivative and a catalyst in an organic solvent, carrying out a secondary reaction for precipitation, and carrying out dialysis vacuum drying to obtain the DOPO side group-containing polyaryletherketone. The prepared DOPO side group-containing polyaryletherketone with a high molecular weight has excellent comprehensive performance, and requirements of a high-level application can be met.

Description

technical field [0001] The invention relates to the technical field of preparation of polyaryletherketone resin containing DOPO side groups, in particular to a method for preparing DOPO side group polyaryletherketone which is a ternary flame-retardant material containing nitrogen, sulfur and phosphorus. 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 develop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48
Inventor 黄雪红陈宇涵丁富传凌启淡
Owner FUJIAN NORMAL UNIV
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