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Phosphorus/silicon-containing reactive high-molecular flame retardant, and preparation method and application thereof

A flame retardant and reactive technology, applied in the field of phosphorus-containing silicon reactive macromolecular flame retardants and their preparation, can solve the problems of affecting the mechanical properties of materials, poor compatibility, etc., and achieve the goal of increasing stability and eliminating mechanical properties. Impact, high-yield effects

Active Publication Date: 2015-01-07
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the flame retardant does not have active groups, it is an additive flame retardant, which has poor compatibility with the epoxy resin matrix and affects the mechanical properties of the material.
At present, there are few reports on phosphorus-containing silicon and reactive macromolecular flame retardants

Method used

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  • Phosphorus/silicon-containing reactive high-molecular flame retardant, and preparation method and application thereof
  • Phosphorus/silicon-containing reactive high-molecular flame retardant, and preparation method and application thereof
  • Phosphorus/silicon-containing reactive high-molecular flame retardant, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Synthesis of 4-methacrylamidoaniline

[0033] Dissolve 21.6g of p-phenylenediamine and 20.2g of triethylamine in 200mL of dichloromethane, slowly add 20.9g of methacryloyl chloride dropwise under stirring at 5°C, and continue the reaction for 20h after the dropwise addition; the reaction is over Afterwards, triethylamine hydrochloride was removed by filtration, and washed several times with 3% NaOH solution, distilled water, and saturated NaCl aqueous solution successively. Anhydrous MgSO for organic layer 4 Without drying, 4-methacrylamidoaniline was obtained by rotary evaporation and drying.

[0034] (2) Synthesis of phosphorus-containing monomers

[0035] Dissolve 21.6g of DOPO, 10.1g of triethylamine and 15.4g of carbon tetrachloride in 200mL of dichloromethane, slowly add 13.0g of hydroxyethyl methacrylate under stirring conditions, and react at 20°C for 8h after the dropwise addition is completed, then Suction filtration under reduced pressure to remove tri...

Embodiment 2～5

[0041] Step (1) and step (2) are the same as embodiment 1. Change the ratio of the amount of material of 4-methacrylamidoaniline, MAiBuPOSS and phosphorus-containing monomer in the step (3) (recorded as x: y: z) and step (4) epoxy resin and phosphorus-containing The mass ratio of silicon-reactive macromolecular flame retardants can obtain epoxy resins with different flame retardant properties.

[0042] Table 1

[0043] Example

[0044] Table 1 gives the results of epoxy resins with different flame retardant properties.

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Abstract

The invention provides a phosphorus / silicon-containing reactive high-molecular flame retardant, and a preparation method and application thereof, relating to flame retardants. The preparation method comprises the following steps: reacting methacryloyl chloride and p-phenylenediamine in the presence of a solvent and an acid-binding agent, carrying out vacuum filtration to remove the acid-binding agent salt generated by the reaction, and purifying the crude product by water washing, rotary evaporation and drying to obtain 4-methacrylamidoaniline; reacting hydroxyethyl methacrylate and 9,10-dihydro-9-oxa-10-phosphaphenanthryl-10-oxide in the presence of carbon tetrachloride, a solvent and an acid-binding agent, carrying out vacuum filtration to remove the acid-binding agent salt generated by the reaction, and purifying the crude product by water washing, rotary evaporation and drying to obtain a phosphorus-containing monomer; and carrying out free-radical polymerization on the 4-methacrylamidoaniline, phosphorus-containing monomer and methylacryloyloxypropyl heptaisobutyl POSS (polyhedral oligomeric silsesquioxane) under the initiation conditions of a solvent and an initiator to obtain the phosphorus / silicon-containing reactive high-molecular flame retardant. The phosphorus / silicon-containing reactive high-molecular flame retardant can be used for preparing a flame-retardant epoxy resin.

Description

technical field [0001] The invention relates to a flame retardant, in particular to a phosphorus-containing silicon reactive macromolecule flame retardant and a preparation method and application thereof. Background technique [0002] Due to its excellent physical and mechanical properties, electrical insulation properties, chemical stability and bonding properties, epoxy resin is widely used in aerospace, weapons, shipbuilding and other fields, and is an indispensable and important material in the development of the national economy. However, the oxygen index of epoxy resin is 19.8, which is a flammable material, which can burn in the air after ignition, and the burning speed is relatively fast. Therefore, the development of epoxy resins with good flame retardancy and high thermal stability has become an urgent problem in the field of epoxy resins at home and abroad. [0003] Among the existing flame retardants, the traditional halogenated flame retardants have the advanta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F230/02C08F230/08C08F220/60C08L63/00C08L43/02
Inventor 戴李宗陈国荣袁丛辉刘诚陈显明李远源项佳懿罗伟昂何凯斌曾碧榕
Owner XIAMEN UNIV
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