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Preparation method of phosphorus-containing flame retardant containing phosphazene/dopo double base structure

A flame retardant and drying technology, applied in the field of flame retardant epoxy resin, can solve the problems of low flame retardant efficiency, poor compatibility between polymer matrix and flame retardant, etc., achieve high flame retardant efficiency, difficult to migrate, overcome heat The effect of low decomposition temperature

Inactive Publication Date: 2017-07-04
NORTHEAST FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to solve the problems of low flame retardant efficiency and poor compatibility between the polymer matrix and the flame retardant existing in the existing epoxy resin materials, and provides a phosphorus-containing flame retardant with a phosphazene / DOPO double base structure, its preparation method and Flame Retardant Epoxy Resin Using It as Raw Material

Method used

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  • Preparation method of phosphorus-containing flame retardant containing phosphazene/dopo double base structure
  • Preparation method of phosphorus-containing flame retardant containing phosphazene/dopo double base structure
  • Preparation method of phosphorus-containing flame retardant containing phosphazene/dopo double base structure

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specific Embodiment approach 1

[0017] Specific implementation mode 1: The structural formula of the phosphorus-containing flame retardant containing phosphazene / DOPO double base structure in this embodiment is:

[0018]

specific Embodiment approach 2

[0019] Specific implementation mode two: the preparation method of the phosphorus-containing flame retardant containing phosphazene / DOPO double base structure in this embodiment is carried out according to the following steps:

[0020] 1. Install a spherical condenser, a nitrogen protection device, a mechanical stirrer, a constant pressure dropping funnel and a heating device on the four-necked round-bottomed flask, vacuumize the inside of the round-bottomed flask and blow in high-purity nitrogen until the flask reaches zero Oxygen anhydrous condition, then add p-hydroxybenzaldehyde into the flask, then add dried tetrahydrofuran to fully dissolve, then add triethylamine as an acid-binding agent, and stir until the reaction system is clear and transparent;

[0021] 2. Dissolve hexachlorocyclotriphosphazene in dried tetrahydrofuran to obtain solution A, and drop solution A into the continuously stirring reaction system through a constant pressure dropping funnel. The heating rat...

specific Embodiment approach 3

[0027] Embodiment 3: This embodiment is different from Embodiment 2 in that: the purity of the high-purity nitrogen in step 1 is 99.99%. Others are the same as in the second embodiment.

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Abstract

The invention relates to a phosphorus-containing fire retardant, a preparation method of the phosphorus-containing fire retardant and a flame-retardant epoxy resin prepared from the phosphorus-containing fire retardant, and especially relates to a phosphorus-containing nitrile / DOPO double-base structure phosphorus-containing fire retardant, a preparation method of the phosphorus-containing nitrile / DOPO double-base structure phosphorus-containing fire retardant, and flame-retardant epoxy resin prepared from the phosphorus-containing nitrile / DOPO double-base structure phosphorus-containing fire retardant. The flame-retardant epoxy resin solves the problem that the existing epoxy resin has low flame retardation efficiency and poor compatibility between a polymer matrix and a fire retardant. The preparation method comprises the following steps of 1, dissolving p-hydroxybenzaldehyde and tetrahydrofuran, adding triethylamine into the solution and carrying out stirring, 2, dissolving phosphonitrilic chloride trimer in tetrahydrofuran, dropwisely adding the solution into the reaction system, and carrying out heating and stirring, 3, cooling the reaction system, concentrating the filtrate, pouring the filtrate into water for precipitate separation, carrying out pumping filtration, carrying out recrystallization on the precipitates and carrying out drying to obtain intermediates, and 4, dissolving the intermediates by a solvent, adding p-aminophenol into the solution, carrying out heating reflux, adding DOPO into the reflux product, carrying out condensation, pouring the concentrate into cold ethanol for solid precipitation, and washing and drying the solids to obtain the phosphorus-containing nitrile / DOPO double-base structure phosphorus-containing fire retardant. The flame-retardant epoxy resin comprises epoxy resin, a curing agent and the phosphorus-containing nitrile / DOPO double-base structure phosphorus-containing fire retardant. The preparation method is used for preparing the phosphorus-containing nitrile / DOPO double-base structure phosphorus-containing fire retardant.

Description

technical field [0001] The invention relates to a phosphorus-containing flame retardant, a preparation method thereof and a flame-retardant epoxy resin using the phosphorus-containing flame retardant as a raw material. Background technique [0002] Polymer materials have excellent comprehensive properties and are widely used in aerospace, electronic appliances, automobile industry and other fields, but the flammability of polymer materials and the hazards of burning and releasing toxic gases hinder their wider application. Flame retardants are a class of functional additives that can impart flame retardancy to polymer materials. Halogenated flame retardants, especially bromine-containing flame retardants, have been widely used due to their high flame retardant efficiency and low price. However, when halogenated flame retardants are thermally cracked or burned, they will generate a lot of smoke and corrosive toxic gases, such as: polybrominated dibenzofurans, dioxins, etc. Ba...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/5399C07F9/6593C08L63/00
Inventor 李斌徐广锐许苗军
Owner NORTHEAST FORESTRY UNIVERSITY
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