Method for preparing phenyl hypophosphite flame retardant

A technology of phenyl hypophosphite and flame retardant, which is applied in the field of preparation of phenyl hypophosphite flame retardant, can solve the problems of harsh conditions, cumbersome steps and high cost, and achieves short reaction period, good thermal stability, mild conditions

Active Publication Date: 2013-06-12
PRESAFER QINGYUAN PHOSPHOR CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

EP1969052A1, CN1660857A, CN1660858A, CN1280581A, CN1280582A, etc. have proposed the preparation method and application of dialkyl hypophosphite flame retardants. Dialkyl hypophosphite flame retardants have a good effect in polyester or nylon, but , these preparation processes are complicated, the reaction cycle is long, the conditions are harsh, the steps are cumbersome, and the cost is high. At the same time, the thermal stability is not good, and it cannot meet the high-temperature processing conditions of glass fiber reinforced polyester or nylon.

Method used

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  • Method for preparing phenyl hypophosphite flame retardant

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[0016] A preparation method of phenyl hypophosphite flame retardant, comprising the steps of:

[0017] 1) In the reaction kettle with stirring, reflux device and acid absorption tower, add water at a temperature of 40-100 ° C, start stirring, N 2 protection, then add phenylphosphine dichloride to water within 1 to 6 hours, and keep stirring;

[0018] 2) After adding phenylphosphine dichloride, under stirring, keep the temperature at 40-100°C and keep the reaction for 1-6 hours;

[0019] 3) Cool down to room temperature, adjust the pH of the reaction solution to 6~8 with an alkaline substance, then add an inorganic metal salt within 0.5~3 hours, maintain the reaction for 1~2 hours, then filter and dry to obtain a phenyl hypophosphorous acid Salt flame retardant;

[0020] Among them, the volume of water: the amount of phenylphosphine dichloride: the amount of inorganic metal salt = 1L: (1~7mol): (1~5mol).

[0021] The alkaline substance is at least one of sodium hydroxide, po...

Embodiment 1

[0024] 1) Add 500ml of deionized water at 40~50°C in a 2L reaction kettle with stirring, reflux device and acid absorption tower, start stirring, N 2 Protection, dropwise add 2mol of phenyl phosphorus dichloride in 1~2 hours, and keep stirring;

[0025] 2) After adding phenylphosphine dichloride, under stirring, keep the temperature at 90-100°C and keep the reaction for 1-2 hours;

[0026] 3) Cool down to room temperature, adjust the pH of the reaction solution to 6~8 with 20% NaOH solution, and then add 0.8molAlCl in 0.5~1h 3 Solute, AlCl with a mass fraction of 30% 3 Solution, maintain reaction for 1-2 hours, then filter and dry to obtain a phenyl hypophosphite flame retardant.

Embodiment 2

[0028] 1) In a 5L reaction kettle with stirring, reflux device and acid absorption tower, add 1000ml deionized water at 40~50°C, start stirring, N 2 For protection, 6mol of phenylphosphorous dichloride was added dropwise within 3 to 4 hours;

[0029] 2) After adding phenylphosphine dichloride, under stirring, keep the temperature at 90-100°C and keep the reaction for 3-5 hours;

[0030] 3) Cool down to room temperature, adjust the pH of the reaction solution to 6~8 with 20% KOH solution, and then add 2mol solute with a mass fraction of 30% AlCl within 0.5~1h 3 Solution, maintain reaction for 1-2 hours, then filter and dry to obtain a phenyl hypophosphite flame retardant.

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Abstract

The invention discloses a method for preparing a phenyl hypophosphite flame retardant, which comprises the following steps of: adding dichlorophenylphosphine into water at the temperature of between 40 and 100 DEG C within 1 to 6 hours in a reaction kettle with a stirring and refluxing device, and continuously stirring; keeping the temperature to be between 40 and 100 DEG C, and maintaining reaction for 1 to 6 hours; and reducing the temperature to room temperature, regulating the pH of reaction liquid to be between 6 and 8 by using an alkaline material, adding metal salt within 0.5 to 3 hours, maintaining reaction for 1 to 2 hours, filtering, and drying to obtain the phenyl hypophosphite flame retardant, wherein the molar ratio of the water to the dichlorophenylphosphine to the metal salt is 1L:(1-7mol):(1-5mol). Phenyl hypophosphite is prepared from a simple raw material, an intermediate product is not required to be separated, the method is simple, the reaction period is short, conditions are mild, cost is low, and the obtained product has high heat stability.

Description

technical field [0001] The invention relates to a preparation method of a phenyl hypophosphite flame retardant. Background technique [0002] Flame retardants can be roughly divided into additive flame retardants and reactive flame retardants. Additive flame retardants roughly include inorganic metal compound flame retardants, such as Al(OH) 3 , Mg(OH) 2 etc.; halogen flame retardants, such as decabromodiphenyl ether, octabromoether, etc.; phosphorus flame retardants, such as triphenyl phosphate, red phosphorus microcapsules, etc., nitrogen flame retardants, such as melamine, melamine Reactive flame retardants are generally organic halides or organic phosphorus monomers containing reactive groups. [0003] Inorganic metal flame retardants will greatly damage the mechanical properties of the matrix material; halogenated flame retardants will pollute the environment during combustion, and when materials containing halogenated flame retardants are discarded into the environme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/30C08K5/5313C08L67/00C08L77/00C08K7/14
Inventor 张秀芹周侃陈敏聪
Owner PRESAFER QINGYUAN PHOSPHOR CHEM
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