Organic phosphonate nitrogen fire retardant dibenzyl phosphinous-N-cage phosphate amine compound, and preparation method thereof

A technology of caged phosphate amine and diphenylphosphinate is applied in the field involving a diphenylphosphinate-N-1-oxo-1, and achieves high decomposition temperature, low equipment investment, and phosphorus content. high effect

Inactive Publication Date: 2019-01-11
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, although flame retardant technology has been developed rapidly, flame retardants are very rich in both varieties ...

Method used

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  • Organic phosphonate nitrogen fire retardant dibenzyl phosphinous-N-cage phosphate amine compound, and preparation method thereof
  • Organic phosphonate nitrogen fire retardant dibenzyl phosphinous-N-cage phosphate amine compound, and preparation method thereof
  • Organic phosphonate nitrogen fire retardant dibenzyl phosphinous-N-cage phosphate amine compound, and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Example 1 In a 250ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel, and a high-efficiency reflux condenser connected to a drying tube, add 100ml of dichloroethane, 6.60g of caged phosphate amine and 4.05g of triethylamine Amine, use nitrogen to drive out the air in the bottle, start to drop 8.83g of diphenylphosphine chloride at 20°C, and control the reaction temperature at a rate of drop to not exceed 50°C. Then cool to 20°C, filter, wash with water, and dry in vacuo to obtain diphenylphosphinoyl-N-caged phosphate amine as a light yellow solid. The yield was 86.7%. The decomposition temperature is 292±5°C.

Embodiment 2

[0026] Example 2 In a 250ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel, and a high-efficiency reflux condenser connected to a drying tube, add 80ml of dioxane, 6.60g of caged phosphate amine and 4.05g of triethylamine For amine, use nitrogen to drive out the air in the bottle, start to drop 8.83g of diphenylphosphine chloride at 20°C, and control the reaction temperature at a rate of addition not to exceed 50°C. Then it was cooled to 20° C., filtered, washed with water, and dried in vacuo to obtain a light yellow solid diphenylphosphono-N-cage phosphate amine. The yield was 88.5%. The decomposition temperature is 292±5°C.

Embodiment 3

[0027] Example 3 In a 250ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel, and a high-efficiency reflux condenser connected to a drying tube, add 90ml of diethylene glycol dimethyl ether, 6.60g of caged phosphate amine and 4.05 g triethylamine, use nitrogen to drive out the air in the bottle, start to add 8.83g diphenylphosphine chloride dropwise at 20°C, control the reaction temperature at a rate not exceeding 50°C, and raise the temperature to 100°C to reflux after the addition is completed React for 5 hours, then cool to 20°C, filter, wash with water, and dry in vacuo to obtain diphenylphosphono-N-caged phosphate amine as a light yellow solid. The yield was 89.5%. The decomposition temperature is 292±5°C.

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Abstract

The invention relates to an organic phosphonate nitrogen fire retardant dibenzyl phosphinous-N-cage phosphate amine compound, and a preparation method thereof. The structure of the organic phosphonatenitrogen fire retardant dibenzyl phosphinous-N-cage phosphate amine compound is disclosed in the invention. The preparation method comprises following steps: a cage phosphate amine and triethylamineare added into an organic solvent, the air in a reactor is replaced by nitrogen gas, at 20 DEG C, dibenzyl phosphonium chloride is added drop by drop in 1h, wherein the dibenzyl phosphonium chloride:cage phosphate amine :triethylamine molar ratio is controlled to be 1:1:1 to 1:1.2:1, and the dropwise adding temperature is controlled to be 50 DEG C or lower; after dropwise adding, the temperatureis increased to 80 to 110 DEG C for 4 to 6h of backflow reaction, then an obtained product is subjected to cooling, filtering, water washing, and vacuum drying so as to obtain the slightly yellow solid dibenzyl phosphinous-N-cage phosphate amine. The dibenzyl phosphinous-N-cage phosphate amine is an excellent phosphonate nitrogen cooperative fire retardant, and is suitable to be taken as fire retardants of polyamide, polyester, polyurethane, glass fiber reinforced plastic, and polyolefin materials; the preparation method is simple; equipment investment is low; and industrialized production isconvenient to realize.

Description

technical field [0001] The invention relates to an organic phosphine nitrogen flame retardant diphenylphosphono-N-caged phosphate amine compound and a preparation method thereof, in particular to a diphenylphosphono-N-1-oxygen-1- Phospha-2,6,7-trioxa-octyl <4> compound and preparation method thereof, the compound is suitable for use as polyamide, polyester, polyurethane, epoxy resin, unsaturated resin, polyolefin and other materials flame retardant. Background technique [0002] With the continuous progress of social economy and the development of flame retardant technology, flame retardants and flame retardant polymer materials have played an important role in preventing and reducing fires. With the continuous improvement of people's living standards, the demand for high-performance flame-retardant materials is also increasing. At present, although the flame retardant technology has been developed rapidly, the flame retardants are very rich in both varieties and qua...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08K5/5399C08K5/3492C08L67/02
CPCC07F9/65748C08K5/34924C08K5/5399C08L2201/02C08L67/02
Inventor 张刚沈敏杰魏怀鑫王彦林
Owner SUZHOU UNIV OF SCI & TECH
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