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Fire retardant phosphinous-(N, N', N''-tri-cage phosphate) triamine compound, and preparation method thereof

A technology of flame retardant phosphorous acid and tricage phosphate, which is applied in the field of N, can solve problems such as restrictions on the use of halogenated flame retardants, and achieve good phosphorus and nitrogen synergistic flame retardant effects, high phosphorus content, and good compatibility sexual effect

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

AI Technical Summary

Problems solved by technology

However, since the European Union promulgated the RoHS directive in 1986, the use of halogenated flame retardants has been subject to certain restrictions.

Method used

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  • Fire retardant phosphinous-(N, N', N''-tri-cage phosphate) triamine compound, and preparation method thereof
  • Fire retardant phosphinous-(N, N', N''-tri-cage phosphate) triamine compound, and preparation method thereof
  • Fire retardant phosphinous-(N, N', N''-tri-cage phosphate) triamine compound, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1 In a 250ml four-neck flask equipped with a stirring device, dropping funnel, thermometer, and a high-efficiency reflux condenser connected to a drying tube, add 100ml of tetrachloroethane, 4.95g of caged phosphate amine and 3.03g of triethylamine , use nitrogen to drive out the air in the bottle, add 1.38g of phosphorus trichloride dropwise into the four-necked bottle at 10°C for about 1 hour, control the reaction temperature at 10°C-20°C, and raise the temperature to 100°C after the dropwise addition Insulated for 3 hours, then cooled, filtered, and vacuum-dried to obtain a solid mixture of a yellow product and triethylamine hydrochloride. The solid mixture was dissolved with 60ml of dimethyl sulfoxide, filtered, and the filtrate was evaporated to dryness to obtain the target product phosphorous acid-(N, N', N"-three cage phosphate) triamine, the yield was 89.4%, and the decomposition temperature was 261°C .

Embodiment 2

[0028] Example 2 In a 250ml four-neck flask equipped with a stirring device, dropping funnel, thermometer, and high-efficiency reflux condenser connected to a drying tube, add 80ml of dioxane, 4.95g of caged phosphate amine and 3.03g of triethylamine , use nitrogen to drive out the air in the bottle, and drop 1.38g of phosphorus trichloride into the four-necked bottle at 10°C for about 1 hour, control the reaction temperature at 10°C-20°C, and raise the temperature to 90°C after the addition is completed Insulated for 3 hours, then cooled, filtered, and vacuum-dried to obtain a solid mixture of a yellow product and triethylamine hydrochloride. The solid mixture was dissolved with 70ml of dimethyl sulfoxide, filtered, and the filtrate was evaporated to dryness to obtain the target product phosphorous acid-(N, N', N"-three cage phosphate) triamine, the yield was 90.1%, and the decomposition temperature was 261°C .

Embodiment 3

[0029] Example 3 In a 250ml four-neck flask with a stirring device, dropping funnel, thermometer, and high-efficiency reflux condenser connected to a drying tube, add 80ml of acetonitrile, 4.95g of caged phosphate amine and 3.03g of triethylamine, and use nitrogen Drive out the air in the bottle, add 1.38g of phosphorus trichloride dropwise into the four-necked bottle at 10°C for about 1 hour, control the reaction temperature at 10°C-20°C, and raise the temperature to 80°C for 4 hours after the dropwise addition , then cooled, filtered, and vacuum-dried to obtain a solid mixture of a yellow product and triethylamine hydrochloride. The solid mixture was dissolved with 80ml of dimethyl sulfoxide, filtered, and the filtrate was evaporated to dryness to obtain the target product phosphorous acid-(N, N', N"-three cage phosphate) triamine, the yield was 91.0%, and the decomposition temperature was 261°C .

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Abstract

The invention relates to a fire retardant phosphinous-(N, N', N''-tri-cage phosphate) triamine compound, and a preparation method thereof. The structure of the fire retardant phosphinous-(N, N', N''-tri-cage phosphate) triamine compound is disclosed in the invention. The preparation method comprises following steps: a cage phosphate amine and triethylamine are added into an organic solvent, cooling is carried out until the temperature is reduced to 10 DEG C, phosphorus trichloride is added drop by drop, the dropswise adding temerpature is controlled to be 10 to 20 DEG C, after dropwise adding,the temerpature is increased to 70 to 100 DEG C, thermal insulation reaction is carried out for 3 to 5h, an obtained product is cooled and filtered, and is subjected to vacuum drying so as to obtaina solid mixture of a yellow target product and a triethylamine hydrochloride; the solid mixture is dissolved with dimethyl sulphoxide, and filtering and filtrate evaporation are carried out so as to obtain the target product phosphinous-(N, N', N''-tri-cage phosphate) triamine. The phosphinous-(N, N', N''-tri-cage phosphate) triamine compound 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 is convenient to realize.

Description

technical field [0001] The invention relates to a preparation method of an organic phosphine nitrogen flame retardant phosphorous acid-(N, N', N"-tricage phosphate) triamine compound, in particular to a N, N', N"-tri( 1-oxo-1-phospha-2,6,7-trioxa-octyl <4>) phosphoramidite compound and preparation method thereof, the compound is suitable for polyester, polyurethane, epoxy resin, unsaturated Flame retardant for resin, polyvinyl chloride and other materials. Background technique [0002] In recent years, due to the continuous development of the economy, flammable polymer materials have been widely used, so the flame retardant technology has also developed rapidly. Currently widely used flame retardants include halogen-based, phosphorus-based and inorganic flame retardants. Halogenated flame retardants have been a popular product in the field of flame retardants since the 1960s. This type of flame retardant has high flame retardant efficiency, has little impact on the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08K5/5399
CPCC07F9/65748C08K5/5399
Inventor 魏怀鑫沈敏杰王彦林
Owner SUZHOU UNIV OF SCI & TECH
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