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Flame retardant thiophosphoryl-(N,N',N'-tricaged phosphate) triamine compound and preparation method thereof

The technology of flame retardant thiophosphoryl and caged phosphate ester amine is applied in the field of flame retardant thiophosphoryl-triamine compound and its preparation, and can solve the problems of toxicity, limitation on the use of halogen-based flame retardants, and the like. Achieve low cost, good compatibility and flame retardant effect, good symmetry of cage ring structure

Pending Publication Date: 2019-01-18
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Halogenated flame retardants have been widely used since the 1960s, and their application technology is relatively mature. However, due to the toxicity of burning, since the European Union promulgated the RoHS directive in 1986, the use of halogenated flame retardants in some some areas are restricted

Method used

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  • Flame retardant thiophosphoryl-(N,N',N'-tricaged phosphate) triamine compound and preparation method thereof
  • Flame retardant thiophosphoryl-(N,N',N'-tricaged phosphate) triamine compound and preparation method thereof
  • Flame retardant thiophosphoryl-(N,N',N'-tricaged phosphate) triamine compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Example 1 In a 250ml four-neck flask with a stirrer, a thermometer, a dropping funnel, and a 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 1.70g of phosphorous trichloride dropwise to the reaction bottle within 1 hour at 10°C, control the dropping temperature at 10°C to 20°C, after the dropwise addition, raise the temperature to 80°C for heat preservation reaction 3h, then cooled to 20°C, filtered, and dried in vacuo to obtain a solid mixture of yellow product and triethylamine hydrochloride. The solid mixture is dissolved with 60ml dimethylsulfoxide, filters, and the filtrate is evaporated to dryness to obtain the product phosphorothioate-(N, N', N "-tricage phosphoric acid ester) triamine. The productive rate is 87.3%, and the decomposition temperature is 264°C.

Embodiment 2

[0029] Example 2 In a 250ml four-neck flask with a stirrer, a thermometer, a dropping funnel, and a high-efficiency reflux condenser connected to a drying tube, add 90ml of dioxane, 4.95g of caged phosphate amine and 3.03g of triethylamine , use nitrogen to drive out the air in the bottle, and under the condition of 10°C, add 1.70g of phosphorus trichloride dropwise into the reaction bottle within 1h, control the dropping temperature at 10°C-20°C, after the dropwise addition, raise the temperature to 90 ℃ for 3 hours, then cooled to 20 ℃, filtered, and vacuum-dried to obtain a solid mixture of yellow product and triethylamine hydrochloride. Solid mixture is dissolved with 70ml dimethyl sulfoxide, filters, and the filtrate is evaporated to dryness to obtain product phosphorothioate-(N, N ', N "-three caged phosphoric acid ester) triamine. Productive rate is 90.1%, and decomposition temperature is 264°C.

Embodiment 3

[0030] Example 3 In a 250ml four-neck flask 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, 4.95g of caged phosphate amine and 3.03g of Triethylamine, use nitrogen to drive out the air in the bottle, and under the condition of 10°C, drop 1.70g of phosphorus trichloride into the reaction bottle within 1h, control the dropping temperature at 10°C to 20°C, after the dropwise addition, Raise the temperature to 100°C for 4 hours, then cool to 20°C, filter, and dry in vacuo to obtain a solid mixture of a yellow product and triethylamine hydrochloride. The solid mixture was dissolved with 80ml dimethyl sulfoxide, filtered, and the filtrate was evaporated to dryness to obtain the product phosphorothioate-(N, N', N "-tricage phosphate) triamine. The yield was 91.5%, and the decomposition temperature was 264 ℃.

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Abstract

The invention relates to a flame retardant thiophosphoryl-(N,N',N'-tricaged phosphate) triamine compound and a preparation method thereof. The compound has a structure as shown in the formula in the specification. The preparation method comprises the following steps: adding amine of caged phosphate and triethylamine, cooling to 10 DEG C, dropwise adding phosphorus trichloride, controlling the dropwise adding temperature to be 10-20 DEG C, heating to 80-110 DEG C after dropwise addition is completed, insulating to react for 3-5 hours, cooling, filtering and drying in vacuum to obtain solid mixture a yellow target product and triethylamine hydrochloride; dissolving the solid mixture with dimethyl sulfoxide, filtering, and drying the filtrate by distillation to obtain the target product thiophosphoryl-(N,N',N'-tricaged phosphate) triamine. The compound is an excellent phosphorus-nitrogen synergistic flame retardant, is suitable for flame retardants of polyester, polyurethane, epoxy resin,unsaturated resin, polyvinyl chloride and other materials, is simple in process and less in equipment investment, and is easy to realize industrial production.

Description

technical field [0001] The invention relates to a flame retardant thiophosphoryl-(N, N', N"-tricage phosphate) triamine compound and a preparation method thereof, in particular to a flame retardant thiophosphoryl tri[N , N′, N″-tris(1-oxo-1-phospha-2,6,7-trioxahoctyl<4>)] amine compound and preparation method thereof, the compound is suitable for use as polyester, Flame retardant for polyurethane, epoxy resin, unsaturated resin, polyvinyl chloride and other materials. Background technique [0002] With the continuous development of the global economy, flammable polymer materials have been widely used, and flame retardant technology has also been developed rapidly. Currently widely used flame retardants include halogen-based, phosphorus-based, and nitrogen-based flame retardants. Halogenated flame retardants have been widely used since the 1960s, and their application technology is relatively mature. However, due to the toxicity of burning, since the European Union pr...

Claims

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Application Information

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IPC IPC(8): C08K5/5399C08K5/3492C08L67/02C07F9/6574
CPCC07F9/65748C08K5/34928C08K5/5399C08L67/02C08L2201/02
Inventor 魏怀鑫沈敏杰王彦林
Owner SUZHOU UNIV OF SCI & TECH
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