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Flame retardant namely trimeric O,O-2-hydroxymethylphosphonyl heteropropylene phosphazene compound and preparation method thereof

A technology of hydroxymethylphosphonoheterylene phosphazene and trimethylolphosphorus oxide is applied in the field of flame retardant trimer O, which can solve the problems such as the limitation of halogen-based flame retardants, and achieve high flame retardant efficiency and structure. Novel and symmetrical structure

Inactive Publication Date: 2019-04-02
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the increasing awareness of people's health and environmental protection, halogenated flame retardants are restricted in many ways

Method used

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  • Flame retardant namely trimeric O,O-2-hydroxymethylphosphonyl heteropropylene phosphazene compound and preparation method thereof
  • Flame retardant namely trimeric O,O-2-hydroxymethylphosphonyl heteropropylene phosphazene compound and preparation method thereof
  • Flame retardant namely trimeric O,O-2-hydroxymethylphosphonyl heteropropylene phosphazene compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 In a 250ml three-necked flask equipped with a stirrer, a thermometer and a condenser tube, and a drying tube at the top of the condenser tube, replace the air in the bottle with nitrogen, and add 10.42g (0.03mol) of hexachlorocyclotri Phosphazene, 80ml dioxane and 18.18g (0.18mol) triethylamine, after stirring to dissolve hexachlorocyclotriphosphazene, add 12.61g (0.09mol) trimethylol phosphorus oxide dropwise, and control the reaction with the dropping rate The temperature is not higher than 40°C. After dropping, the temperature is raised to 100°C, and the temperature is kept for 8 hours; the temperature is lowered to below 30°C, and the formed triethylamine hydrochloride is removed by suction filtration, and dioxane is removed by vacuum distillation (recycling). Add 35ml of distilled water to wash twice, separate the lower organic phase, add 35ml of ethyl acetate, dry with 1g of anhydrous magnesium sulfate, filter with suction, distill the filtrate under redu...

Embodiment 2

[0025] Example 2 In a 250ml three-necked flask equipped with a stirrer, a thermometer and a condenser tube, and a drying tube at the top of the condenser tube, replace the air in the bottle with nitrogen, and add 10.42g (0.03mol) of hexachlorocyclotri Phosphazene, 80ml toluene and 21.78g (0.18mol) N, N-dimethylaniline, after stirring to dissolve hexachlorocyclotriphosphazene, add 12.61g (0.09mol) trihydroxymethyl phosphorus oxide dropwise, at the rate of addition Control the reaction temperature not to be higher than 40°C, raise the temperature to 110°C after dripping, and keep the temperature for 7 hours; lower the temperature to below 30°C, remove the generated N,N-dimethylaniline hydrochloride by suction filtration, and remove the toluene ( Recycling), add 35ml of distilled water to wash twice, separate the lower organic phase, add 35ml of ethyl acetate, dry with 1g of anhydrous magnesium sulfate, filter with suction, and distill the filtrate under reduced pressure to remove...

Embodiment 3

[0026] Example 3 In a 250ml three-neck flask equipped with a stirrer, a thermometer and a condenser tube, and a drying tube at the top of the condenser tube, replace the air in the bottle with nitrogen, and add 10.42g (0.03mol) of hexachlorocyclotri Phosphazene, 80ml ethylene glycol diethyl ether and 14.22g (0.18mol) pyridine, after stirring to dissolve hexachlorocyclotriphosphazene, add 12.61g (0.09mol) trimethylol phosphorus oxide dropwise, and control the reaction temperature with the dropping rate Not higher than 40°C, after dripping, raise the temperature to 120°C, keep the temperature for 6 hours; cool down to below 30°C, remove the generated pyridine hydrochloride by suction filtration, remove ethylene glycol diethyl ether (recycling) by vacuum distillation, add Wash twice with 35ml of distilled water, separate the lower organic phase, add 35ml of ethyl acetate, dry with 1g of anhydrous magnesium sulfate, filter with suction, distill the filtrate under reduced pressure t...

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Abstract

The invention relates to a flame retardant namely a trimeric O,O-2-hydroxymethylphosphonyl heteropropylene phosphazene compound and a preparation method thereof. The compound has a structure as shownin a formula which is described in the specification. The preparation method comprises the following steps: subjecting hexachlorocyclotriphosphazene and tris(hydroxymethyl)phosphine oxide to a reaction in an organic solvent at 100 DEG C to 130 DEG C for 5 to 11 h, wherein the molar ratio of the hexachlorocyclotriphosphazene to the tris(hydroxymethyl)phosphine oxide is controlled to be 1:3; and carrying out purifying treatment so as to obtain a colorless transparent viscous liquid namely trimeric O,O-2-hydroxymethylphosphonyl heteropropylene phosphazene. The compound provided by the invention is an excellent halogen-free phosphorus-nitrogen synergistic flame retardant, can be used as a flame retardant for polyester, polyamide, polyvinyl chloride, polyurethane, epoxy resin, unsaturated resinand the like, has simple process and less equipment investment, and facilitates realizing industrial production.

Description

technical field [0001] The invention relates to a flame retardant trimerized O, O-2-hydroxymethylphosphonopropylene phosphazene compound and a preparation method thereof. The compound contains phosphorus and nitrogen dual flame retardant elements and can be used as a polyester, poly Flame retardant for amides, polyurethanes, epoxy resins, unsaturated resins, polyvinyl alcohol and coatings, etc. Background technique [0002] The advancement of science and technology and the improvement of people's living standards have promoted the rapid development and wide application of the polymer material industry. At the same time, the flammability of polymer materials often causes fires, which will endanger people's lives and property. , thus promoting the development of flame retardant technology. With the increasing awareness of people's health and environmental protection, halogenated flame retardants are restricted in many ways. The intumescent flame retardant with phosphorus and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/659
CPCC07F9/659
Inventor 董淑玲王伟光王彦林
Owner SUZHOU UNIV OF SCI & TECH
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