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Preparation method of trihydroxymethylphosphine oxide caged phosphorothioate compound

A technology of phosphorothioate and trimethylol is applied in the field of preparation of trimethylol phosphine oxide caged phosphorothioate compounds, which can solve problems such as secondary hazards to people's life safety, and achieve easy large-scale transformation and production. The effect of production, good compatibility and easy operation

Active Publication Date: 2017-10-31
HUZHOU RUIGAO NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although traditional halogenated flame retardants have good flame retardant properties and are cheap, the toxic gases such as dioxins produced during combustion will cause secondary hazards to people's lives.

Method used

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  • Preparation method of trihydroxymethylphosphine oxide caged phosphorothioate compound
  • Preparation method of trihydroxymethylphosphine oxide caged phosphorothioate compound
  • Preparation method of trihydroxymethylphosphine oxide caged phosphorothioate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a hydrogen chloride absorption device connected to the upper mouth of the condenser, the air in the bottle was driven away with nitrogen, and 30ml of diethylene glycol dimethyl was added. Ether, 14.00g (0.1mol) trimethylolphosphine oxide, under stirring, add 16.93g (0.1mol) phosphorous trichloride dropwise at 20°C, make it fully mixed, heat up to 60°C, hydrogen chloride begins to be released , heat up to 90°C for 2 hours, then heat up to 160°C for 4 hours, wait until no hydrogen chloride is released, remove diethylene glycol dimethyl ether (recycled) by distillation under reduced pressure, cool down to below 20°C, and then add 50ml of ice water, Under stirring, 5% sodium carbonate solution was added dropwise to make the reaction system pH=7, the product solid was dispersed in water, filtered, the filter cake was rinsed with 10ml of ice water, compacted an...

Embodiment 2

[0026] Example 2 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and connected to a hydrogen chloride absorption device on the condenser, the air in the bottle was driven away with nitrogen, and 40ml of anisole was added, 14.00g (0.1mol) trihydroxymethylphosphine oxide, under stirring, at 20°C, add 16.93g (0.1mol) of phosphorus thionium chloride dropwise, make it fully mixed, heat up to 60°C, hydrogen chloride begins to be released, heat up to 90 Insulate at ℃ for 2 hours, then raise the temperature to 150℃ and keep the reaction for 6 hours. After no hydrogen chloride is released, distill under reduced pressure to remove anisole (recycling), cool down to below 20℃, add 45ml of ice water, and add 5% of Sodium carbonate solution, make the reaction system pH=7, disperse the product solid in water, filter, rinse the filter cake with 10ml ice water, compact and drain, and dry the filter cake in vacuum to obtain white solid tris...

Embodiment 3

[0027] Example 3 In a 150ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and connected to a hydrogen chloride absorption device on the condenser, the air in the bottle was driven away with nitrogen, and 50ml xylene was added, and 14.00g ( 0.1mol) Trishydroxymethyl phosphine oxide, under stirring, at 20°C, add 16.93g (0.1mol) of phosphorus thionium chloride dropwise, make it fully mixed, heat up to 60°C, hydrogen chloride begins to be released, heat up to 90°C Keep warm for 2 hours, then raise the temperature to 140°C and keep it warm for 7 hours. After no hydrogen chloride is released, distill off xylene (recycled) under reduced pressure, cool down to below 20°C, add 55ml of ice water, and add 5% sodium carbonate dropwise under stirring. solution, make the reaction system pH=7, disperse the product solid in water, filter, rinse the filter cake with 10ml of ice water, compact and drain, and dry the filter cake in vacuum to obtain w...

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Abstract

The invention relates to a preparation method of a flame retardant trishydroxymethylphosphine oxide cage phosphorothioate compound. The structure of the compound is shown in the following formula: the preparation method is: under the protection of nitrogen, at 20 ° C, equimolar Chlorathion and trishydroxymethyl phosphine oxide are fully mixed, heated to 90°C and kept for 2 hours, then heated to 130-160°C and kept for 4-9 hours, hydrogen chloride was exhausted, and after purification, a tris-hydroxymethyl phosphine oxide cage was obtained Phosphorothioate. The compound of the invention has high phosphorus content and excellent flame retardant performance, and is suitable for use as a flame retardant for polyester, polyurethane, epoxy resin, unsaturated resin, polyolefin and the like. And the preparation method is one-step reaction, the process is simple, the equipment investment is small, and the industrialized production is easy to realize.

Description

technical field [0001] The invention relates to a method for preparing an organic phosphine flame retardant trishydroxymethylphosphine oxide cage phosphorothioate compound, in particular to a 1-thio-4-oxo-2,6,7-trioxa- A preparation method of 1,4-diphosphabicyclo[2.2.2]octane compound, the compound is suitable for use as a flame retardant for materials such as polyester, polyurethane, epoxy resin, unsaturated resin, polyolefin and the like. Background technique [0002] With the rapid development of polymer materials, the application range of flame retardant materials is also continuously expanding, and due to the enhancement of people's environmental protection awareness, there are higher requirements for flame retardants. At the same time, it is also required to be friendly to the environment, so the non-halogenation of flame retardants has become one of the research hotspots in this field, which promotes the development of green and environmentally friendly flame retardan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/5398C08L67/02
Inventor 王彦林杨珂珂
Owner HUZHOU RUIGAO NEW MATERIALS CO LTD
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