Fire retardant silicon phosphine heterocyclic methylene diphenylthioc phosphinate compound and preparation method thereof

A technology of diphenylthiophosphinic acid and heterocyclic methylene ester, which is applied in the field of flame retardant diphenylthiophosphinic acid silicon phosphine heterocyclic methylene ester compound and its preparation field, and can solve the problem of fire Threat and other issues, to achieve the effect of less investment in equipment, stable structure, and convenient operation

Inactive Publication Date: 2019-06-21
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] With the advancement and development of science and technology, polymer materials have been widely used in all walks of life, but most of them are flammable, which will bring fire threats to people, so flame retardant technology has been developed rapidly; With the enhancement of social awareness of environmental protection, while people require flame retardants to be more efficient, they also put forward stricter environmental protection and safety requirements, which also promotes the development of non-halogenated flame retardants.

Method used

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  • Fire retardant silicon phosphine heterocyclic methylene diphenylthioc phosphinate compound and preparation method thereof
  • Fire retardant silicon phosphine heterocyclic methylene diphenylthioc phosphinate compound and preparation method thereof
  • Fire retardant silicon phosphine heterocyclic methylene diphenylthioc phosphinate compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Example 1 In a 250ml four-neck 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 out with nitrogen, and 100ml of diethylene glycol dimethyl was added. Ether, 11.76g (0.06mol) trimethylolphosphine oxide cyclic ester of dimethyl silicate, after the trimethylol phosphine oxide cyclic ester of dimethyl silicate is completely dissolved, 12.65g ( 0.05mol) of diphenylthiophosphinyl chloride, control the temperature during the dropping process to not exceed 60°C, raise the temperature to 135°C after the dropwise addition, and keep the temperature for 11 hours to keep the hydrogen chloride released, adjust the pH of the reaction system to 6 with a pyridine acid-binding agent -7, Diethylene glycol dimethyl ether (recycled) was removed by distillation under reduced pressure, 90ml of ethanol was added to the crude product for heatin...

Embodiment 2

[0027] Example 2 In a 250ml four-neck 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 out with nitrogen, and 90ml of diethylene glycol dimethyl was added. Ether, 10.78g (0.055mol) trimethylolphosphine oxide cyclic ester of dimethyl silicate, after the trimethylol phosphine oxide cyclic ester of dimethyl silicate is completely dissolved, add 12.65g dropwise with stirring at 30°C (0.05mol) diphenylphosphinyl thiochloride, control the temperature during the dropwise addition to not exceed 60°C, raise the temperature to 140°C after the dropwise addition, keep the temperature for 11 hours, and adjust the reaction system with triethylamine acid-binding agent after the hydrogen chloride is released pH = 6-7, diethylene glycol dimethyl ether (recycled) was removed by distillation under reduced pressure, 90ml of ethanol was added to t...

Embodiment 3

[0028] Example 3 In a 250ml four-neck 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 out with nitrogen, and 110ml of diethylene glycol dimethyl was added. Ether, 9.80g (0.05mol) trihydroxymethylphosphine oxide cyclic ester of dimethyl silicate, after the trimethylol phosphine oxide cyclic ester of dimethyl silicate is completely dissolved, add 12.65g dropwise with stirring at 30°C (0.05mol) diphenylphosphinyl thiochloride, the dropwise addition process controls the temperature not to exceed 60°C, after the dropwise addition, the temperature is raised to 130°C, and the temperature is kept for 10 hours. After the hydrogen chloride is released, the pH of the reaction system is adjusted with a pyridine acid-binding agent. 6-7, Diethylene glycol dimethyl ether (recycled) was removed by distillation under reduced pressure, 90ml of...

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Abstract

The invention relates to a fire retardant silicon phosphine heterocyclic methylene diphenylthioc phosphinate compound and a preparation method of the compound. A structure of the compound is shown asthe following formula. The preparation method comprises the steps of controlling a mole ratio of diphenylphosphinyl chloride to trimethylol phosphine oxide cyclic dimethyl silicate in an organic solvent to be 1.0:1.0-1.0:1.2, dropwise adding diphenylphosphinyl chloride at 30 DEG C, controlling a temperature not to exceed 60 DEG C in a dropwise adding process, after dropwise adding, heating to 120-140 DEG C, performing heat insulation reaction for 9-12h, completely discharging hydrogen chloride, and performing purification treatment to form the white solid organosilicon, phosphine and sulfur fire retardant silicon phosphine heterocyclic methylene diphenylthioc phosphinate. The compound is an excellent silicon, phosphorus and sulfur synergic fire retardant, and can be used for fire retardance of materials such as epoxy resin, polyester and unsaturated resin; a technology of the compound is simple; the equipment investment is low; and the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a flame retardant diphenylphosphinophosphine heterocyclic methylene ester compound and a preparation method thereof, in particular to a three-element organic silicon, phosphine and sulfur synergistic flame retardant diphenylsulfur Phosphinic acid (1,1-dimethyl-1-sila-2,6-dioxa-4-oxyl-4-phosphine-<4>-methylene) ester compound and preparation method thereof , the compound is a flame retardant containing three flame retardant elements of silicon, phosphorus and sulfur, and can be used as a flame retardant for epoxy resin, polyester, unsaturated resin and other materials. Background technique [0002] With the advancement and development of science and technology, polymer materials have been widely used in all walks of life, but most of them are flammable, which will bring fire threats to people, so flame retardant technology has been developed rapidly; With the enhancement of social awareness of environmental protection, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/549C08L63/00C08L67/02C07F9/6596
Inventor 王世杰陈竹王彦林
Owner SUZHOU UNIV OF SCI & TECH
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