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Fire retardant namely tri(dimethyl silicon phosphonyl heterocyclic methylene) thiophosphate compound and preparation method thereof

A technology of dimethylsilylphosphonyl heterocyclic methylene and flame retardant thiophosphoric acid tris, which is applied to the flame retardant thiophosphoric acid tris (dimethyl silylphosphono heterocyclic methylene) ester compound and the same In the field of preparation, it can solve problems such as secondary hazards to people's life safety, and achieve the effects of easy large-scale transformation and production, high decomposition temperature, and low equipment investment.

Inactive Publication Date: 2019-05-31
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although traditional halogenated flame retardants have good flame retardant performance and moderate price, the toxic gases such as dioxin produced during combustion will cause secondary harm to people's life safety

Method used

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  • Fire retardant namely tri(dimethyl silicon phosphonyl heterocyclic methylene) thiophosphate compound and preparation method thereof
  • Fire retardant namely tri(dimethyl silicon phosphonyl heterocyclic methylene) thiophosphate compound and preparation method thereof
  • Fire retardant namely tri(dimethyl silicon phosphonyl heterocyclic methylene) thiophosphate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 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, use nitrogen to exhaust the air in the bottle, and at 20°C, add 29.4g ( 0.15mol) trimethylol phosphine oxide cyclic ester of dimethyl silicate and 90ml of diethylene glycol dimethyl ether, after the trimethylol phosphine oxide cyclic ester of dimethyl silicate is completely dissolved and dispersed, add dropwise 8.47g (0.05mol) of phosphorus trichloride, control the dropwise addition process not to exceed 60°C, after the dropwise addition, the temperature is raised to 120°C, and the heat preservation reaction is carried out for 10h, so that the hydrogen chloride is released completely, and the solvent is distilled off under reduced pressure to obtain a turbid viscous liquid; The crude product was poured into 100 ml of ice water and stirred rapidly for 30 min, filtered with s...

Embodiment 2

[0026] 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, use nitrogen to exhaust the air in the bottle, and at 20°C, add 30.38g ( 0.155mol) trimethylol phosphine oxide cyclic ester of dimethyl silicate and 120ml anisole, after the trimethylol phosphine oxide cyclic ester of dimethyl silicate is completely dissolved and dispersed, add 8.47g (0.05 mol) phosphorus trichloride, control the dropping process not to exceed 60°C, raise the temperature to 150°C after dropping, keep the temperature for 11 hours, let the hydrogen chloride be released, remove the solvent by distillation under reduced pressure, and obtain a turbid viscous liquid; then pour the crude product into Stir rapidly in 100 ml of ice water for 30 min, filter with suction, rinse with 50 ml of water, and vacuum-dry the filter cake to obtain the product tris(dimethylsily...

Embodiment 3

[0027] 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 exhausted with nitrogen, and at 20°C, 31.36g ( 0.16mol) trihydroxymethylphosphine oxide dimethylsilicate cyclic ester and 140ml xylene, after the trihydroxymethylphosphine oxide dimethylsilicate cyclic ester is completely dissolved and dispersed, add 8.47g (0.05mol ) Phosphorus trichloride, control the dropping process not to exceed 60°C, heat up to 140°C after dropping, keep the temperature for 9 hours, let the hydrogen chloride be released, and distill the solvent under reduced pressure to obtain a turbid viscous liquid; then pour the crude product into 100ml Stir rapidly in ice water for 30 min, filter with suction, rinse with 50 ml of water, and vacuum-dry the filter cake to obtain the product tris(dimethylsilylphosphonoheterocyclic methylene) ...

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Abstract

The invention relates to a fire retardant namely a tri(dimethyl silicon phosphonyl heterocyclic methylene) thiophosphate compound and a preparation method thereof. The structure of the compound is represented in the description. The preparation method comprises following steps: under the protection of nitrogen, at a temperature of 20 DEG C, dimethyl silicic acid trihydroxymethyl phosphine oxide cyclic ester is dissolved in an organic solvent, then thiophosphoryl chloride is dropwise added, the mole ratio of thiophosphoryl chloride to dimethyl silicic acid trihydroxymethyl phosphine oxide cyclic ester is controlled to be 1:3-1:3.6, during the dropwise addition process, the temperature is not higher than 60 DEG C; after the dropwise addition, the temperature is raised to 100 to 150 DEG C; the temperature is maintained to carry out reactions for 8 to 12 hours, and after hydrogen chloride is completely released, the reaction product is purified to obtain tri(dimethyl silicon phosphonyl heterocyclic methylene) thiophosphate. Through the cooperation among phosphor, silicon, and sulfur, a synergetic flame retardant effect is generated, the flame retardant performance is strong, the compound can be used as a fire retardant for polyester, polyurethane, epoxy resin, unsaturated resin, polyolefin, and the like; the preparation method adopts one-step reactions, the technology is simple, the equipment investment is little, and the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a flame retardant tris(dimethylsilylphosphonoheterocyclic methylene) phosphorothioate compound and a preparation method thereof, in particular to a tris[1,1-dimethyl-1 phosphorothioate] - Sila-2,6-dioxa-4-oxyl-4-phosphine-(4)-methylene] ester compound and its preparation method, the compound is suitable for use as polyester, polyurethane, epoxy resin , unsaturated resin, polyolefin and other materials flame retardant. 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. In the hope that flame retardant materials have good flame retardant properties At the same time, it is also emphasized that it is friendly to the environment, so the non-halogenation of flame retardants has become one of the hot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6596C08K5/549C08L63/00
Inventor 王彦林王世杰吴希雯
Owner SUZHOU UNIV OF SCI & TECH
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