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Reactive flame retardant thiophosphoryl heterocyclic silicate compound and preparation method thereof

A flame retardant thiophosphonyl and reactive technology, which is applied in the field of reactive flame retardant thiophosphono heterocyclic silicate compounds and their preparation, can solve problems such as affecting the performance of materials, and achieve less investment in equipment , High flame retardant efficiency, improve the effect of flame retardant carbonization

Inactive Publication Date: 2019-06-14
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are two types of flame retardants used: additive flame retardants and reactive flame retardants. Due to the more or less incompatibility between the additive flame retardants and the polymer matrix, it will be accompanied by escape during processing. Phenomena such as exudation and decomposition affect the performance of materials

Method used

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  • Reactive flame retardant thiophosphoryl heterocyclic silicate compound and preparation method thereof
  • Reactive flame retardant thiophosphoryl heterocyclic silicate compound and preparation method thereof
  • Reactive flame retardant thiophosphoryl heterocyclic silicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 In a 100ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a drying tube and a hydrogen chloride absorption device at the upper mouth of the condenser, add 50ml of diethylene glycol dimethyl ether and 7.8g (0.05 mol) trihydroxymethylphosphorus sulfide, at 20°C, add 6.45g (0.05mol) dimethyldichlorosilane dropwise, the temperature during the dropwise addition should not exceed 40°C, after the dropping, heat up to 70°C for 1 hour, and keep warm for the reaction 5h, then heat up to 130°C, keep warm for 7h, distill off the solvent and a small amount of low boiling point substances under reduced pressure, cool down to 30°C, add 20 ml of water, add 5% sodium carbonate solution dropwise, adjust the system to pH = 7, statically Place, separate layers, remove the colorless transparent viscous liquid in the lower layer, and obtain the reactive flame retardant thiophosphonoheterocyclic silicate, and the product yield is 95.3%....

Embodiment 2

[0023] Example 2 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a drying tube and a hydrogen chloride absorbing device at the upper mouth of the condenser, add 60ml of tetrachloroethane and 7.8g (0.05mol) of trichloride Hydroxymethylphosphorus sulfide, at 20°C, add 6.45g (0.05mol) of dimethyldichlorosilane dropwise, and control the temperature during the dropwise addition to not exceed 40°C. Raise the temperature to 140°C, keep it warm for 6 hours, distill off the solvent and a small amount of low boiling point substances under reduced pressure, cool down to 30°C, add 20 ml of water, add 5% sodium carbonate solution dropwise, adjust the system to pH = 7, let stand, and divide layer, and the lower layer was removed as a colorless transparent viscous liquid to obtain a reactive flame retardant thiophosphonoheterocyclic silicate with a product yield of 94.1%.

Embodiment 3

[0024] Example 3 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a drying tube and a hydrogen chloride absorption device at the upper mouth of the condenser, add 40ml of ethylene glycol diethyl ether and 7.8g (0.05mol) Trihydroxymethylphosphorus sulfide, at 20°C, add 6.45g (0.05mol) of dimethyldichlorosilane dropwise, and control the temperature during the dropwise addition to not exceed 40°C. After the dropping, heat up to 70°C for 1 hour, and keep the temperature for 5 hours. Then heat up to 120°C, keep the temperature for 8 hours, distill off the solvent and a small amount of low boiling point substances under reduced pressure, cool down to 30°C, add 20 ml of water, add 5% sodium carbonate solution dropwise, adjust the system to pH=7, let it stand, Separate layers, and remove the lower layer of colorless transparent viscous liquid to obtain the reactive flame retardant thiophosphonoheterocyclic silicate, with a prod...

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Abstract

The invention relates to a reactive flame retardant thiophosphoryl heterocyclic silicate compound and a preparation method thereof. The structure formula of the compound is shown by a formula in the description. The preparation method of the compound comprises the following steps: adding an organic solvent and trihydroxymethyl phosphorus sulfide into a reaction container, dropwise adding equimolardimethyldichlorosilane, controlling the temperature to be not higher than 40 DEG C in the dropwise-adding process, increasing the temperature to 70 DEG C in one hour after dropwise adding is completed, then keeping the temperature and reacting for 5 hours, then increasing the temperature to 120-140 DEG C, then keeping the temperature and reacting for 6-8 hours, and carrying out purification treatment to obtain reactive flame retardant thiophosphoryl heterocyclic silicate. The compound provided by the invention contains three flame-retardant elements including phosphorus, silicon and sulfur, achieves a synergistic effect, is excellent in flame retardance and carbon-forming performance, is suitably used as flame retardants of unsaturated polyester resin, polyvinyl alcohol, epoxy resin and the like, is applied to reactive flame retardant added with polyurethane, and can also be used as an organic synthesis intermediate; meanwhile, the preparation method of the compound is one-step reaction, simple in process, low in equipment investment and easy in realization of industrial production.

Description

technical field [0001] The invention relates to a reactive flame retardant thiophosphono heterocyclic silicate compound and a preparation method thereof, in particular to a reactive flame retardant 1,1-dimethyl-1-sila-2, 6-dioxa-4-thio-4-phosphine-4-hydroxymethylcyclohexane compound and its preparation method, the compound is suitable for use as flame retardant of unsaturated resin, polyvinyl alcohol, epoxy resin, etc. It is used as a reactive flame retardant for polyurethane; it can also be used as an intermediate in organic synthesis. Background technique [0002] At present, organic synthetic materials have been widely used in construction, electronic appliances, transportation and other fields, but their flammability will pose a serious threat to people's lives and property. Combustible organic synthetic materials are already one of the main sources of fire in cities and buildings. People are always eager to use flame-retardant materials to prevent or reduce the disaste...

Claims

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Application Information

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IPC IPC(8): C07F9/6596C08K5/549
Inventor 许梓轩王世杰王彦林
Owner SUZHOU UNIV OF SCI & TECH
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