Fire retardant - phenyl tri-(phosphonia cyclomethoxy) silane compound and preparation method thereof

A technology of phenyltrimethoxysilane and phenyltrisilane, which is applied in the field of flame retardant phenyltrisilane compounds and their preparation, can solve the problems of limited application range, influence of polymer thermal stability and mechanical properties, etc. Stable physical and chemical properties, promoting flame retardant effect, and no three-waste emission effect

Active Publication Date: 2016-01-20
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when silicon-based flame retardants and phosphorus-based flame retardants are used alone, there are inevitably some defects.
For example, silicon-based flame retardants only have excellent flame-retardant properties for some polymers, and their application range is not wide; phosphorus-based flame retardants will have a negative impact on the thermal stability and mechanical properties of polymers

Method used

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  • Fire retardant - phenyl tri-(phosphonia cyclomethoxy) silane compound and preparation method thereof
  • Fire retardant - phenyl tri-(phosphonia cyclomethoxy) silane compound and preparation method thereof
  • Fire retardant - phenyl tri-(phosphonia cyclomethoxy) silane compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 In a 250ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, replace the air in the bottle with nitrogen, and add 51.87g (0.32mol) of caged phosphate, 90ml of diethylene glycol dimethyl ether , 19.83g (0.10mol) phenyltrimethoxysilane and 1.45g dimethyl sulfate, heat up to 155°C, keep warm for 18h, remove diethylene glycol dimethyl ether (recycled) by distillation under reduced pressure, and cool to 50°C , then add 68ml of petroleum ether, stir to make the solid dispersed in petroleum ether, filter with suction and dry to get white solid phenyl tris (phosphacyclomethoxy) silane, product yield 85.0%, its decomposition temperature: 335 ±5°C.

Embodiment 2

[0029] Example 2 In a 150ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, replace the air in the bottle with nitrogen, and add 50.25g (0.31mol) of caged phosphate, 19.83g (0.10mol) of phenyl Trimethoxysilane and 1.35g dimethyl sulfate, heat up to 140°C, keep warm for 20h, cool to 50°C, add 68ml of petroleum ether, stir to disperse the solid in petroleum ether, filter with suction and dry to obtain a white solid Phenyltris(phosphacyclomethoxy)silane, the product yield is 83.7%, and its decomposition temperature: 335±5°C.

Embodiment 3

[0030] Example 3 In a 250ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, replace the air in the bottle with nitrogen, and add 53.49g (0.33mol) of caged phosphate ester, 100mlDMF, 19.83g (0.10mol) Phenyltrimethoxysilane and 0.80g methyl p-toluenesulfonate, heat up to 130°C, keep warm for 22h, distill off DMF (recycled) under reduced pressure, cool to 50°C, add 68ml of petroleum ether, stir to make the solid Disperse in petroleum ether, filter with suction, and dry to obtain white solid phenyltris(phosphacyclomethoxy)silane with a product yield of 86.4%, and its decomposition temperature: 335±5°C.

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Abstract

The invention relates to a fire retardant - phenyl tri-(phosphonia cyclomethoxy) silane compound and a preparation method thereof. The structure of the compound is shown in the following formula (please see the specifications). According to the preparation method, under the protection of nitrogen, the molar ratio of phenyl trimethoxy silane to 4-ethyl-2,6,7-trioxa-1-phosphonia bicyclo-[2.2.2] octane is controlled between 1 to 3 and 1 to 3.3, the temperature is raised to the level between 130 DEG C and 200 DEG C under the action of catalysts and maintained for reaction for 15-22h, and purification is conducted to obtain phenyl tri-(phosphonia cyclomethoxy) silane. The product is stable in performance, good in fire retarding effect, capable of preventing melting drips and suitable for being used as the fire retardant for nylon, polyester PBT, PET, polyurethane, PC, ABS and other materials; moreover, the production process is simple, equipment investment is little, industrial production is easy, and a good development and application prospect is obtained.

Description

technical field [0001] The present invention relates to a kind of organosilicon phosphorus flame retardant phenyl tris (phosphacyclomethoxy) silane compound and preparation method thereof, in particular to a kind of flame retardant phenyl tris (1-oxo-1-methyl-4 -Ethyl-1-phospha-2,6-dioxa-cyclohexyl-<4>-methoxy)silane compound and its preparation method, the compound contains silicon and phosphorus double flame retardant elements, silicon phosphorus Synergy has high flame retardant performance, suitable for use as a flame retardant for nylon, polyester PBT, PET, polyurethane, PC, ABS and other materials. Background technique [0002] Due to the advantages of less added amount, good flame retardant effect, and little impact on the mechanical properties of materials, halogenated flame retardants occupy a major share in the flame retardant market in my country. However, with the enhancement of people's awareness of environmental protection, the disadvantages of this kind ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6571C07F9/6574C08K5/5435C08L77/02
Inventor 王彦林李果
Owner SUZHOU UNIV OF SCI & TECH
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