Methyl phenyl bis(phosphorous heterocycle methoxy group) silane compound and preparation method thereof

A technology of methylphenyldimethoxysilane and methylphenyl, which is applied in the field of flame retardant methylphenylbissilane compound and its preparation, can solve problems such as changes in mechanical properties of materials, and achieve little impact on mechanical properties. , high flame retardant efficiency, good dispersion effect

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

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Problems solved by technology

[0002] In the development trend of non-halogenated flame retardants, phosphorus-based flame retardants are favored because of their high efficiency, environmental protection, and low toxicity. However, because the addition of such flame retardants will cause changes in the mechanical properties of materials, people hope that Improve the deficiencies of phosphorus flame retardants by introducing other excellent flame retardant elements into the molecule

Method used

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  • Methyl phenyl bis(phosphorous heterocycle methoxy group) silane compound and preparation method thereof
  • Methyl phenyl bis(phosphorous heterocycle methoxy group) silane compound and preparation method thereof
  • Methyl phenyl bis(phosphorous heterocycle methoxy group) silane compound and preparation method thereof

Examples

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Effect test

Embodiment 1

[0028] Example 1 In a 200ml 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 37.28g (0.23mol) of cage-like phosphate ester and 90ml of diethylene glycol dimethyl ether , 18.23g (0.10mol) methylphenyldimethoxysilane and 0.85g dimethyl sulfate, heat up to 160 ° C, keep the temperature for 14 hours, remove diethylene glycol dimethyl ether (recycled) by distillation under reduced pressure, and then Add 80ml of distilled water, stir to disperse the solid in water, suction filter and dry to obtain white solid methylphenylbis(phosphacyclomethoxy)silane, the product yield is 87.4%, melting point: 160±2°C, decompose Temperature: 328±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 38.90g (0.24mol) of caged phosphoric acid ester, 18.23g (0.10mol) of methyl Phenyldimethoxysilane and 0.55g dimethyl sulfate, heat up to 130°C, keep warm for 18h, cool to 60°C, add 60ml of distilled water, stir to disperse the solid in the water, filter and dry to obtain a white solid Methylphenylbis(phosphacyclomethoxy)silane, product yield 88.7%, melting point: 160±2°C, decomposition temperature: 328±5°C.

Embodiment 3

[0030] Example 3 In a 200ml 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 34.04g (0.21mol) of caged phosphate ester, 60mlDMF, 18.23g (0.10mol) Methylphenyldimethoxysilane and 0.65g methyl p-toluenesulfonate, heat up to 140°C, keep warm for 16 hours, distill off DMF under reduced pressure (for recycling), then add 100ml of distilled water, stir to disperse the solid in water , suction filtration, and drying to obtain white solid methylphenylbis(phosphacyclomethoxy)silane with a product yield of 84.0%, melting point: 160±2°C, and decomposition temperature: 328±5°C.

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Abstract

The invention relates to a methyl phenyl bis(phosphorous heterocycle methoxy group) silane compound and a preparation method thereof. The structural formula of the compound is shown in the following specifications. The preparation method includes the steps that under protection of nitrogen, the molar ratio of methyl phenyldimethoxysilane to 4-ethyl-2,6,7-trioxa-1-phosphabicyclo (2.2.2) octane is 1:2-1:2.5, under the action of catalyst, temperature is increased to 120 DEG C-180 DEG C, thermal-insulation reaction is performed for 13-19 h, and through purification, the methyl phenyl bis(phosphorous heterocycle methoxy group) silane product is obtained. The compound is suitable for being used as flame retardant of PBT, PET, nylon, PC, polyurethane and furan resin. The production technology is simple, the requirement for environmental friendliness is met, industrialized production is easy to achieve, and good development and application prospects are achieved.

Description

technical field [0001] The invention relates to a flame retardant methylphenyl bis(phosphacyclomethoxy)silane compound and a preparation method thereof, in particular to a flame retardant methylphenyl bis(1-oxo-1-methyl- 4-Ethyl-1-phospha-2,6-dioxa-cyclohexyl-<4>-methoxy)silane compound and its preparation method, the compound contains phosphorus and silicon double flame retardant elements, phosphorus Silicon Synergy has a high flame retardant performance, suitable for use as a flame retardant for polyester PBT, PET, nylon, PC, polyurethane, furan resin and other materials. Background technique [0002] In the development trend of non-halogenated flame retardants, phosphorus-based flame retardants are favored because of their high efficiency, environmental protection, and low toxicity. However, because the addition of such flame retardants will cause changes in the mechanical properties of materials, people hope that Improve the deficiencies of phosphorus-based flame ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08K5/5419C08L67/02
Inventor 王彦林李果
Owner SUZHOU UNIV OF SCI & TECH
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