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Alkyl dimethoxy silicic phosphine heterocyclic methyl ester compound and preparing method thereof

A technology of alkyl dimethoxy phosphine and flame retardant alkyl dimethoxy silicate is applied in the field of alkyl dimethoxy phosphine heterocyclic methyl ester compound and preparation thereof, and can solve the problem Organosilicon flame retardants have problems such as slow development, poor electrical properties, and large polarity, which achieve the effects of easy large-scale production, high atom utilization, and good compatibility.

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

Although there are many studies on organophosphine flame retardants, they still have disadvantages such as high cost, high polarity, easy migration, and poor electrical performance. There is a strong market demand for organophosphine flame retardants with excellent comprehensive cost performance; The performance of flame retardants is better, but the development of silicone flame retardants is also very slow

Method used

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  • Alkyl dimethoxy silicic phosphine heterocyclic methyl ester compound and preparing method thereof
  • Alkyl dimethoxy silicic phosphine heterocyclic methyl ester compound and preparing method thereof
  • Alkyl dimethoxy silicic phosphine heterocyclic methyl ester compound and preparing method thereof

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Effect test

Embodiment 1

[0036] Example 1 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 16.21g (0.10mol) of cage-like phosphate, 30ml of diethylene glycol dimethyl ether , 14.99g (0.11mol) methyltrimethoxysilane and 0.45g dimethyl sulfate, heated to 102 ° C, reflux reaction, as the reaction progressed, the reflux temperature gradually increased to 130 ° C, reflux and heat preservation for 17 hours, and then Cool to 60°C, transfer to a separatory funnel to stand for stratification, separate the lower layer of material liquid, then add 30ml of toluene to wash, stand still to separate the lower layer of material liquid, and then distill under reduced pressure to remove toluene and a small amount of low boiling point substances to obtain light Yellow liquid methyl dimethoxyphosphonomethyl heterocyclic methyl dimethoxysilicate, product yield 90.5%, flash point (open cup): 204±5°C, decomposition ...

Embodiment 2

[0037] Example 2 In a 100ml 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 16.21g (0.10mol) of cage-like phosphate, 16.36g (0.12mol) of methyl Trimethoxysilane and 0.32g dimethyl sulfate, heated to 102°C, reflux reaction, as the reaction progressed, the reflux temperature gradually increased to 120°C, reflux and heat preservation for 20h, then cooled to 60°C, added 30ml toluene to wash , stand to separate the lower layer feed liquid, and then remove toluene and a small amount of low boiling point matter by distillation under reduced pressure to obtain light yellow liquid methyl dimethoxyphosphine heterocyclic methyl silicate, the product yield is 87.2%, and its flash point (open cup): 204±5℃, decomposition temperature: 248±5℃, density (25℃): 1.679g / cm 3 , Refractive index: n D 25 = 1.3842.

Embodiment 3

[0038] Example 3 In a 100ml 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 16.21g (0.10mol) of caged phosphate ester, 20mlDMF, 13.63g (0.10mol) Methyltrimethoxysilane and 0.40g methyl p-toluenesulfonate, heated to 102 °C, reflux reaction, as the reaction progressed, the reflux temperature gradually increased to 130 °C, reflux and heat preservation for 15 hours, and then cooled to 60 °C, Transfer to a separatory funnel and let stand for layering, separate the lower layer of feed liquid, then add 30ml of toluene to wash, let stand to separate the lower layer of feed liquid, and then distill under reduced pressure to remove toluene and a small amount of low boiling point matter to obtain light yellow liquid methyl dimethicone. Phosphine heterocyclic methyl methoxysilicate, product yield 88.0%, flash point (open cup): 204±5°C, decomposition temperature: 248±5°C, density (25°C): 1.6...

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Abstract

The invention relates to an alkyl dimethoxy silicic phosphine heterocyclic methyl ester compound and a preparing method thereof. The structure of the compound is shown in the following formula (see the formula in description), wherein R represents a methyl, or ethyl, or propyl or butyl group. The preparing method includes the steps that under protection of nitrogen, the molar ratio of 4-ethyl-2,6,7-trioxa-1-phosphine heterobicyclic [2.2.2] octane to alkyl trimethoxy silane is controlled to be 1:1-1:1.5, under the action of a catalyst, 4-ethyl-2,6,7-trioxa-1-phosphine heterobicyclic [2.2.2] octane and alkyl trimethoxy silane are heated to reflux and react for 10-20 h at the temperature of 100 DEG C-180 DEG C on the reflux and heat-preserving conditions, and alkyl dimethoxy silicic phosphine heterocyclic methyl ester is obtained through purification. The alkyl dimethoxy silicic phosphine heterocyclic methyl ester compound is suitable for serving as fire retardant of polyester PBT, PET, polyurethane, unsaturated resin, epoxy resin and the like. The production process is simple, equipment investment is small, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to a flame retardant alkyl dimethoxy phosphine heterocyclic methyl silicate compound and a preparation method thereof, in particular to a flame retardant alkyl dimethoxy (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, polyurethane, unsaturated resin, epoxy resin and other materials. Background technique [0002] With the rapid development of science and technology, the flame retardant industry is also developing rapidly. With the enhancement of people's awareness of safety and environmental protection, the requirements for flame retardants and flame retardant materials are also getting higher and higher. Although traditional halogen-based flame retardants ha...

Claims

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Application Information

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