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Dodecyl dimethyoxy phosphonic heterocyclic methyl ester compound and preparation method thereof

A technology of dodecyl dimethoxy phosphine and heterocyclic methyl ester is applied in the field of dodecyl dimethoxy phosphine heterocyclic methyl ester compound and preparation thereof, and can solve serious pollution, limited application scope and toxicity. Large and other problems, to achieve the effect of high decomposition temperature, small mechanical properties, and no three waste emissions

Active Publication Date: 2016-03-09
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the problems of high toxicity and serious pollution, the application range of traditional halogenated flame retardants has been gradually limited.

Method used

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  • Dodecyl dimethyoxy phosphonic heterocyclic methyl ester compound and preparation method thereof
  • Dodecyl dimethyoxy phosphonic heterocyclic methyl ester compound and preparation method thereof
  • Dodecyl dimethyoxy phosphonic heterocyclic methyl ester compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Example 1 In a 200ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, the air in the bottle was replaced with nitrogen, and 16.21g (0.10mol) of caged phosphoric acid ester and 80ml of diethylene glycol dimethyl ether were added. Solution, 29.06g (0.10mol) dodecyltrimethoxysilane and 0.45g dimethyl sulfate, heated up to 160°C, kept warm for 14h, then cooled to 60°C, transferred to a separatory funnel to stand for layering, Separate the lower layer of feed liquid, then add 62ml of toluene to wash, let stand to separate the lower layer of feed liquid, then distill under reduced pressure to remove toluene and a small amount of low boiling point matter, to obtain light yellow liquid dodecyl dimethoxyphosphine heterocyclic methyl ester, Product yield 87.5%, flash point (open cup): 206±5°C, decomposition temperature: 293±5°C, density (25°C): 1.713g / cm 3 , Refractive index: n D 25 = 1.4036.

Embodiment 2

[0027] Example 2 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 16.21g (0.10mol) of cage-like phosphate, 31.97g (0.11mol) of twelve Alkyl trimethoxysilane and 0.32g dimethyl sulfate, heat up to 155°C, reflux and keep warm for 16h, then cool to 60°C, add 62ml of toluene to wash, let stand 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 gave light yellow liquid dodecyl dimethoxyphosphine heterocyclic methyl ester, the product yield was 86.7%, its flash point (open cup): 206±5°C, decomposition temperature: 293±5°C, Density (25°C): 1.713g / cm 3 , Refractive index: n D 25 = 1.4036.

Embodiment 3

[0028]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 16.21g (0.10mol) of caged phosphate ester, 20mlDMF, 34.87g (0.12mol) Dodecyltrimethoxysilane and 0.49g methyl p-toluenesulfonate were heated up to 130°C, kept for 19 hours, then cooled to 60°C, transferred to a separatory funnel to stand for stratification, and the lower layer of material liquid was separated. Then add 62ml of toluene to wash, let stand to separate the lower layer feed liquid, then distill under reduced pressure to remove toluene and a small amount of low boiling point, to obtain light yellow liquid dodecyl dimethoxyphosphine heterocyclic methyl ester, the product yield is 88.2%, Its flash point (open cup): 206±5°C, decomposition temperature: 293±5°C, density (25°C): 1.713g / cm 3 , Refractive index: n D 25 = 1.4036.

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Abstract

The invention relates to a dodecyl dimethyoxy phosphonic heterocyclic methyl ester compound as a fire retardant and a preparation method thereof. The structure of the compound is shown in the following formula (as shown in the description). The preparation method comprises the following steps of under nitrogen protection, controlling the molar ratio of 4-ethyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane and dodecyl trimethoxysilane to be 1:1 to 1:1.4, and under the action of a catalyst, enabling the temperature to rise to 130-180 DEG C; and through purification treatment, obtaining products of dodecyl dimethyoxy phosphonic heterocyclic methyl ester. The dodecyl dimethyoxy phosphonic heterocyclic methyl ester compound disclosed by the invention is suitable for being used as a fire retardant of materials, polyvinyl chloride, polyurethane, unsaturated resins, epoxy resins, furan resins, polyvinyl alcohol and the like, is simple in production technology and low in equipment investment, and industrialized production is easy to realize.

Description

technical field [0001] The invention relates to a flame retardant dodecyl dimethoxyphosphine heterocyclic methyl ester compound and a preparation method thereof, in particular to a flame retardant dodecyl dimethoxy (1-oxygen-1-methyl Base-4-ethyl-1-phospha-2,6-dioxa-cyclohexyl-<4>-methoxy)silane compound and preparation method thereof, the compound contains phosphorus and silicon dual flame retardant elements , Phosphorus-silicon synergy has a high flame-retardant performance, suitable for use as a flame retardant for polyvinyl chloride, polyurethane, unsaturated resin, epoxy resin, furan resin, polyvinyl alcohol and other materials. Background technique [0002] With the successive promulgation of increasingly stringent flame retardant regulations, fire safety standards and industry directives around the world, the demand for flame retardants is also increasing. In recent years, the global market demand for flame retardants has shown a rapid growth trend, especially f...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08L67/06C08K5/5435
CPCC07F9/657181C08K5/5435C08L2201/02C08L67/06
Inventor 王彦林贺婧李果
Owner SUZHOU UNIV OF SCI & TECH
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