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Phenyl dimethoxyphosphine heterocyclic methyl silicate compound and preparation method thereof

A flame retardant technology of phenyldimethoxyphosphine silicate and heterocyclic methyl ester, which is applied in chemical instruments and methods, compounds of elements of Group 5/15 of the periodic table, organic chemistry, etc., to prevent melting and dripping , small mechanical properties, good dispersion effect

Active Publication Date: 2018-04-27
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when phosphorus-based or silicon-based flame retardants are used alone, there will be some defects. The combination of the two flame retardants will produce better results. If the phosphorus and silicon flame-retardant elements are designed into the same molecule , Phosphorus and silicon flame retardant elements are compounded in the molecule, and it will be easier to exert the synergistic flame retardant synergistic effect of phosphorus and silicon, so that the product can obtain high-efficiency flame retardants with superior flame retardant properties of both

Method used

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  • Phenyl dimethoxyphosphine heterocyclic methyl silicate compound and preparation method thereof
  • Phenyl dimethoxyphosphine heterocyclic methyl silicate compound and preparation method thereof
  • Phenyl dimethoxyphosphine heterocyclic methyl silicate compound and preparation method thereof

Examples

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Effect test

Embodiment 1

[0028] Example 1 In a 150ml 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, 80ml of diethylene glycol dimethyl ether Solution, 27.76g (0.14mol) phenyltrimethoxysilane and 0.49g dimethyl sulfate, heated up to 155°C, kept the temperature for 13h, then cooled to 60°C, transferred to a separatory funnel to stand for stratification, separated Add 35ml of toluene to the lower layer of feed liquid, 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 matter to obtain light yellow liquid phenyl dimethoxyphosphine heterocyclic methyl silicate, the product is The rate is 89.0%, its flash point (open cup): 210±5°C, decomposition temperature: 300±5°C, density (25°C): 1.762g / cm 3 , Refractive index: n D 25 = 1.4023.

Embodiment 2

[0029] Example 2 In a 100ml 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 phosphoric acid ester, 19.83g (0.10mol) of phenyl Trimethoxysilane and 0.32g dimethyl sulfate, heat up to 130°C, keep warm for 16h, then cool to 60°C, add 35ml 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 The product was obtained as a pale yellow liquid phenyl dimethoxyphosphine heterocyclic methyl silicate, the product yield was 81.4%, its flash point (open cup): 210±5°C, decomposition temperature: 300±5°C, density (25 °C): 1.762g / cm 3 , Refractive index: n D 25 = 1.4023.

Embodiment 3

[0030]Example 3 In a 150ml 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, 60mlDMF, 23.80g (0.12mol) Phenyltrimethoxysilane and 0.45g methyl p-toluenesulfonate, heat up to 140°C, keep warm for 14h, then cool to 60°C, transfer to a separatory funnel to stand for stratification, separate the lower layer of material liquid, and then add Wash with 35ml of toluene, 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 substances to obtain light yellow liquid phenyl dimethoxyphosphine heterocyclic methyl silicate, the product yield is 86.8%. Point (open cup): 210±5°C, decomposition temperature: 300±5°C, density (25°C): 1.762g / cm 3 , Refractive index: n D 25 = 1.4023.

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Abstract

The invention relates to a phosphorus and silicon synergistic flame retardant phenyl dimethoxy silicate phosphonic heterocyclic methyl ester compound and a preparation method thereof. The structural formula of the compound is shown in the specification. The preparation method comprises the steps that under the protection of nitrogen, the molar ratio of 4-ethyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane and phenyl trimethoxy silane ranges from 1:1 to 1:1.4, under the action of a catalyst, the temperature is increased to range from 120 DEG C to 180 DEG C, heat-retaining reaction is conducted for 12-17 h, and a product of phenyl dimethoxy silicate phosphonic heterocyclic methyl ester is obtained after purification treatment is conducted. The phenyl dimethoxy silicate phosphonic heterocyclic methyl ester compound is suitable for being used for a flame retardant of materials such as polyester PBT, PET, polyvinyl chloride, PC, polyurethane, unsaturated resin and epoxy resin, the production technology is simple, the equipment investment is low, industrial production is easy to achieve, and a good development and application prospect is achieved.

Description

technical field [0001] The invention relates to a phosphorus-silicon synergistic flame retardant phenyl dimethoxyphosphine heterocyclic methyl silicate compound and a preparation method thereof, in particular to a phosphorus-silicon synergistic flame retardant phenyl dimethoxy (1-oxygen -1-methyl-4-ethyl-1-phospha-2,6-dioxa-cyclohexyl-<4>-methoxy)silane compound and its preparation method, the compound contains phosphorus, silicon Dual flame retardant elements, phosphorus and silicon synergistically have high flame retardant performance, suitable for use as flame retardants for polyester PBT, PET, PC, polyurethane, epoxy resin and other materials. Background technique [0002] Because most of the polymer materials widely used in various aspects of people's lives are flammable, the fires caused by them are also very frequent, which poses a great threat to people's life and property safety. With the continuous development of science and technology and the continuous enh...

Claims

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Application Information

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