The preparation method of methylphenylmethoxy (phosphacyclomethoxy) silane compound

A technology of methyl phenyl methoxy and silane compounds is applied in the field of preparation of flame retardant methyl phenyl methoxy silane compounds, which can solve problems such as causing fire, threats to life and property safety, and prevent melting and dripping. , to promote the flame retardant effect, the effect of small mechanical properties

Active Publication Date: 2017-12-22
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The advancement of science and technology has promoted the rapid development of the polymer industry. The consumption of organically synthesized polymer materials has become an important indicator to measure the development of a country or region. However, most polymer materials are flammable and often cause fires. People's life and property safety is seriously threatened, fire prevention has attracted great attention, and the flame retardant rate of synthetic polymer materials has become a new standard to measure whether a country or region is developed, thus greatly promoting flame retardant materials and flame retardant technology. improvement

Method used

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  • The preparation method of methylphenylmethoxy (phosphacyclomethoxy) silane compound
  • The preparation method of methylphenylmethoxy (phosphacyclomethoxy) silane compound
  • The preparation method of methylphenylmethoxy (phosphacyclomethoxy) silane compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 In a 150ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, replace the air in the bottle with nitrogen, and add 19.4g (0.10mol) of 4-hydroxymethyl-4-ethyl-cycloformazol base phosphonate, 18.23g (0.10mol) methylphenyldimethoxysilane and 40ml diethylene glycol dimethyl ether, the temperature is raised to 140°C, the temperature at the top of the fractionation column is controlled to be no higher than 65°C, and the generated Methanol, react for 6h, after no methanol is produced, change it to a vacuum distillation device, diethylene glycol dimethyl ether (recycled) is removed by vacuum distillation, then add 35ml of toluene, stir for 20min, transfer to a separatory funnel to statically Set the layers, separate the lower layer feed liquid, and remove a small amount of toluene and low boiling point substances by distillation under reduced pressure to obtain a light yellow liquid methylphenylmethoxy (phosphacyclometho...

Embodiment 2

[0025] Example 2 In a 200ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, replace the air in the bottle with nitrogen, and add 19.4g (0.10mol) of 4-hydroxymethyl-4-ethyl-cycloformazol base phosphonate, 23.70g (0.13mol) methylphenyldimethoxysilane and 50ml tetrachloroethane, the temperature is raised to 120°C, the temperature at the top of the fractionation column is controlled to be no higher than 65°C, and the generated methanol is fractionated, and the reaction 8h, after no methanol was produced, it was changed to a vacuum distillation device, and tetrachloroethane (recycled) was removed by vacuum distillation, then 70ml of toluene was added, stirred for 20min, transferred to a separatory funnel to stand for stratification, and separated The lower layer of feed liquid, a small amount of toluene and low boiling point substances were removed by distillation under reduced pressure to obtain light yellow liquid methylphenylmet...

Embodiment 3

[0026] Example 3 In a 150ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, replace the air in the bottle with nitrogen, and add 19.4g (0.10mol) of 4-hydroxymethyl-4-ethyl-cycloformazol Base phosphonate, 20.05g (0.11mol) methylphenyldimethoxysilane and 20ml DMF, heat up to 130°C, control the temperature at the top of the fractionation column to not be higher than 65°C, fractionate the generated methanol, and fractionate for 7h. After no methanol is produced, change it to a vacuum distillation device, and remove DMF (recovery and use) by distillation under reduced pressure, then add 45ml of toluene, stir for 20min, transfer to a separatory funnel to stand for layering, separate the lower layer of feed liquid, and reduce A small amount of toluene and low boiling point substances were removed by pressure distillation to obtain light yellow liquid methylphenylmethoxy (phosphacyclomethoxy) silane, the product yield was 85.5%, and i...

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Abstract

The present invention relates to a kind of preparation method of flame retardant methylphenylmethoxy (phosphacyclomethoxy) silane compound, the structure of the compound is shown in the following formula: the preparation method is: under the protection of nitrogen, add an organic solvent, Then add 1-oxygen-1-methyl-4-ethyl-4-hydroxymethyl-2, 6-dioxa-1-phosphorinane and methylphenyldimethoxysilane to control its The molar ratio is 1:1-1:1.4, the temperature is raised to 100-140°C, the temperature at the top of the fractionation column is controlled not to be higher than 65°C, and the generated methanol is fractionated, and the fractionation reaction is 6-10h until the fractionated methanol reaches the theoretical amount. The reaction is stopped, and after purification treatment, methylphenylmethoxyl (phosphacyclomethoxyl) silane is obtained; the product of the present invention has high flame retardancy, good compatibility with macromolecules, and is suitable for use as polyvinyl chloride, polyurethane, Flame retardant for polyester, unsaturated resin, epoxy resin, furan resin, polyvinyl alcohol and other materials. The preparation process is simple, the equipment investment is small, the large-scale production is easy, and the application and development prospects are very good.

Description

technical field [0001] The present invention relates to a kind of preparation method of flame retardant methylphenylmethoxyl (phosphacyclomethoxy) silane compound, in particular to a kind of flame retardant methylphenylmethoxyl (1-oxygen-1- Method for preparing methyl-4-ethyl-1-phospha-2,6-dioxa-cyclohexyl-<4>-methoxy)silane compound. The compound contains two flame retardant elements, phosphorus and silicon. Phosphorus and silicon synergistically have high flame retardant properties, and are suitable for polyvinyl chloride, polyurethane, polyester, unsaturated resin, epoxy resin, furan resin, polyvinyl alcohol, etc. Flame retardant for materials. Background technique [0002] The advancement of science and technology has promoted the rapid development of the polymer industry. The consumption of organically synthesized polymer materials has become an important indicator to measure the development of a country or region. However, most polymer materials are flammable an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6571
Inventor 王彦林侯宁李果
Owner SUZHOU UNIV OF SCI & TECH
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