The preparation method of dodecyl dimethoxy (phosphacyclomethoxy) silane compound

A technology of dodecyl dimethoxy and silane compounds is applied in the field of preparation of flame retardant dodecyl dimethoxy silane compounds, which can solve the problem of slow development, poor electrical performance, and ease of use of silicone flame retardants. Migration and other problems, to achieve the effect of small mechanical properties, no pollution of three wastes, and stable physical and chemical properties

Active Publication Date: 2018-02-02
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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  • The preparation method of dodecyl dimethoxy (phosphacyclomethoxy) silane compound
  • The preparation method of dodecyl dimethoxy (phosphacyclomethoxy) silane compound
  • The preparation method of dodecyl dimethoxy (phosphacyclomethoxy) silane compound

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Example 1 In a 200ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, the air in the flask was replaced with nitrogen, and 19.40g (0.10mol) 4-hydroxymethyl-4-ethyl-cyclomethan was added. Base phosphonate, 29.05g (0.10mol) dodecyltrimethoxysilane, 80ml diethylene glycol dimethyl ether, heat up to 140℃, control the top temperature of the fractionation column to be not higher than 65℃, and fractionate the methanol produced After reacting for 6h, when no methanol is produced, change to a vacuum distillation device, distill off diethylene glycol dimethyl ether (recycled) under reduced pressure, then add 50ml of toluene, stir for 20min, and transfer to a separatory funnel to stand still Separate the lower layer of the liquid, and distill under reduced pressure to remove a small amount of toluene and low boiling point substances to obtain a light yellow liquid dodecyl dimethoxy (phosphorheterocyclic methoxy) silane. The produc...

Embodiment 2

[0022] Example 2 In a 200ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency fractionation device, the air in the flask was replaced with nitrogen, and 19.40g (0.10mol) 4-hydroxymethyl-4-ethyl-cyclomethan was added. Base phosphonate, 37.77g (0.13mol) dodecyltrimethoxysilane, 100ml ethylene glycol diethyl ether, heat up to 120℃, control the top temperature of the fractionation column to be not higher than 65℃, fractionate the methanol produced, and react After 9h, when no methanol is produced, change to a vacuum distillation device, distill out ethylene glycol diethyl ether under reduced pressure (recovered and used), then add 80ml of toluene, stir for 20min, transfer to a separatory funnel and let stand for layering. Take out the lower layer of liquid, and distill under reduced pressure to remove a small amount of toluene and low boiling point substances to obtain a light yellow liquid dodecyl dimethoxy (phosphorheterocyclic methoxy) silane. The pr...

Embodiment 3

[0023] Example 3 In a 200ml four-necked flask equipped with a stirrer, a thermometer and a high-efficiency fractionation device, the air in the flask was replaced with nitrogen, and 19.40g (0.10mol) 4-hydroxymethyl-4-ethyl-cyclomethan was added. Phosphonate, 40.67g (0.14mol) dodecyltrimethoxysilane, 60ml DMF, heat up to 130℃, control the top temperature of the fractionation column to be not higher than 65℃, fractionate the methanol produced, and react for 8h. After no methanol is produced, change to a vacuum distillation device, distill out DMF under reduced pressure (recovered and used), then add 70ml of toluene, stir for 20min, transfer to a separatory funnel, stand still for stratification, separate the lower layer of liquid, reduce pressure A small amount of toluene and low boiling point substances are removed by distillation to obtain a light yellow liquid dodecyl dimethoxy (phosphorheterocyclic methoxy) silane. The yield of the product is 97.6%. Its flash point (open cup):...

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Abstract

The invention relates to a preparation method of a flame retardant dodecyl dimethoxy (phosphacyclomethoxy) silane compound. The structure of the compound is shown in the following formula: the preparation method is: under the protection of nitrogen, the In a reactor with a high-efficiency fractionation device, control 1-oxygen-1-methyl-4-ethyl-4-hydroxymethyl-2, 6-dioxa-1-phosphorinyl and dodecyl The molar ratio of trimethoxysilane is 1:1-1:1.4, adding an organic solvent, raising the temperature to 90-140°C, and fractionally distilling off the generated methanol. The fractional distillation reaction lasts for 6-11 hours until no methanol is produced, and is purified to obtain dodecane Dimethoxy (phosphacyclomethoxy) silane; the product of the present invention is suitable for flame retardants of materials such as polyvinyl chloride, polyurethane, unsaturated resin, epoxy resin, furan resin, polyvinyl alcohol, and production The process is simple, the equipment investment is small, the industrialized production is easy to realize, and the method has good application and development prospects.

Description

Technical field [0001] The invention relates to a preparation method of a flame retardant dodecyl dimethoxy (phosphorheterocyclic methoxy) silane compound, in particular to a flame retardant dodecyl dimethoxy (1-oxy- 1-methyl-4-ethyl-1-phospha-2,6-dioxa-cyclohexyl- <4> -Methoxy) silane compound preparation method. The compound contains two flame-retardant elements: phosphorus and silicon. Phosphorus-silicon synergistically has high flame-retardant properties and is suitable for use as a barrier for materials such as polyvinyl chloride, polyurethane, unsaturated resin, epoxy resin, furan resin, and polyvinyl alcohol. Burning agent. Background technique [0002] With the continuous promulgation of new environmental protection regulations and people's awareness of safety and environmental protection, the requirements for flame retardants and flame retardant materials are becoming higher and higher. Although traditional halogen-based flame retardants have high-efficiency flam...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/5435
Inventor 王彦林陈秀丽李果
Owner SUZHOU UNIV OF SCI & TECH
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