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Preparation method of flame retardant alkyl dimethoxy (phosphacyclomethoxy) silane compound

A technology of flame retardant alkyl dimethoxy and alkyl trimethoxy silane is applied in the field of preparation of flame retardant alkyl dimethoxy silane compound, which can solve the development limitation and electrical performance of silicon-based flame retardants. Poor, expensive and other problems, to achieve the effect of novel preparation method, good compatibility and good plasticity

Active Publication Date: 2017-11-24
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, there are many studies on phosphorus-based flame retardants, but traditional organophosphorus flame retardants still have problems such as high polarity, easy migration, and poor electrical performance; silicon-based flame retardants are a new type of halogen-free flame retardants , has the advantages of high efficiency, non-toxic, low smoke, anti-dripping, no pollution, etc., but due to problems such as high price, the development of silicon-based flame retardants has been limited to a certain extent

Method used

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  • Preparation method of flame retardant alkyl dimethoxy (phosphacyclomethoxy) silane compound
  • Preparation method of flame retardant alkyl dimethoxy (phosphacyclomethoxy) silane compound
  • Preparation method of flame retardant alkyl dimethoxy (phosphacyclomethoxy) silane compound

Examples

Experimental program
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Effect test

Embodiment 1

[0030] 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 19.40g (0.10mol) of 4-hydroxymethyl-4-ethyl-cycloformazol Base phosphonate, 13.62g (0.10mol) methyl trimethoxysilane, 40ml diethylene glycol dimethyl ether, heat up to 100 ° C, control the fractionation column top temperature is not higher than 65 ° C, fractionate the generated methanol, and react 8h, after no methanol is produced, change it to a vacuum distillation device, and diethylene glycol dimethyl ether (recycled) is removed by vacuum distillation, then add 30ml of toluene to stir and wash, transfer to a separatory funnel to stand for stratification, Separate the lower layer of feed liquid, and distill under reduced pressure to remove toluene and a small amount of low boiling point substances to obtain methyl dimethoxy (phosphacyclomethoxy) silane. The product yield is 95.5%, and its flash poi...

Embodiment 2

[0031] Example 2 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 19.40g (0.10mol) of 4-hydroxymethyl-4-ethyl-cycloformazol Base phosphonate, 17.71g (0.13mol) methyltrimethoxysilane, 75ml ethylene glycol diethyl ether, raise the temperature to 80°C, control the temperature at the top of the fractionation column to not be higher than 65°C, fractionate the generated methanol, and react for 11h. After no methanol is produced, change it to a vacuum distillation device, and remove ethylene glycol diethyl ether (recycled) by vacuum distillation, then add 30ml of toluene to wash, transfer to a separatory funnel to stand for stratification, and separate the lower layer of feed liquid , toluene and a small amount of low boiling point were removed by distillation under reduced pressure to obtain methyl dimethoxy (phosphacyclomethoxy) silane, the product yield was 90.6%, its ...

Embodiment 3

[0032] 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 19.40g (0.10mol) of 4-hydroxymethyl-4-ethyl-cycloformazol Base phosphonate, 14.98g (0.11mol) methyltrimethoxysilane, 50ml DMF, heat up to 110°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 6 hours until no methanol is produced Afterwards, change it into a vacuum distillation device, and remove DMF (recovery and use) by distillation under reduced pressure, then add 30ml of toluene to wash, transfer to a separatory funnel to stand for layering, separate the lower floor material liquid, and remove toluene and a small amount of toluene by distillation under reduced pressure. Low boiling point, get methyl dimethoxy (phosphacyclomethoxy) silane, product yield 86.5%, its flash point (open cup): 204 ± 5 ​​℃...

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Abstract

The invention relates to a preparation method of an alkyl - dimethoxy (phosphorus heterocycle) silane compound as a fire retardant. The structure of the compound is shown in the following formula (as shown in the description), wherein R is equal to methyl, ethyl, propyl or butyl. The preparation method comprises the following steps of using nitrogen for replacing air in a reactor, controlling the molar ratio of 1-oxo methyl-4-ethyl -4-methylol-2,6-dioxa-1-phosphorus heterocycle hexane to alkyl group trimethoxysilane to be 1:1 to 1:1.4, and performing a reaction at 80-130 DEG C in an organic solvent; controlling the top temperature of a fractionating column to be equal to or lower than 65 DEG C, and performing a fractional distillation reaction for 6-13 hours until no methanol is generated; and through purification treatment, obtaining alkyl-dimethoxy (phosphorus heterocycle) silane. The product disclosed by the invention is high in flame resistant efficiency, good in carbon forming performance, good in plasticity, and suitable for being used as the fire retardant of materials of polyester PBT, PET, polyurethane, unsaturated resins, epoxy resins, polyvinyl chloride and the like. The production technology is simple, the equipment investment is low, and the industrialized production is easy to realize.

Description

technical field [0001] The present invention relates to a kind of preparation method of flame retardant alkyl dimethoxyl (phosphacyclomethoxy) silane compound, in particular to a kind of flame retardant alkyl dimethoxyl (1-oxo-1-methyl - Preparation method of 4-ethyl-1-phospha-2,6-dioxa-cyclohexyl-<4>-methoxy)silane compound. The compound contains dual flame retardant elements of phosphorus and silicon, and phosphorus and silicon synergistically have higher flame retardant performance. It is suitable for use as a flame retardant for polyester PBT, PET, polyurethane, unsaturated resin, epoxy resin, polyvinyl chloride and other materials . Background technique [0002] With the rapid development of science and technology, synthetic polymer materials have been widely used, which brings great convenience to people's life and also brings great fire hazards due to their flammability, which promotes the development of flame retardant science and technology. The rapid develo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08L67/02C08K5/5435
CPCC07F9/657181C08K5/5435C08L2201/02C08L67/02
Inventor 王彦林陈秀丽李果
Owner SUZHOU UNIV OF SCI & TECH
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