Preparing method for phenyl dimethoxy (phosphor heterocycle methoxyl) silicane compound

A technology of phenyldimethoxy and flame retardant phenyldimethoxy, which is applied in the field of preparation of flame retardant phenyldimethoxysilane compounds, can solve the threat to life safety, poor electrical performance, use of Restriction and other problems, to achieve high decomposition temperature, promote flame retardant effect, prevent melting and dripping effect

Active Publication Date: 2015-12-23
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this kind of flame retardant will release a large amount of harmful gas when it burns, which poses a great threat to people's life safety, so the use of this kind of flame retardant will be more and more restricted in the future
At present, phosphorus-based flame retardants are the best substitutes for halogen-based flame retardants, which have the advantages of low toxicity, low smoke, and good flame-retardant effects. However, traditional organic phosphine flame retardants still have certain toxicity, high polarity, Easy migration, poor electrical performance, etc.; silicon-based flame retardants are a new type of flame retardants, which have the advantages of high flame retardant efficiency, non-toxicity, less smoke, and environmental friendliness, but their prices are high, so their use is limited

Method used

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  • Preparing method for phenyl dimethoxy (phosphor heterocycle methoxyl) silicane compound
  • Preparing method for phenyl dimethoxy (phosphor heterocycle methoxyl) silicane compound
  • Preparing method for phenyl dimethoxy (phosphor heterocycle methoxyl) silicane compound

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Example 1 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 19.40g (0.10mol) of 4-hydroxymethyl-4-ethyl-cycloformazol Base phosphonate, 19.83g (0.10mol) phenyltrimethoxysilane, 40ml diethylene glycol dimethyl ether, heat up to 140°C, control the fractionation column top temperature not higher than 65°C, fractionate the generated methanol, and react 5h, after no methanol is produced, change it to a vacuum distillation device, diethylene glycol dimethyl ether (recovered and used) is removed by vacuum distillation, then add 35ml of toluene, stir, transfer to a separatory funnel to stand for stratification, The lower layer material liquid was separated, and a small amount of toluene and low boiling point substances were removed by distillation under reduced pressure to obtain light yellow liquid phenyldimethoxy (phosphacyclomethoxy) silane with a product yield of...

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 19.40g (0.10mol) of 4-hydroxymethyl-4-ethyl-cycloformazol Base phosphonate, 25.78g (0.13mol) phenyltrimethoxysilane, 50ml ethylene glycol diethyl ether, raise the temperature to 120°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 7h. After no methanol is produced, change it to a vacuum distillation device, and remove ethylene glycol diethyl ether (recovery and use) by vacuum distillation, then add 70ml of toluene, stir, transfer to a separatory funnel to stand for stratification, and separate the lower layer of material Liquid, a small amount of toluene and low boiling point substances were distilled off under reduced pressure to obtain light yellow liquid phenyl dimethoxy (phosphacyclomethoxy) silane, and...

Embodiment 3

[0026] Example 3 In a 200ml four-necked 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, 27.76g (0.14mol) phenyltrimethoxysilane, 80ml 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, fractionate for 6 hours, and wait 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 50ml of toluene, stir, transfer to a separatory funnel and leave it to stand for layering, separate the lower floor material liquid, and remove a small amount of toluene by distillation under reduced pressure. And low boiling point, to obtain light yellow liquid phenyl dimethoxy (phosphacyclomethoxy) silane, product yield 96.8%.

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Abstract

The invention relates to a preparing method for a phosphorus-silicon synergistic flame retardant phenyl dimethoxy (phosphor heterocycle methoxyl) silicane compound. The structure of the compound is as shown in the description. The preparing method comprises the steps that under protection of nitrogen, the mole ratio of 1-oxo-1-methyl-4-ethyl-4-hydroxymethyl-2,6-dioxa-1-phosphorinane to phenyl trimethoxy silane is controlled to be 1:1-1:1.4, organic solvent is added, temperature is raised to 100 DEG C-140 DEG C, the temperature of a fractional distillation column top is controlled to be not higher than 65 DEG C, generated methyl alcohol is distilled, the fractional distillation reaction is carried out for 5-9 h, the reaction is not stopped until the quantity of methyl alcohol distilled reaches the theory amount, and purification is carried out to obtain phenyl dimethoxy (phosphor heterocycle methoxyl) silicane. The compound is suitable for serving as flame retardant of materials such as polyvinyl chloride, polyurethane, unsaturated polyester resin, epoxy resin, furan resin and polyvinyl alcohol, the production technology is simple, equipment investment is small, industrialized production is achieved easily, and the compound has good application and development prospects.

Description

technical field [0001] The present invention relates to a kind of preparation method of flame retardant phenyl dimethoxy (phosphacyclomethoxy) silane compound, in particular to a kind of flame retardant phenyl dimethoxy (1-oxo-1-methyl - the preparation method of 4-ethyl-1-phospha-2,6-dioxa-cyclohexyl-<4>-methoxy)silane compound, which belongs to phosphorus and silicon synergistic flame retardant, suitable for Used as a flame retardant for polyester PBT, PET, polyurethane, unsaturated resin, epoxy resin and other materials. Background technique [0002] With the advancement of science and technology, polymer materials have been used more and more widely. While it brings great convenience to people's lives, it also brings new fire threats due to its flammability, which promotes the flame retardant industry. rapid development. At present, a large number of halogenated flame retardants are used, which have good flame retardant effect and wide application range, and can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6571C07F9/6574C08K5/5419C08L67/06
Inventor 王彦林袁文常李果
Owner SUZHOU UNIV OF SCI & TECH
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