Production method of tetramethyl divinyl disiloxane

A technology of tetramethyldivinyldisiloxane and vinyldimethylethoxysilane, which is applied in the production field of tetramethyldivinyldisiloxane, can solve the problem of easy burning, unsafe, Vinyl chloride is toxic and other problems, achieving the effect of reducing three wastes, reducing production costs, and good safety

Inactive Publication Date: 2012-03-28
衢州瑞力杰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because metal sodium is used in production, it is easy to burn when it encounters humid air and water, which is unsafe; the vinyl chloride used is also poisonous

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Take 2.63mol of magnesium and 800mL of anhydrous ether solvent of alkanes respectively, add to a cooler equipped with dry ice and feed N 2 Into the flask with dry nitrogen, add methyl bromide dropwise, react to form methyl magnesium bromide, evaporate excess methyl bromide, and then drop vinyltriethoxysilane into methyl magnesium bromide under stirring 510g (2.68mol) and ether 900ml solution. The reaction was refluxed for one hour and the ether was distilled off. Then, distill off the fraction before 70°C, and distill off the silane mixture at 5.3kPa. Then, by fractional distillation at atmospheric pressure, the refractive index nD was collected 20 1.3983; density d 20 0.790; b.p 93 ~ 99 ° C fraction, vinyl dimethyl ethoxy silane.

[0010] Take 20.9 g of vinyl dimethyl ethoxysilane prepared above, 100 ml of acetone, 10 ml of 0.1 mol / L hydrochloric acid, and reflux for four hours. After distilling off the acetone, get a two-phase raffinate, remove the non-aqueous ph...

Embodiment 2

[0012] Get the xylene solvent 800ml of magnesium 64g and alkanes respectively, add and be equipped with reflux cooler, dry ice cooler and pass into N 2 In the 3000ml flask of tube, pass into dry nitrogen therein, dropwise add methyl bromide 100g under stirring, react to form methylmagnesium bromide, excess methyl bromide is evaporated. Then, the mixture of 510 g (2.68 mol) of vinyltriethoxysilane and 800 ml of xylene was added dropwise into the xylene solution of methylmagnesium bromide under stirring, and the reaction was refluxed for two hours after the addition was completed. Then, by fractional distillation at atmospheric pressure, the refractive index nD was collected 20 1.3983; density d 20 0.790; b.p 93 ~ 99 ° C fraction, vinyl dimethyl ethoxy silane.

[0013] Take 20.9 g of vinyldimethylethoxysilane prepared above, 100 ml of acetone, 10 ml of 0.1 mol / L hydrochloric acid, and reflux for four hours. After distilling off the acetone, get a two-phase raffinate, remove t...

example 3

[0015] Get respectively the sherwood oil of magnesium 64g and alkane (main component is Hexane ) solvent 800ml, add reflux cooler, dry ice cooler and pass into N 2 In the 3000ml flask of tube, pass into dry nitrogen therein, dropwise add methyl bromide 100g under stirring, react to form methylmagnesium bromide, excess methyl bromide is evaporated. Then, under stirring, a mixture of 510 g (2.68 mol) of vinyltriethoxysilane and 800 ml of petroleum ether was added dropwise into the petroleum ether solution of methylmagnesium bromide, and the reaction was refluxed for two hours after the addition was completed. Then, by fractional distillation at atmospheric pressure, the refractive index nD was collected 20 1.3983; density d 20 0.790; b.p 93 ~ 99 ° C fraction, vinyl dimethyl ethoxy silane.

[0016] Take 20.9 g of vinyldimethylethoxysilane prepared above, 100 ml of acetone, and 10 ml of 0.1 mol / L hydrochloric acid, and reflux for four hours. After distilling off the acetone, g...

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Abstract

The invention relates to a production method of tetramethyl divinyl disiloxane. The method comprises the following steps of: mixing and dissolving magnesium and bromomethane in an alkane solvent under a protection condition of dry nitrogen to prepare Grignard reagent; making the Grignard reagent further react with vinyl triethoxy silane to prepare vinyl dimethyl ethyoxyl silane; and then carryingout hydrolysis to generate the tetramethyl divinyl disiloxane. In the production method, the magnesium does not react with water at a normal temperature and is safer than metal sodium in use; the vinyl triethoxy silane is used, so the method is more environment-friendly than the prior process using chloroethylene; in addition, the method carries out reaction in the solvent under the protection ofthe dry nitrogen and has high yield and good safety; and simultaneously ethanol magnesium and bromine ethanol generated in the reaction can be recycled so as to reduce the production cost and reduce three wastes.

Description

technical field [0001] The invention relates to a production method of tetramethyldivinyldisiloxane. Background technique [0002] Generally, the method for producing tetramethyldivinyldisiloxane is: using the basic organosilicon chemical raw material dimethyldiethylsilane, under the action of metal sodium, reacting vinyl chloride to generate dimethylvinylethoxy base silane and sodium salt, and then hydrolyze dimethyl vinyl ethoxy silane in one step to obtain tetramethyl divinyl disiloxane, and evaporate the resulting sodium salt to dryness at high temperature before packaging. Because metal sodium needs to be used in production, it is easy to burn when it encounters humid air and water, which is unsafe; the vinyl chloride used is also poisonous. Contents of the invention [0003] The purpose of the present invention is to provide a kind of production method of tetramethyldivinyldisiloxane with high safety and environmental protection. [0004] The technical scheme adopt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08
Inventor 吕起余金全刘登政
Owner 衢州瑞力杰化工有限公司
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