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
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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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