Method for industrially producing dialkyl dialkoxy silane

A technology of dihydrocarbyl dialkoxysilane and hydrocarbyl trialkoxysilane is applied in the field of industrial production of dihydrocarbyl dialkoxysilane, and can solve the problems of low reaction activity, many by-products, and high cost, and reduce production costs. , the effect of reducing by-products and improving yield

Active Publication Date: 2020-04-07
HUBEI HUABANG CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome above-mentioned technical deficiency, propose a kind of method of industrial production dihydroc

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  • Method for industrially producing dialkyl dialkoxy silane

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Experimental program
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Effect test

Embodiment 1

[0044] Under nitrogen protection, 54kg magnesium chips (purity 99%, 2.25Kmol), bromoisobutane 8.4kg (purity 99%, 0.062Kmol), methyl iodide 68.4g (purity 99%, 0.48mol), tetrahydrofuran 120kg join in In a 500-liter enamel kettle A with a stirring device, a reflux condenser, a thermometer and multiple high-level dripping liquid material devices and a jacket, steam is passed through the jacket to heat the material to reflux, and the reflux is stable for 0.2 hours until the reflux flow suddenly Increase the reaction to start, stop heating and wait for the reflux to be stable, start to drop the mixture of chloroisobutane 192.6kg (purity 99%, 2.08Kmol) and tetrahydrofuran 29.4kg (purity 99%, 0.4Kmol) under stirring, Add dropwise the isobutane bromide 20.6kg (purity 99%, 0.14Kmol) in the second head tank simultaneously, adjust the rate of addition of isobutane bromide according to the remaining mixture amount in the first head tank, 1 hour After the dropwise addition was completed, th...

Embodiment 2

[0047] Under nitrogen protection, 44.6kg magnesium chips (purity 99%, 1.83Kmol), bromoisobutane 7kg (purity 99%, 0.051Kmol), methyl iodide 56.5g (purity 99%, 0.40mol), tetrahydrofuran 100kg join in In a jacketed 500-liter enamel kettle A with a stirring device, a reflux condenser, a thermometer, and multiple high-level dripping liquid material devices, the jacket is passed through steam to heat the material to reflux, and the reflux is stable for 0.1 hour, until the reflux suddenly increases. Reaction starts, stop heating and after the reflux is stable, start dropwise adding the mixture of chloroisobutane 159kg (purity 99%, 1.72Kmol) and tetrahydrofuran 25kg (purity 99%, 0.35Kmol) under stirring, add dropwise at the same time Bromoisobutane 17kg (purity 99%, 0.12Kmol) in two head tanks, adjust the rate of addition of bromoisobutane according to the remaining mixture amount in the first head tank, dropwise after 1.2 hours, keep warm Reflux for 0.8 hours.

[0048] Under the pro...

Embodiment 3

[0050] Under the protection of nitrogen, 48.6kg magnesium chips (purity 99%, 2.0Kmol), bromoisobutane 7.4kg (purity 99%, 0.054Kmol), methyl iodide 61.4g (purity 99%, 0.43mol), tetrahydrofuran 108kg were added Put it into a jacketed 500-liter enamel kettle A with a stirring device, a reflux condenser, a thermometer, and multiple high-level dripping liquid material devices. The jacket is passed through steam to heat the material to reflux, and the reflux is stable for 0.2 hours, until the reflux suddenly increases. That is, the reaction starts, stop heating and wait for the reflux to be stable, start to add dropwise the mixture of chloroisobutane 173.3kg (purity 99%, 1.87Kmol) and tetrahydrofuran 26.5kg (purity 99%, 0.37Kmol) under stirring, and drop Add the isobutane bromide 18.5kg (purity 99%, 0.135Kmol) in the second head tank, adjust the rate of addition of isobutane bromide according to the remaining mixture amount in the first head tank, drop after 1.5 hours After the addi...

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Abstract

The invention discloses a method for industrially producing dialkyl dialkoxy silane, which comprises the following steps: in the presence of a catalyst and a solvent A, heating brominated hydrocarbonA and metal magnesium to reflux, and initiating reaction to obtain a first reaction solution; synchronously and dropwise adding chlorinated hydrocarbon and brominated hydrocarbon B which are diluted by a solvent B into the first reaction solution, and continuing reaction to obtain a second reaction solution; dropwise adding the second reaction solution into alkyl trialkoxy silane, and carrying outreflux reaction to obtain a third reaction solution; and cooling the third reaction solution, carrying out solid-liquid separation, and finally, carrying out washing and rectifying to obtain the dialkyl dialkoxy silane. The Grignard reaction of the chlorinated hydrocarbon is promoted by utilizing the high activity of the brominated hydrocarbon, so that on one hand, the overall conversion rate ofthe Grignard reaction can be remarkably improved, byproducts are reduced, the yield of a final product is improved, and on the other hand, the production cost can be reduced.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for industrially producing dihydrocarbyldialkoxysilane. Background technique [0002] Dihydrocarbyldialkoxysilane is a silylating agent, which is generally used in the industry as an external electron donor for propylene polymerization catalysts to improve the stereoregularity of polymers, and can also be used in the preparation of organosilicon. [0003] At present, the synthesis process routes of dihydrocarbyldialkoxysilane mainly include the alcoholysis method of dihydrocarbyl dichlorosilane and alcohol, the Grignard reagent method of reacting Grignard reagent with hydrocarbyl trialkoxysilane, etc. Among them, the disadvantage of the alcoholysis method is that a large amount of HCl will be produced in the alcoholysis process, which will cause great harm to equipment and the environment, and the introduction of an acid-binding agent will increase the producti...

Claims

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Application Information

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IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/1876Y02P20/584
Inventor 任家君霍晓剑常贺飞毛满意邓国伟罗念白雪琴常思乔武卫华熊丽霞黄艳刚
Owner HUBEI HUABANG CHEM
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