Method for directly synthesizing dialkyl dialkoxy silicane by one-step process

The technology of dialkyl dialkoxy silane and tetraalkoxy silane is applied in the field of synthesis of dialkyl dialkoxy silane and can solve the problem of raw material damage loss, low reaction efficiency and solvent circulation of tetraalkoxy silane. Difficulty in use, etc.

Active Publication Date: 2008-07-23
山东鲁晶化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] In order to overcome the deficiencies of the prior art, the present invention provides a method for directly synthesizing dialkyldialkoxysilane in one step, so as to solve the difficulty of industrial implementation of the above synthesis method, excessive molar ratio, high production cost and low reaction efficiency. , Solvent recycling is difficult, tetraalkoxysilane raw materials are easily damaged and lost, etc.

Method used

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  • Method for directly synthesizing dialkyl dialkoxy silicane by one-step process
  • Method for directly synthesizing dialkyl dialkoxy silicane by one-step process
  • Method for directly synthesizing dialkyl dialkoxy silicane by one-step process

Examples

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Effect test

example 1

[0048] Example 1. Preparation of dicyclopentyldimethoxysilane

[0049] Replace air with nitrogen in a 2000ml four-necked flask equipped with electric stirrer, thermometer, reflux condenser, and constant pressure dropping funnel, and drop 60.4g (purity 99%, 2.46mole) particle size less than 150 purpose magnesium powder, 40g (purity 99%, 0.38mole) chlorocyclopentane, 180g (purity 99%, 1.17mole) tetramethoxysilane, add 224g (purity 99%, 2.12 mole) the mixed solution of chlorocyclopentane and 400ml methyl-tert-butyl ether. Nitrogen was passed through the reaction system again, two grains of iodine were added to the reactant in the reaction bottle, and then heated to about 55°C, the reaction was violently initiated, and a large amount of reaction heat was released. When the exothermic reaction is initiated for 2 to 3 minutes, add the mixture in the dropping funnel to the reaction bottle dropwise within 20 to 30 minutes, keep the reactants under a relatively vigorous reflux, and th...

example 2

[0051] Example 2. Preparation of diisopropyldimethoxysilane

[0052] Replace the air with nitrogen in a 500ml four-necked flask equipped with an electric stirrer, a thermometer, a reflux condenser, and a constant pressure dropping funnel, and drop 15g (purity 99%, 0.61mole) into the reaction bottle under a nitrogen atmosphere, and the particle size is less than 150 Purpose magnesium powder, 11.9g (purity 99%, 0.096mole) bromoisopropane, 44.5g (purity 99%, 0.29mole) tetramethoxysilane, in constant pressure dropping funnel, add 64.8g (purity 99%, 0.52mole) a mixture of bromoisopropane and 100ml methyl-tert-butyl ether. Nitrogen was passed through the reaction system again, a grain of iodine was added to the reactant in the reaction bottle, and then heated to raise the temperature, the reaction was violently triggered, and a large amount of reaction heat was released. When the exothermic reaction is initiated for 2-3 minutes, add the mixture in the dropping funnel dropwise to th...

example 3

[0054] Example 3. Preparation of diisobutyldimethoxysilane

[0055] The preparation process is the same as that of Example 2, except that isopropane bromide is replaced by equimolar chloroisobutane to obtain 54.2 g of diisobutyldimethoxysilane with a purity of 99.5% and a yield of 91.2% (according to tetramethoxy Silane), 85.5% (based on chloroisobutane).

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Abstract

The invention discloses a method, which is characterized in that: reactant 4-alkoxy silicane is used as solvent; grignard reaction is firstly caused by alkyl halide with small amount and metal magnesium powder with particle size less than 150 mesh; then alkyl halide diluted by ethers or hydrocarbon solvent is added through dropping; the preparation method for grignard reagent at the spot enables the grignard reaction and synthesis reaction of dialkyl dialkoxy silicane to be made in the same vessel at the same time, thereby directly synthesizing dialkyl dialkoxy silicane by one step; solid substance separated from reaction suspension is washed using dispersing agent; the filtrate and the lotion are fractionated, thereby getting dispersing agent and reactant successively and finally getting dialkyl dialkoxy silicane with the content of bigger than 99.5%. The preparation method of Grignard reagent at the spot has an advantage of realizing ideal result of more than 85% of product yield and more than 99.5% of product content.

Description

technical field [0001] The invention belongs to the technical field of chemistry and relates to a method for synthesizing dialkyldialkoxysilane. [0002] Specifically, the reactant tetraalkoxysilane is used as a solvent. In the presence of a catalyst, a small amount of haloalkane and metal magnesium powder are used to initiate the Grignard reaction, and then the haloalkane diluted with a hydrocarbon or ether solvent is added dropwise. A method for synthesizing dialkyldialkoxysilane in one step by reacting reagent with tetraalkoxysilane. Background technique [0003] The general formula is [0004] [0005] The main function of the dialkyldialkoxysilane is as an external electron donor and stereoconfiguration modifier for high-efficiency Ziegler-Natta catalysts. In the α-olefin polymerization reaction, they cooperate with the internal electron donor of the catalyst to significantly improve the isotacticity and physical and mechanical properties of the α-olefin polymer. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 黄学才陈旭马殿伟
Owner 山东鲁晶化工科技有限公司
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