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Preparation method of pentamethyldisiloxane

A technology of pentamethyldisiloxane and dimethylhalosilane, which is applied in the field of preparation of high-purity pentamethyldisiloxane to achieve the effects of no by-products, single product and high yield

Inactive Publication Date: 2016-10-26
ZHENJIANG SINOWA POLYURETHANE EQUIP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, in order to achieve the purpose of obtaining a higher purity sample (such as 98%), it is necessary to carry out multiple rectification purifications, and the yield of the final product will be reduced to less than 10% from 50% of the initial yield of the reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Tetrahydrofuran was used as the solvent in the reaction, and the two reactants of potassium trimethylsiliconate and dimethyl-hydrogen-chloride were added to the above-mentioned solvent at a molar ratio of 1:1 at the same flow rate. Stir vigorously until the pH value of the solution reaches 6, stop adding the reactants, and pay attention to controlling the addition speed of the two raw materials during the process, so that the two raw materials are always added to the reaction system at a roughly equimolar speed. After the addition of the two is completed, reflux for a short time and the reaction ends. The product system is filtered to remove potassium chloride, purified by rectification, and tetrahydrofuran is removed to obtain more than 98% of pentamethyldisiloxane products.

Embodiment 2

[0021] Example 2: Tetrahydrofuran was used as a solvent in the reaction, and the two reactants of potassium trimethylsiliconate and dimethyl-hydrogen-chloride were added to the above-mentioned solvent at a molar ratio of 1:1 at the same flow rate. Stir vigorously, and stop adding reactants when the pH value of the solution reaches 4. During the process, pay attention to controlling the addition speed of the two raw materials so that the two raw materials are always added to the reaction system at a roughly equimolar speed. After the addition of the two is completed, reflux for a short time and the reaction ends. The product system is filtered to remove potassium chloride, purified by rectification, and tetrahydrofuran is removed to obtain more than 97% of pentamethyldisiloxane products.

Embodiment 3

[0022] Example 3: Tetrahydrofuran was used as the solvent in the reaction, and the two reactants of potassium trimethylsiliconate and dimethyl-hydrogen-chloride were added to the above-mentioned solvent at a molar ratio of 1:1 at the same flow rate, and during the addition process Stir vigorously until the pH value of the solution reaches 7, stop adding the reactants, and pay attention to controlling the addition speed of the two raw materials during the process, so that the two raw materials are always added to the reaction system at a roughly equimolar speed. After the addition of the two is completed, reflux for a short time and the reaction ends. The product system is filtered to remove potassium chloride, purified by rectification, and tetrahydrofuran is removed to obtain more than 97% of pentamethyldisiloxane products.

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Abstract

The invention discloses a preparation method of pentamethyldisiloxane. The method comprises the steps that alkanes and ethers are selected as a solvent, two reactants of alkali metal silicon alkoxide and a dimethyl halogenosilane compound are added into the above-mentioned solvent according to the molar ratio of 1:1 at uniform velocity, vigorous stirring is conduced during the adding process, adding of the reactants is stopped when the PH value of the solution is between 4 and 7, filtration and rectification are conducted, and a product of which the purity is larger than 97% is obtained. Industrial production is achieved, and a huge market prospect and economic value are achieved.

Description

technical field [0001] The invention relates to a preparation method for high-purity pentamethyldisiloxane. Background technique [0002] 1,1,1,3,3-Pentamethyldisiloxane is a common organopolysiloxane characterized by the asymmetry of the functional groups on the two silicons. In its molecular structure, there is an active hydrogen, which allows the molecule to link with other compounds. Since the compound is limited to a small amount of application in medicine and scientific research, there is no large-scale industrial production method. [0003] The existing small-batch preparation method is a chemical equilibrium method, and the specific process is as follows: equimolar trimethylchlorosilane (or hexamethyldisiloxane), dimethylhydrogenmonochlorosilane (or tetramethyldisiloxane) Hydrogen disiloxane) in the presence of a small amount of water and concentrated sulfuric acid, chemical rearrangement can be obtained containing pentamethyldisiloxane (1), tetramethyldisiloxane (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08C07F7/20
CPCC07F7/0896C07F7/20
Inventor 徐应刚
Owner ZHENJIANG SINOWA POLYURETHANE EQUIP
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