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Method for purifying dimethylchlorosilane by extraction and distillation

A technology of dimethylchlorosilane and methylchlorosilane, which is applied in chemical instruments and methods, silicon organic compounds, compounds of group 4/14 elements of the periodic table, etc., can solve low-boiling mixtures that cannot be directly applied to organosilicon Separation and purification and other issues to achieve the effect of easy separation, increased relative volatility, and easy rectification separation

Active Publication Date: 2009-09-30
JIAXING UNITED CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the selection of extractant for different systems is very different, and the selection of extractant is crucial for extractive distillation, so the existing research on extractive distillation of other systems cannot be directly applied In the separation and purification of low-boiling mixtures of organosilicon, there is no report on the use of extractive distillation to purify dimethylchlorosilane in the prior art

Method used

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  • Method for purifying dimethylchlorosilane by extraction and distillation
  • Method for purifying dimethylchlorosilane by extraction and distillation
  • Method for purifying dimethylchlorosilane by extraction and distillation

Examples

Experimental program
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Effect test

Embodiment 1

[0036] In a set of tower kettle volume 1m 3 , in the batch rectification device of the theoretical plate number 80, add 200kg low-boiling mixture to the tower kettle, continuously add the extraction agent n-butyl n-butyrate at the speed of 3kg / min from the top of the tower, the boiling point of n-butyl n-butyrate is 164 ° C; the total amount of extractant added is 720kg. The rectification tower is controlled to be at normal pressure, and the distillate extraction rate is 1-1.5kg / min. The entire rectification process was followed by gas chromatography, and fractions were cut according to changes in the composition of the overhead. When the rectification of the low-boiling mixture is completed or the extractant fraction appears at the top of the tower, the rectification is terminated, and the tower kettle is cooled to normal temperature, and the extractant can be directly reused.

[0037] The gas chromatography detection results of each fraction are as follows:

[0038]

...

Embodiment 2

[0044] The extraction agent is diethylene glycol dimethyl ether, and the boiling point is 162 ° C. Others are the same as in Example 1, and the gas chromatographic detection results of each fraction are as follows:

[0045]

Embodiment 3

[0047] Extraction agent is dibutyl phthalate, and boiling point is 340 ℃, other is identical with embodiment 1, and the gas chromatographic detection result of each fraction is as follows:

[0048]

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Abstract

The invention discloses a method for purifying dimethylchlorosilane, which is to add an extractant to extract and distillate a low-boiling mixture produced in a process for producing methyl chlorosilane by a direct method to separate the dimethylchlorosilane, wherein extractant is an apolar aprotic solvent having a boiling point of no less than 70 DEG C. The extraction and distillation method adopted can effectively separate a hydrocarbon of 2-methyl-2-butylene having a boiling point similar to that of the dimethylchlorosilane, so the method for purifying the dimethylchlorosilane by extraction and distillation breaks a limit of the conventional distillation purification method that the maximum content of the dimethylchlorosilane is less than 88 percent, achieves a content of the dimethylchlorosilane in distillation of up to 95 percent, even 98 percent.

Description

technical field [0001] The invention relates to a method for purifying dimethylchlorosilane, in particular to a method for extracting, rectifying and purifying dimethylchlorosilane from a low-boiling mixture of organic silicon, belonging to the field of organic chemistry. Background technique [0002] In the process of preparing methylchlorosilane by the direct method of reacting silicon powder with methyl chloride, in addition to the main product dimethyldichlorosilane, by-products such as high-boiling mixture, low-boiling mixture and methyltrichlorosilane are also formed. The low-boiling mixture refers to the by-products whose boiling point is lower than 40℃, and its composition is quite complicated and changes with the change of production conditions. The usual mass percentage composition of the low boiling mixture is: 20-70% of tetramethylsilane, 5-35% of dimethylchlorosilane, 2-15% of methyldichlorosilane, 10-35% of hydrocarbons, and 0-35% of others. 8%. [0003] Dire...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/12C07F7/20C07F7/16
Inventor 吴清洲陈关喜周婷婷柴子斌
Owner JIAXING UNITED CHEM
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