Method for purifying dimethylchlorosilane by extraction and distillation

A technology of dimethylchlorosilane and methylchlorosilane, 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, easy distillation and separation, and increased relative volatility

Active Publication Date: 2011-09-14
JIAXING UNITED CHEM +1
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  • Abstract
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  • 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

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Embodiment 1

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

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

[0038] ...

Embodiment 2

[0044] Extractant is diethylene glycol dimethyl ether, and boiling point is 162 ℃, and other is identical with embodiment 1, and the gas chromatography detection result of each cut is as follows:

[0045]

Embodiment 3

[0047] Extractant is dibutyl phthalate, and boiling point is 340 ℃, and other is identical with embodiment 1, and the gas chromatography detection result of each cut 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 and rectifying 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 generated. Among them, the low boiling mixture refers to by-products with a boiling point lower than 40°C, and its composition is quite complex and changes with the change of production conditions. The usual mass percent composition of low boiling mixtures is: tetramethylsilane 20-70%, dimethylchlorosilane 5-35%, methyldichlorosilane 2-15%, hydrocarbon 10-35%, other 0-35%. 8%. [0003] Direct distillation of the...

Claims

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Application Information

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Patent Type & Authority Patents(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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