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Method for producing pure octachlorotrisilane and decachlorotetrasilanes

A technology of silicon compounds and general formulas, applied in chemical instruments and methods, halosilanes, silicon compounds, etc.

Inactive Publication Date: 2017-02-22
EVONIK DEGUSSA GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A disadvantage in particular in the prior art is that it is necessary to prepare polychlorosilanes in the presence of gaseous hydrogen

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0104] Embodiment 1 (preparation of octachlorotrisilane)

[0105] 1212 g of a silane mixture comprising tri- and oligomeric silanes were fed into the rectification vessel in the rectification apparatus under nitrogen as protective gas. Thereafter, the apparatus was evacuated to 8 mbar and heated to 157°C. Obtained 269 g of octachlorotrisilane.

[0106] Octachlorotrisilane obtained as a result of column distillation was filtered through a 0.45 μm polypropylene filter under protective gas, thus economically obtaining high purity octachlorotrisilane.

Embodiment 2

[0107] Embodiment 2 (preparation of octachlorotrisilane)

[0108] In the rectification plant under protective gas conditions (nitrogen atmosphere) 300 kg of a silane mixture including tri- and oligosilanes were fed into the rectification vessel.

[0109] The rectification unit is packed with stainless steel distillation packings, with between 80 and 120 theoretical separation stages.

[0110] The apparatus was evacuated to 9.3 mbar and heated to 170°C. 121.6 kg of octachlorotrisilane was obtained, and the purity measured by gas chromatography was over 95%.

[0111] The octachlorotrisilane obtained as a result of column distillation is then filtered through a 0.45 μm polypropylene filter under protective gas. This obtains high-purity octachlorotrisilane.

Embodiment 3

[0112] Embodiment 3 (preparation of decachlorotetrasilane)

[0113] In the rectification apparatus under nitrogen atmosphere as protective gas, 468 g of the silane mixture containing oligosilanes were fed into the rectification vessel. Thereafter, the apparatus was evacuated to 2 mbar and heated to 157°C. Obtain 160 g of decachlorotetrasilane.

[0114] The decachlorotetrasilane obtained as a result of column distillation was filtered through a 0.45 μm polypropylene filter under protective gas, and high-purity decachlorotetrasilane was obtained economically in this way.

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PUM

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Abstract

The invention relates to a method for producing trimeric and / or quaternary silicon compounds or trimeric and / or quaternary germanium compounds. A mixture of silicon compounds or a mixture of germanium compounds is exposed to a non-thermal plasma and the resulting phase is subjected, at least once to vacuum rectification and filtration.

Description

technical field [0001] The present invention relates to a method and apparatus for the preparation of high or ultrahigh purity octachlorotrisilane or decachlorotetrasilane from chlorosilanes by exposing monomeric chlorosilanes to a non-thermal plasma and subjecting the resulting phase to vacuum distillation. Background technique [0002] From the state of the art, processes for the preparation of polychlorosilanes are known. Thus DE 10 2006 034 061 discloses the reaction of silicon tetrachloride with hydrogen to prepare polysilanes. As a result of the transformation in the presence of hydrogen, the polysilanes prepared contain hydrogen. In order that the plant can be maintained in continuous operation, tetrachlorosilane is added in excess relative to the hydrogen. The devices known for this purpose are complex in construction and only allow the preparation of polysilane mixtures. An increased molecular weight of polysilanes can only be achieved by sequentially switching m...

Claims

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Application Information

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IPC IPC(8): C01B33/107B01J19/02B01J19/08C01G17/04
CPCC01G17/04C01B33/107C01B33/10773B01J2219/0847B01J2219/0849B01J2219/0888B01J2219/0894B01J19/088B01J2219/0896C01B33/10778C01P2006/80B01D3/10B01J19/02B01J2219/0254
Inventor J·马里纳斯佩雷斯H·劳莱德J·E·朗C·格茨G·于伦布鲁克
Owner EVONIK DEGUSSA GMBH
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