Fiber-level high purity silicon tetrachloride continuous azeotropy lightness removing rectification method

A pure silicon tetrachloride and delight rectification technology, which is applied in the field of optical fiber-grade high-purity silicon tetrachloride continuous azeotropic delight rectification, can solve the problem of difficult separation, great influence on the purity of silicon tetrachloride, and unsuitable for purification. and other problems to achieve the effect of reducing system energy consumption and ensuring purity

Active Publication Date: 2011-05-11
TIANJIN UNIV
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  • Claims
  • Application Information

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Problems solved by technology

And most of the existing silicon tetrachloride rectification purification methods are batch processes, which are not suitable for the purification of large-scale silicon tetrachloride industrial raw materials
In addition, among silicon tetrachloride impurities, the boiling point of trimethylchlorosilane is 57.6°C, and the boiling point of silicon tetrachloride is 57°C. The azeotrope at ℃ is difficult to separate completely by traditional distillation
Although the content of trimethylchlorosilane in the raw material is very low (<0.05%), it has a great impact on the purity of the separation and purification of high-purity silicon tetrachloride

Method used

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Experimental program
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Effect test

Embodiment 1

[0023] Processing 2 tons / year of silicon tetrachloride purification, the feed composition is as follows: dichlorodihydrosilane content is 0.5%; trichlorosilane content is 2%; silicon tetrachloride content is 96.95%, dimethyl dichloride The monosilane content is 0.5%, and the trimethylchlorosilane content is 0.05%.

[0024] The pressure of the upper tower of the light removal tower is controlled at 220KPa A, and the theoretical number of stages is 100 in total, and the ratio of top reflux to feed is 10; The heavy tower adopts a pressurized tower, the pressure is controlled at 250KPa A, the ratio of the reflux at the top of the tower to the feed is 15, and the theoretical number of stages is 80; a part of the bottom stream of the heavy removal tower is returned to the light removal tower for feeding, and the bottom of the heavy removal tower is returned to the stream and extracted The logistics ratio is 3:1. The impurity content is controlled at 10 in the silicon tetrachloride ...

Embodiment 2

[0026] Processing 4 tons / year of silicon tetrachloride purification, the feed composition is as follows: dichlorodihydrosilane content is 1.5%; trichlorosilane content is 18%; silicon tetrachloride content is 79.99%, dimethyl dichlorosilane The monosilane content is 0.5%, and the trimethylchlorosilane content is 0.01%.

[0027] The pressure of the upper tower of the light removal tower is controlled at 200KPa A, and the theoretical number of stages is 80 in total, and the ratio of reflux to feed at the top of the tower is 5; The heavy tower adopts a pressurized tower, the pressure is controlled at 200KPa A, the ratio of reflux to feed at the top of the tower is 8, and the theoretical number of stages is 60; a part of the bottom stream of the de-heavy tower returns to the de-light tower to feed, and the return stream changes elastically according to the concentration range of the raw material. The ratio of the return stream to the output stream at the bottom of the de-weighting...

Embodiment 3

[0029] Processing 4 tons / year of silicon tetrachloride purification, the feed composition is as follows: dichlorodihydrosilane content is 0.05%; trichlorosilane content is 1%; silicon tetrachloride content is 98.4%, dimethyl dichlorosilane The monosilane content is 0.5%, and the trimethylchlorosilane content is 0.05%.

[0030] The upper tower of the light removal tower adopts a pressurized tower, the pressure is controlled at 250KPa A, the theoretical number of stages is 120, and the ratio of top reflux to feed is 12; the lower tower of the light removal tower adopts a pressurized tower, the pressure is controlled at 250KPa A, and the theoretical number of stages is total The weight removal tower adopts a pressurized tower, the pressure is controlled at 300KPa A, the tower top reflux to feed ratio is 20, and the theoretical number of stages is 100; a part of the weight removal tower bottom stream is returned to the light removal tower to feed, and the return flow is based on th...

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Abstract

The invention belongs to a fiber-level high purity silicon tetrachloride continuous azeotropy lightness removing rectification method. A lightness removing tower and a heaviness removing tower are adopted; light components and azeotropic mixtures are removed from the raw material, the material at the bottom of the lightness removing tower enters the heaviness removing tower to lead the heaviness to be removed, partial material at the bottom of the heaviness removing tower returns to the lightness removing tower as incoming stock and the fiber-level silicon tetrachloride product is obtained at the top of the heaviness removing tower. The lightness removing tower is divided into an upper lightness removing tower and a lower lightness removing tower. The upper lightness removing tower adopts a pressurizing tower with the pressure being 200-250 KPa, the total theoretical stage being 80-120, and the rate of top reflux to the incoming material being 5-12; the lower lightness removing tower adopts a pressurizing tower with the pressure being 200-250KPa, and the total theoretical stage being 80-120; and the heaviness removing tower adopts a pressurizing tower with the pressure being 200-300KPa, the rate of the top reflux to the incoming material being 8-20 and the theoretical stage being 60-100. The system adopts continuous operation, is suitable for large-scale silicon tetrachloride purification and reduces energy consumption. The method has wide requirements on the raw materials of the silicon tetrachloride and is applicable to the purification of silicon tetrachloride with the concentration range of 50-98 percent in raw materials.

Description

technical field [0001] The invention belongs to the technical field of rectification, and particularly proposes a continuous azeotropic lightening and rectification method for optical fiber-grade high-purity silicon tetrachloride. Background technique [0002] Silicon tetrachloride (SiCl 4 ) is a high value-added product, mainly used in the preparation of organosilicon compounds such as silicate, organosilicon oil, high-temperature insulating varnish, organosilicon resin, silicone rubber and heat-resistant gaskets, etc. SiCl 4 It is used in the manufacture of smoke screen agents in the military industry, used in the manufacture of corrosion-resistant ferrosilicon in the metallurgical industry, and used as a release agent in the foundry industry. SiCl 4 It can also be used to produce white carbon black with large specific surface area, synthesize hydrazide and be used as a catalyst for olefin polymerization. Purified high-purity SiCl 4 Mainly used in the manufacture of p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D3/14C01B33/107
Inventor 黄国强郑艳梅王红星李鑫钢华超田玉峰
Owner TIANJIN UNIV
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