Method and device for treating dichlorosilane waste by utilizing reactive distillation

A technology of dichlorodihydrosilane and reactive distillation, which is applied in the field of reactive distillation, can solve problems such as complicated process and many circulation flows, and achieve the effects of increasing yield and output, increasing conversion rate, and reducing equipment investment

Active Publication Date: 2013-05-08
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN101955187A proposes a reactive distillation process, the theoretical conversion rate can reach 100%, but t...

Method used

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  • Method and device for treating dichlorosilane waste by utilizing reactive distillation
  • Method and device for treating dichlorosilane waste by utilizing reactive distillation
  • Method and device for treating dichlorosilane waste by utilizing reactive distillation

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Experimental program
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Effect test

Embodiment 1

[0023] 1,700 tons / year of dichlorodihydrosilane waste will be treated by reactive distillation, and 5,000 tons / year of trichlorosilane will be produced.

[0024] The feed conditions of dichlorodihydrosilane, silicon tetrachloride and recycled materials are shown in Table 1.

[0025] Table I

[0026]

[0027] The operating pressure of the reactive distillation tower is 150kPa, the pressure drop of the whole tower is 20kPa, the output at the top of the tower is 624kg / h, the return flow at the top of the tower is 4500kg / h, the diameter of the tower is 0.9m, and the amount of catalyst is 0.1m 3 / m 3 Packing, spray density is 25m 3 / (m 2 h), the heights of the rectifying section, the reaction section and the stripping section packing are 4m, 8m and 4m respectively. The feed position of dichlorodihydrosilane is at the bottom of the reaction section, and the feed position of silicon tetrachloride and circulating materials is at the top of the reaction section.

[0028] Indust...

Embodiment 2

[0030] 1,700 tons / year of dichlorodihydrosilane waste will be treated by reactive distillation, and 5,000 tons / year of trichlorosilane will be produced.

[0031] Adjust the feed molar ratio of dichlorodihydrosilane to silicon tetrachloride to be 1:1, and the feed conditions of dichlorosilane, silicon tetrachloride and recycled materials are shown in Table 2.

[0032] Table II

[0033]

[0034] The operating pressure of the reactive distillation tower is 150kPa, the pressure drop of the whole tower is 20kPa, the output at the top of the tower is 579kg / h, the return flow at the top of the tower is 5000kg / h, the diameter of the tower is 0.9m, and the amount of catalyst is 0.1m 3 / m 3 Packing, spray density is 25m 3 / (m 2h), the heights of the rectifying section, the reaction section and the stripping section packing are 4m, 8m and 4m respectively. The feed position of dichlorodihydrosilane is at the bottom of the reaction section, and the feed position of silicon tetrachlo...

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Abstract

The invention relates to a method and a device for treating dichlorosilane waste by utilizing reactive distillation. A reactive distillation tower is divided to three segments, namely a distillation segment, a reaction segment and a stripping segment, wherein a tower top condenser is arranged on the top of the reactive distillation tower; a tower bottom reboiler is arranged at the bottom of the reactive distillation tower; a cooler is arranged at the bottom of the reactive distillation tower; an inlet of the cooler is connected with a tower bottom material outlet through a pipeline; an outlet of the cooler is connected with an inlet of a low-temperature cooler; and an outlet of the low-temperature cooler is connected to the reactive distillation tower through a pipeline. Raw materials silicon tetrachloride and dichlorosilane respectively enter the reactive distillation tower from the top and the bottom of the reaction segment to generate a disproportionated reaction in the reaction segment so as to produce trichlorosilane, and the trichlorosilane is continuously moved out of the reaction segment under the action of distillation separation; and the silicon tetrachloride in the materials of the tower returns back to the reactive distillation tower through external circulation from the top of the reaction segment so as to further react, and therefore the conversion rate of the reaction can be improved. The conversion rate of the dichlorosilane can achieve 98.50% and the purity of the trichlorosilane in the materials on the top of the tower can achieve 98.48%.

Description

technical field [0001] The invention relates to the technical field of reactive distillation, and in particular proposes a method and equipment for recovering and treating waste dichlorodihydrosilane by using the reactive distillation technology. Background technique [0002] At present, most polysilicon enterprises in my country use the improved Siemens method to produce polysilicon, and the intermediate compound trichlorosilane (SiHCl) 3 , TCS) is deposited in a chemical vapor deposition (CVD) reactor to generate polysilicon, and at the same time a large amount of silicon tetrachloride (SiCl 4 , STC) and a small amount of dichlorosilane (SiH 2 Cl 2 , DCS), among which DCS is flammable, explosive and very dangerous, and will be enriched in the purification process, so far there is no good treatment method. In the traditional process, alkali neutralization method is used to treat it as waste, which not only increases the difficulty of treatment but also increases the mate...

Claims

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Application Information

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IPC IPC(8): C01B33/107
CPCY02P20/10
Inventor 黄国强孙帅帅王红星
Owner TIANJIN UNIV
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