CN104045087A - Device for preparing trichlorosilane - Google Patents
Device for preparing trichlorosilane Download PDFInfo
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- CN104045087A CN104045087A CN201410264535.XA CN201410264535A CN104045087A CN 104045087 A CN104045087 A CN 104045087A CN 201410264535 A CN201410264535 A CN 201410264535A CN 104045087 A CN104045087 A CN 104045087A
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- rectifying tower
- silicon tetrachloride
- pipe
- trichlorosilane
- silicon
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Abstract
The invention discloses a device for preparing trichlorosilane. The device comprises a rectifying tower, a silicon tetrachloride discharge pipe arranged at the bottom of the rectifying tower and a silicon tetrachloride discharge pipe arranged on the rectifying tower, a fixed bed reactor connected with the silicon tetrachloride discharge pipe, a mixing pipe provided with a static mixer, a trichlorosilane discharge pipe arranged in the middle position of the rectifying tower and an impurity outflow pipe arranged at the top position of the rectifying tower, wherein the fixed bed reactor is also connected to a dichlorosilane feed pipe, and the silicon tetrachloride discharge pipe and dichlorosilane feed pipe are subjected to cooperation by the mixing pipe; the discharge outlet of the fixed bed reactor is connected to the upper part of the rectifying tower by a synthesis gas pipe, and the impurity outflow pipe is connected to the reflux tank of the rectifying tower. By virtue of two devices, dichlorosilane and silicon tetrachloride as byproducts in the improved Siemens production process are converted into trichlorosilane, the utilization of raw materials is improved and the problem of enrichment of dichlorosilane and silicon tetrachloride is solved.
Description
Technical field
The present invention relates to trichlorosilane preparation field, be specifically related to prepare the device of trichlorosilane.
Background technology
Trichlorosilane claims again trichlorosilane, trichlorosilane, English name: trichiorosilane or silicochioroform, molecular formula is SIHCL
3, for synthesizing of organosilane and alkyl, aryl and organo-functional group chlorosilane, be monomer the most basic in organo silane coupling agent, be also the raw material of producing semiconductor silicon, silicon single crystal and polysilicon.
Anti-disproportionation technology is under the specific bed height that specific resin is housed, and at certain temperature and pressure, consumes the process that silicon tetrachloride and dichloro-dihydro silicon generate trichlorosilane.By the method for rectifying, isolate the process of product simultaneously, principle is: for reversible reaction, when the volatility of a certain product is greater than or less than reactant, if this product is separated from reaction system, can destroy original balance, make reaction continue to carry out to the direction of resultant, thereby can improve transformation efficiency.For trichlorosilane, come by product and the trace impurity of autoreactor, excessive silicon tetrachloride can carry out separation and circulation by again getting back in rectifying tower.
At present, the production of polysilicon technique of China's most enterprises is improved Siemens, and this technique be take trichlorosilane as raw material, generating portion dichloro-dihydro silicon and a large amount of silicon tetrachloride by product in production process.
For silicon tetrachloride, the methods such as existing cold hydride process are processed it, make it again be converted into trichlorosilane recycling, but domestic technique is immature, and the pending amount of silicon tetrachloride are very large; For dichloro-dihydro silicon, although the technology of existing comparative maturity take that it prepares polysilicon as raw material, due to blockade on new techniques, domesticly in this field, be still almost blank, and dichloro-dihydro silicon boiling point is lower, has larger danger abroad.The enrichment of dichloro-dihydro silicon and silicon tetrachloride and processing problem thereof become a difficult problem for the more domestic production of polysilicon enterprises of puzzlement gradually.
Summary of the invention
The technical problem to be solved in the present invention is to provide the device of preparing trichlorosilane, comprise rectifying tower and fixed-bed reactor, utilizing above-mentioned two devices is trichlorosilane by the by product dichloro-dihydro silicon in improved Siemens production process and converting silicon tetrachloride, improve raw material availability, solved the problem of dichloro-dihydro silicon and silicon tetrachloride enrichment simultaneously.
For achieving the above object, technical scheme of the present invention is as follows:
The device of preparing trichlorosilane, comprising:
One rectifying tower,
The one silicon tetrachloride discharge nozzle and that is arranged at tower bottom of rectifying tower position is arranged at the silicon tetrachloride discharge nozzle on rectifying tower,
One fixed bedreactor connecting by silicon tetrachloride discharge nozzle, on described fixed bedreactor, also connect a dichloro-dihydro silicon feed-pipe, also comprise that one is provided with the mixing tube of static mixer, this mixing tube is by described silicon tetrachloride discharge nozzle and competing the closing of dichloro-dihydro silicon feed-pipe; The discharge port of described fixed bedreactor connects the top of rectifying tower by syngas tube,
Also comprise that one is positioned at the trichlorosilane vent pipe of rectifying tower medium position,
One is positioned at the impurity outlet pipe of rectifying tower top end position, and described impurity outlet pipe connects a rectifying tower return tank, and this rectifying tower return tank is connected with rectifying tower by return line,
One is positioned at the sewer pipe of rectifying tower bottom position.
In a preferred embodiment of the invention, described rectifying tower comprises that a chimney column plate and that is positioned at bottom is positioned at the board-like tower tray of chimney column plate top.
In a preferred embodiment of the invention, described board-like number of trays is 95.
In a preferred embodiment of the invention, in described fixed bedreactor, be filled with basic resin catalyzer.
In a preferred embodiment of the invention, on described silicon tetrachloride discharge nozzle, be provided with discharging pump, on described return line, be provided with reflux pump.
By technique scheme, the invention has the beneficial effects as follows:
(1) utilize said apparatus, the trichlorosilane of preparing high using value with the lower dichloro-dihydro silicon of using value and silicon tetrachloride, improves raw material availability, has solved the problem of dichloro-dihydro silicon and silicon tetrachloride enrichment simultaneously.
(2) application conventional rectification, reaction product is separated from system, change former molecular balance, improve dichloro-dihydro silicon conversion.
(3) for improving the transformation efficiency of dichloro-dihydro silicon, in reaction, silicon tetrachloride should be fully excessive, makes the final transformation efficiency of dichloro-dihydro silicon reach in theory 100%.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skills, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is structural representation of the present invention.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with concrete diagram, further set forth the present invention.
With reference to Fig. 1, prepare the device of trichlorosilane, by the by product dichloro-dihydro silicon in improved Siemens production process and converting silicon tetrachloride, be trichlorosilane.
After silicon tetrachloride is removed impurity in a rectifying tower, be equipped with under certain bed height with a small amount of dichloro-dihydro silicon in the fixed bedreactor of basic resin catalyzer and react, produce trichlorosilane and excessive silicon tetrachloride, enter the rectifying tower that contains chimney column plate, from the tower top of rectifying tower, remove a small amount of silane and the light constituent trace impurity of producing, rectifier lateral line discharging is to other rectifying tower.
Anti-disproportionation reaction involved in the present invention is: SIH
2c1
2+ SICL
4=2SIHCL
3.
Specifically comprise: a rectifying tower 100, rectifying tower 100 comprises that a chimney column plate 110 and that is positioned at bottom is positioned at the board-like tower tray 120 of chimney column plate top, wherein board-like number of trays is 95;
The one silicon tetrachloride discharge nozzle 130 and that is arranged at tower bottom of rectifying tower position is arranged at the silicon tetrachloride discharge nozzle 170 on rectifying tower,
One fixed bedreactor 200 connecting by silicon tetrachloride discharge nozzle 130, in this fixed bedreactor, be filled with basic resin catalyzer, on described fixed bedreactor 200, also connect a dichloro-dihydro silicon feed-pipe 210, also comprise that one is provided with the mixing tube 220 of static mixer 230, this mixing tube 220 is by described silicon tetrachloride discharge nozzle 130 and dichloro-dihydro silicon feed-pipe 210 competing closing; The discharge port of described fixed bedreactor connects the top of rectifying tower by syngas tube 240,
Also comprise that one is positioned at the trichlorosilane vent pipe 140 of rectifying tower 100 medium positions, on trichlorosilane vent pipe 140, be provided with chilled water unit 141,
One is positioned at the impurity outlet pipe 150 of rectifying tower top end position, on this impurity outlet pipe 150, be also provided with overhead condenser 151, described impurity outlet pipe 150 connects a rectifying tower return tank 300, and this rectifying tower return tank is connected with rectifying tower by return line 310, also connect and remove process tail gas treatment unit
One is positioned at the sewer pipe 160 of rectifying tower bottom position.
On above-mentioned silicon tetrachloride discharge nozzle 130, be provided with discharging pump 131, on return line 310, be provided with reflux pump 311, utilize the velocity of flow of discharging pump 131 and reflux pump 311 lift gas, improve speed of response.
Choose an application example and be illustrated, by anti-disproportionation reaction, by fixed-bed reactor and rectifying tower, produce 27000 tons/year of trichlorosilanes.
Mixing raw material forms: dichloro-dihydro silicon DCS: silicon tetrachloride STC=1:10 (mass ratio).
Mixing raw material inlet amount is 14100Kg/h.Rectifying tower 1 is totally 95 board-like tower trays, the about 3300Kg/h of silicon tetrachloride STC enters rectifying tower by rectifier bottoms, in the about 12800kg/h of the silicon tetrachloride STC of bottom lateral line withdrawal function and the about 1280kg/h of dichloro-dihydro silicon DCS, enter static mixer, after interchanger, controlling feeding temperature is 80 ℃ of left and right, and pressure 9barg enters fixed-bed reactor.
3300mm is high for fixed-bed reactor bed height, the about 14080Kg/h of mixing raw material is in fixed-bed reactor its top feed, working pressure is 0.9MPa, 80 ℃ of bed middle part temperature, 90 ℃ of bed temperature of lower, material does not have loss in reactor, reactor outlet extraction 14080Kg/h mixed chlorosilane silicon, each constituent mass mark is trichlorosilane TCS24.2%, silicon tetrachloride STC75.2%, dichloro-dihydro silicon DCS0.10%, all the other are the trace impurity of silane and weight component.Impurity in these components and excessive STC need return to rectifying tower 1.
Rectifying tower 1 is totally 95 board-like tower trays, the about 14080Kg/h of fixed-bed reactor mixture is in the 89th board-like tower tray charging, working pressure is 0.3MPa, 61 ℃ of tower top temperatures, 114 ℃ of column bottom temperatures, the about 10Kg/h of overhead extraction, with the dichloro-dihydro silicon of trace impurity, enters other cell processing, the mixing trichlorosilane of the 45th about 4500kg/h of board-like tower tray side line extraction temperature after interchanger heat exchange is 45 ℃, enters other rectifying tower and carries out separation.
For improving the transformation efficiency of dichloro-dihydro silicon, in reaction, silicon tetrachloride should be fully excessive, makes the final transformation efficiency of dichloro-dihydro silicon reach in theory 100%.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (5)
1. the device of preparing trichlorosilane, is characterized in that, comprising:
One rectifying tower,
The one silicon tetrachloride discharge nozzle and that is arranged at tower bottom of rectifying tower position is arranged at the silicon tetrachloride discharge nozzle on rectifying tower,
One fixed bedreactor connecting by silicon tetrachloride discharge nozzle, on described fixed bedreactor, also connect a dichloro-dihydro silicon feed-pipe, also comprise that one is provided with the mixing tube of static mixer, this mixing tube is by described silicon tetrachloride discharge nozzle and competing the closing of dichloro-dihydro silicon feed-pipe; The discharge port of described fixed bedreactor connects the top of rectifying tower by syngas tube,
Also comprise that one is positioned at the trichlorosilane vent pipe of rectifying tower medium position,
One is positioned at the impurity outlet pipe of rectifying tower top end position, and described impurity outlet pipe connects a rectifying tower return tank, and this rectifying tower return tank is connected with rectifying tower by return line,
One is positioned at the sewer pipe of rectifying tower bottom position.
2. the device of preparing trichlorosilane according to claim 1, is characterized in that, described rectifying tower comprises that a chimney column plate and that is positioned at bottom is positioned at the board-like tower tray of chimney column plate top.
3. the device of preparing trichlorosilane according to claim 2, is characterized in that, described board-like number of trays is 95.
4. the device of preparing trichlorosilane according to claim 1, is characterized in that, is filled with basic resin catalyzer in described fixed bedreactor.
5. the device of preparing trichlorosilane according to claim 1, is characterized in that, on described silicon tetrachloride discharge nozzle, is provided with discharging pump, on described return line, is provided with reflux pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410264535.XA CN104045087B (en) | 2014-06-13 | 2014-06-13 | Prepare the device of trichlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410264535.XA CN104045087B (en) | 2014-06-13 | 2014-06-13 | Prepare the device of trichlorosilane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104045087A true CN104045087A (en) | 2014-09-17 |
| CN104045087B CN104045087B (en) | 2017-01-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410264535.XA Expired - Fee Related CN104045087B (en) | 2014-06-13 | 2014-06-13 | Prepare the device of trichlorosilane |
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| Country | Link |
|---|---|
| CN (1) | CN104045087B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107720758A (en) * | 2017-11-13 | 2018-02-23 | 浙江工业大学上虞研究院有限公司 | Chemical industry production system |
| CN108910894A (en) * | 2018-08-31 | 2018-11-30 | 内蒙古通威高纯晶硅有限公司 | Trichlorosilane rectification system and rectificating method |
| CN112028926A (en) * | 2019-06-03 | 2020-12-04 | 新特能源股份有限公司 | Separation device and separation method for removing silicon tetrachloride in organic silicon monomer azeotrope |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955187A (en) * | 2010-10-21 | 2011-01-26 | 天津大学 | Method and apparatus for preparing trichlorosilane through reaction rectification by using proportionate reaction |
| CN102923716A (en) * | 2012-11-20 | 2013-02-13 | 四川瑞能硅材料有限公司 | Process for producing trichlorosilane through inverse disporportionation of dichlorosilane |
| CN203498102U (en) * | 2013-08-30 | 2014-03-26 | 中国恩菲工程技术有限公司 | Equipment for preparing trichlorosilane |
| CN203513290U (en) * | 2013-09-29 | 2014-04-02 | 河南尚宇新能源股份有限公司 | System for producing trichlorosilane by anti-disproportionation reaction of dichlorosilane |
-
2014
- 2014-06-13 CN CN201410264535.XA patent/CN104045087B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101955187A (en) * | 2010-10-21 | 2011-01-26 | 天津大学 | Method and apparatus for preparing trichlorosilane through reaction rectification by using proportionate reaction |
| CN102923716A (en) * | 2012-11-20 | 2013-02-13 | 四川瑞能硅材料有限公司 | Process for producing trichlorosilane through inverse disporportionation of dichlorosilane |
| CN203498102U (en) * | 2013-08-30 | 2014-03-26 | 中国恩菲工程技术有限公司 | Equipment for preparing trichlorosilane |
| CN203513290U (en) * | 2013-09-29 | 2014-04-02 | 河南尚宇新能源股份有限公司 | System for producing trichlorosilane by anti-disproportionation reaction of dichlorosilane |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107720758A (en) * | 2017-11-13 | 2018-02-23 | 浙江工业大学上虞研究院有限公司 | Chemical industry production system |
| CN108910894A (en) * | 2018-08-31 | 2018-11-30 | 内蒙古通威高纯晶硅有限公司 | Trichlorosilane rectification system and rectificating method |
| CN112028926A (en) * | 2019-06-03 | 2020-12-04 | 新特能源股份有限公司 | Separation device and separation method for removing silicon tetrachloride in organic silicon monomer azeotrope |
| CN112028926B (en) * | 2019-06-03 | 2024-03-12 | 新特能源股份有限公司 | Separation device and separation method for removing silicon tetrachloride in organosilicon monomer azeotrope |
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| Publication number | Publication date |
|---|---|
| CN104045087B (en) | 2017-01-04 |
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Granted publication date: 20170104 Termination date: 20200613 |