CN104045087B - Prepare the device of trichlorosilane - Google Patents
Prepare the device of trichlorosilane Download PDFInfo
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- CN104045087B CN104045087B CN201410264535.XA CN201410264535A CN104045087B CN 104045087 B CN104045087 B CN 104045087B CN 201410264535 A CN201410264535 A CN 201410264535A CN 104045087 B CN104045087 B CN 104045087B
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- China
- Prior art keywords
- trichlorosilane
- silicon chloride
- dichlorosilane
- rectifying column
- discharge nozzle
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Abstract
The invention discloses the device preparing trichlorosilane, including: a rectifying column, Silicon chloride. discharge nozzle that one is arranged on rectifying tower and Silicon chloride. discharge nozzle, one fixed bedreactor connected by Silicon chloride. discharge nozzle, a dichlorosilane feed pipe it is also connected with on described fixed bedreactor, also including a mixing tube being provided with static mixer, this mixing tube is by described Silicon chloride. discharge nozzle and the competing conjunction of dichlorosilane feed pipe；The discharging opening of described fixed bedreactor connects the top of rectifying column by syngas tube, also include a trichlorosilane discharge pipe being positioned at rectifying column medium position, the one impurity effuser being positioned at rectifying tower top end position, described impurity effuser connects a rectifier column reflux tank, utilizing above-mentioned two device is trichlorosilane by the by-product dichlorosilane in improved Siemens production process and converting silicon tetrachloride, improve raw material availability, solve dichlorosilane and the problem of Silicon chloride. enrichment simultaneously.
Description
Technical field
The present invention relates to trichlorosilane preparation field, be specifically related to prepare the device of trichlorosilane.
Background technology
Trichlorosilane also known as trichlorosilane, silicochloroform, English name: trichiorosilane or
Silicochioroform, molecular formula is SIHCL3, for organosilan and alkyl, aryl and organic official
The synthesis of chlorosilane can be rolled into a ball, be monomer most basic in organo silane coupling agent, be also produce semiconductor silicon,
Monocrystal silicon and the raw material of polysilicon.
Anti-disproportionation technology is under the specific bed height equipped with specific resin, disappears at certain temperature and pressure
Consumption Silicon chloride. and dichlorosilane generate the process of trichlorosilane.Isolate product by the method for rectification simultaneously
Process, principle is: for reversible reaction, when the volatility of a certain product is more than or less than reactant,
If separated from reaction system by this product, then can destroy original balance, making reaction continue to product
Direction is carried out, thus can improve conversion ratio.Trichlorosilane is come to by-product and the trace impurity of autoreactor,
Excess Silicon chloride. can separate in rectifying column and circulate by turning again to.
At present, the polysilicon production process of China's most enterprises is improved Siemens, and this technique is with trichlorine
Hydrogen silicon is raw material, produces part dichlorosilane and a large amount of silicon tetrachloride byproduct in production process.
For Silicon chloride., have the methods such as cold hydrogenization method and it is processed so that it is be re-converted into trichlorine
Hydrogen silicon reuses, but domestic technique is immature, and the pending amount of Silicon chloride. is the biggest；For dichloro-dihydro
Silicon, although the external technology having comparative maturity prepares polysilicon with it for raw material, but due to blockade on new techniques,
Domestic still the most blank in this field, and dichlorosilane boiling point is relatively low, has bigger danger.Two
It is raw that chlorine dihydro silicon and the enrichment of Silicon chloride. and process problem thereof have been increasingly becoming the more domestic polysilicon of puzzlement
Produce a difficult problem for enterprise.
Summary of the invention
The technical problem to be solved in the present invention is to provide the device preparing trichlorosilane, including rectifying column with fixing
Bed reactor, utilizes above-mentioned two device by the by-product dichlorosilane in improved Siemens production process
It is trichlorosilane with converting silicon tetrachloride, improves raw material availability, solve dichlorosilane and tetrachloro simultaneously
The problem of SiClx enrichment.
For reaching above-mentioned purpose, technical scheme is as follows:
Prepare the device of trichlorosilane, including:
One rectifying column,
The tetrachloro that the one Silicon chloride. discharge nozzle and being arranged at tower bottom of rectifying tower position is arranged on rectifying column
SiClx discharge nozzle,
One fixed bedreactor connected by Silicon chloride. discharge nozzle, described fixed bedreactor is also connected with
One dichlorosilane feed pipe, also includes a mixing tube being provided with static mixer, and this mixing tube is by described
Silicon chloride. discharge nozzle and the competing conjunction of dichlorosilane feed pipe；The discharging opening of described fixed bedreactor is by closing
Trachea is become to connect the top of rectifying column,
Also include a trichlorosilane discharge pipe being positioned at rectifying column medium position,
The one impurity effuser being positioned at rectifying tower top end position, described impurity effuser connects a rectifier column reflux
Tank, this rectifier column reflux tank is connected by return duct rectifying column,
One sewer pipe being positioned at rectifying column bottom position.
In a preferred embodiment of the invention, described rectifying column include one be positioned at bottom chimney column plate and
One is positioned at the board-like tower tray above chimney column plate.
In a preferred embodiment of the invention, described board-like number of trays is 95 pieces.
In a preferred embodiment of the invention, described fixed bedreactor is filled with basic resin catalysis
Agent.
In a preferred embodiment of the invention, described Silicon chloride. discharge nozzle is provided with discharging pump, institute
State and on return duct, be provided with reflux pump.
By technique scheme, the invention has the beneficial effects as follows:
(1) utilizing said apparatus, the dichlorosilane relatively low by using value and Silicon chloride. prepare high application
Be worth trichlorosilane, improve raw material availability, solve simultaneously dichlorosilane and Silicon chloride. enrichment
Problem.
(2) application conventional rectification, separates product from system, changes former molecular balance, improves two
Chlorine dihydro silicon conversion.
(3) for improving the conversion ratio of dichlorosilane, in reaction, Silicon chloride. should be fully excessive, makes dichloro two
The final conversion ratio of hydrogen silicon reaches 100% in theory.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to enforcement
In example or description of the prior art, the required accompanying drawing used is briefly described, it should be apparent that, describe below
In accompanying drawing be only some embodiments of the present invention, for those of ordinary skill in the art, do not paying
On the premise of going out creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the structural representation of the present invention.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reach purpose and be easy to understand with effect,
Below in conjunction with being specifically illustrating, the present invention is expanded on further.
With reference to Fig. 1, prepare the device of trichlorosilane, by the by-product two in improved Siemens production process
Chlorine dihydro silicon and converting silicon tetrachloride are trichlorosilane.
Silicon chloride. is high at certain bed with a small amount of dichlorosilane after going the removal of impurity in a rectifying column
Under degree, fixed bedreactor equipped with basic resin catalyst reacts, produce trichlorosilane and excess
Silicon chloride., enter containing the rectifying column of chimney column plate, remove produce a small amount of from the tower top of rectifying column
Silane and light component trace impurity, rectifier lateral line discharging is to other rectifying columns.
Anti-dismutation reaction involved in the present invention is: SIH2C12+SICL4=2SIHCL3。
Specifically including: a rectifying column 100, rectifying column 100 includes chimney column plate 110 He being positioned at bottom
One is positioned at the board-like tower tray 120 above chimney column plate, and the most board-like number of trays is 95 pieces；
The one Silicon chloride. discharge nozzle 130 being arranged at tower bottom of rectifying tower position and one be arranged on rectifying column four
Silicon chloride discharge nozzle 170,
One fixed bedreactor 200 connected by Silicon chloride. discharge nozzle 130, in this fixed bedreactor
It is filled with basic resin catalyst, described fixed bedreactor 200 is also connected with a dichlorosilane feed pipe
210, also include a mixing tube 220 being provided with static mixer 230, this mixing tube 220 is by described tetrachloro
SiClx discharge nozzle 130 and the competing conjunction of dichlorosilane feed pipe 210；The discharging opening of described fixed bedreactor leads to
Cross syngas tube 240 and connect the top of rectifying column,
Also including a trichlorosilane discharge pipe 140 being positioned at rectifying column 100 medium position, trichlorosilane is discharged
Chilled water unit 141 it is provided with on pipe 140,
The one impurity effuser 150 being positioned at rectifying tower top end position, this impurity effuser 150 is additionally provided with
Overhead condenser 151, described impurity effuser 150 connects a rectifier column reflux tank 300, and this rectifying column returns
Stream tank is connected by return duct 310 rectifying column, is also connected with process tail gas processing means,
One sewer pipe 160 being positioned at rectifying column bottom position.
It is provided with discharging pump 131 on above-mentioned Silicon chloride. discharge nozzle 130, return duct 310 is provided with backflow
Pump 311, utilizes discharging pump 131 and the flowing velocity of reflux pump 311 lift gas, improves response speed.
Choose an application example to be illustrated, raw by fixed bed reactors and rectifying column with anti-dismutation reaction
Produce 27000 tons/year of trichlorosilanes.
Mixing raw material composition: dichlorosilane DCS: Silicon chloride. STC=1:10 (mass ratio).
Mixing feedstock amount is 14100Kg/h.Rectifying column 1 totally 95 pieces of board-like tower trays, Silicon chloride. STC
About 3300Kg/h is entered rectifying column by rectifier bottoms, in bottom lateral line withdrawal function Silicon chloride. STC about
12800kg/h and dichlorosilane DCS about 1280kg/h enters static mixer, controls after heat exchanger
Feeding temperature is about 80 DEG C, and pressure 9barg enters fixed bed reactors.
Fixed bed reactors bed height 3300mm is high, and raw material about 14080Kg/h is in fixed bed reaction in mixing
Device its top feed, operation pressure is 0.9MPa, bed middle portion temperature 80 DEG C, bed temperature of lower 90 DEG C,
Material does not has loss, reactor outlet extraction 14080Kg/h mixed chlorosilane silicon, each component in the reactor
Mass fraction is trichlorosilane TCS24.2%, Silicon chloride. STC75.2%, dichlorosilane DCS
0.10%, remaining is silane and the trace impurity of weight component.Impurity in these components and the STC of excess
Rectifying column 1 need to be returned to.
Rectifying column 1 totally 95 pieces of board-like tower trays, fixed bed reactors mixed material about 14080Kg/h is in the 89th
The board-like tower tray of block feeds, and operation pressure is 0.3MPa, tower top temperature 61 DEG C, column bottom temperature 114 DEG C, tower
Top extraction about 10Kg/h, with the dichlorosilane of trace impurity, enters other cell processing, the 45th block of plate
Mixing trichlorosilane temperature after heat exchanger heat exchange of formula tower tray side take-off about 4500kg/h is 45 DEG C,
Enter other rectifying column to separate.
For improving the conversion ratio of dichlorosilane, in reaction, Silicon chloride. should be fully excessive, makes dichlorosilane
Final conversion ratio reaches 100% in theory.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.The industry
Skilled person will appreciate that, the present invention is not restricted to the described embodiments, in above-described embodiment and description
The principle that the present invention is simply described described, without departing from the spirit and scope of the present invention, the present invention
Also having various changes and modifications, these changes and improvements both fall within scope of the claimed invention.This
The claimed scope of invention is defined by appending claims and equivalent thereof.
Claims (5)
1. prepare the device of trichlorosilane, it is characterised in that including:
One rectifying column,
The one Silicon chloride. discharge nozzle being arranged at tower bottom of rectifying tower position,
One fixed bed reactors connected by Silicon chloride. discharge nozzle, described fixed bed reactors are also connected with
One dichlorosilane feed pipe, also includes a mixing tube being provided with static mixer, and described Silicon chloride. goes out
Material pipe and dichlorosilane feed pipe cause described mixing tube；The discharging opening of described fixed bed reactors is by closing
Trachea is become to connect the top of rectifying column,
Also include a trichlorosilane discharge pipe being positioned at rectifying column medium position,
The one impurity effuser being positioned at rectifying tower top end position, described impurity effuser connects a rectifier column reflux
Tank, this rectifier column reflux tank is connected by return duct above-mentioned rectifying column,
One sewer pipe being positioned at rectifying column bottom position.
The device preparing trichlorosilane the most according to claim 1, it is characterised in that described rectification
Tower includes that a chimney column plate and being positioned at bottom is positioned at the board-like tower tray above chimney column plate.
The device preparing trichlorosilane the most according to claim 2, it is characterised in that described board-like
Number of trays is 95 pieces.
The device preparing trichlorosilane the most according to claim 1, it is characterised in that described fixing
Bed reactor is filled with basic resin catalyst.
The device preparing trichlorosilane the most according to claim 1, it is characterised in that described tetrachloro
It is provided with discharging pump on SiClx discharge nozzle, described return duct 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 CN104045087A (en) | 2014-09-17 |
| CN104045087B true 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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Families Citing this family (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 |
| 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 |
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 |
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| CN104045087A (en) | 2014-09-17 |
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