CN202246101U - Trichlorosilane separation device for purification of substance with high/low boiling point - Google Patents
Trichlorosilane separation device for purification of substance with high/low boiling point Download PDFInfo
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- CN202246101U CN202246101U CN2011203477828U CN201120347782U CN202246101U CN 202246101 U CN202246101 U CN 202246101U CN 2011203477828 U CN2011203477828 U CN 2011203477828U CN 201120347782 U CN201120347782 U CN 201120347782U CN 202246101 U CN202246101 U CN 202246101U
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- trichlorosilane
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Abstract
The utility model discloses a trichlorosilane separation device for purification of a substance with a high/low boiling point, which mainly comprises a raw material tank, a feeding pump, a reboiler, a tower top condenser, a backflow tank, a backflow pump and a high-efficiency distillation tower. The high-efficiency distillation tower is internally provided with high-efficiency regulating fillers and sieve plates, the layer number of the sieve plates is 55-60, the reboiler adopts a horizontal type, and the tower top condenser adopts a floating head type. By adopting pressure distillation, the boiling point of each distillate can be increased, the differences of boiling points can be increased, and the efficiency of separation and purification can be improved. Moreover, after the device is applied to purification, the low-temperature freezing system with condensed water circulation can adopt industrial circulating water, the investment in equipment can be reduced greatly, and the heat transfer efficiency in the process can be increased greatly. Meanwhile, since the floating head type condenser is used as the tower top condenser and the horizontal reboiler is used instead of the vertical reboiler, the equipment failure rate and the hidden safety risks can be reduced, the problem that leakage can be easily caused on the welded part of the tubular part of the condenser in the trichlorosilane industry in the practice can be solved, and the service life of the equipment can be prolonged.
Description
Technical field
The utility model relates to the technical field of rectification and purification, the tripping device of trichlorosilane in particularly a kind of high-boiling and low-boiling components of purifying.
Background technology
Trichlorosilane is claimed trichlorosilane, trichlorosilane again, English name: trichlorlsilane or sili ℃ ochlorlform, molecular formula is SiH ℃ of L
3, be used for the synthetic of organosilane and alkyl, aryl and organic functional group chlorosilane, be monomer the most basic in the organo silane coupling agent, also be the raw material of giving birth to semiconductor silicon, silicon single crystal.
Trichlorosilane is the important intermediate of synthesizing organo-silicon, also is the main raw material of making polysilicon.Along with developing rapidly of organosilicon industry; To being in great demand of trichlorosilane; But the restriction that blocked by foreign technology, the at present domestic manufacturing enterprise that only has several families to produce trichlorosilane, and receive that foreign technology blocks limit the requirement and the market requirement that its product production and quality far can not satisfy synthetic single crystal silicon; Supply falls short of demand to we can say on the present home market trichlorosilane, and breach is bigger.
In the polysilicon production process of producing solar-energy photo-voltaic cell level and unicircuit level; Be exactly to utilize trichlorosilane and vinylchlorid or propenyl chloride to react in its organo silane coupling agent; But it requires more than 99.999% the trichlorosilane monomer purity, and wherein the content of elements such as institute's boracic, phosphorus must be below 10ppb.Adopt normal pressure from the pure technology of load in the Siemens trichlorosilane purification separation worker generation in the world at present; Belong to high energy consumption technology; But because trichlorosilane and impurity compound boiling point thereof are lower; So that overhead condenser need adopt 5 ℃ chilled water system, thereby the working cost of this technology and process energy consumption are very high, the facility investment increase is very big and the journey complicated operation.
Chinese patent CN1693192A has proposed method of purification and the device thereof that single tower separates trichlorosilane; But in its raw material to contain light constituent content such as boron, phosphorus on a small quantity higher; Though can satisfy the requirement of solar battery grade polysilicon; But still there are a little weak points in its quality, and the separation efficiency of whole process is lower, energy consumption is bigger; Chinese patent CN1010455362A has proposed the technology that double tower separates trichlorosilane, but its technology falls behind so that exist product index unstable, and its working pressure is that normal pressure makes whole technology need that a large amount of freezing consequently the process energy consumption is not bigger in addition; Chinese patent CN2008100506.1 has proposed the tripping device and the method for highly efficient distilling purify trichlorosilane, but its trichlorosilane that is primarily aimed at more than 99.5% is a raw material.Therefore present domestic also efficiently the purification to the trichlorosilane in the high-boiling and low-boiling components separated the technology and the device of trichlorosilane.
The utility model content
In view of this; The purpose of the utility model provides the tripping device of trichlorosilane in a kind of high-boiling and low-boiling components of purifying; Trichlorosilane product gas purity after purifying can reach more than 99.99%, has the advantage that design variable is reasonable in the purify trichlorosilane technology from high-boiling and low-boiling components, facility investment is little and energy consumption is less and separation rate is high.
The technical scheme of the utility model realizes with following method:
The tripping device of trichlorosilane in a kind of high-boiling and low-boiling components of purifying; Mainly comprise head tank, fresh feed pump, reboiler, overhead condenser, return tank, reflux pump and high-efficient spiral-screen column; Wherein, The discharge end of head tank is connected with the feed end of fresh feed pump through pipeline, and the discharge end of fresh feed pump is connected with the feed end of rectifying tower through pipeline, and the rectifying tower top is provided with overhead condenser; The rectifying tower below is connected with reboiler with the trichlorosilane jar respectively through pipeline; The outlet of overhead condenser is connected with the import of return tank through pipeline, and return tank is connected with dichloro-dihydro silicon storage tank with reflux pump respectively through pipeline, and reflux pump is connected with reboiler with dichloro-dihydro silicon storage tank, silicon tetrachloride storage tank respectively through pipeline.
Efficient structured packing and sieve plate are housed in the rectifying tower.
The number of plies of sieve plate is 55-60 layers.
Reboiler is horizontal.
Overhead condenser is a floating head type.
Use the method for trichlorosilane in the tripping device purification high-boiling and low-boiling components, its step is following:
1) high-boiling and low-boiling components that, contains trichlorosilane gets into the high-efficient spiral-screen column middle and lower part via head tank through fresh feed pump; Cat head material vapour line links to each other with overhead condenser; Liquid phase is back to the highly efficient distilling column overhead through reflux pump after the condensation, and horizontal reboiler uses thermal oil that heat is provided.
2), dichloro-dihydro silicon, boron trichloride and methyl phosphuret-(t)ed hydrogen low-boiler in the raw material all reflux again, via reflux pump part extraction to dichloro-dihydro silicon storage tank, major part is back to high-efficient spiral-screen column, reflux ratio is 25:1.
3), in the extraction of dichloro-dihydro silicon after can not satisfy technic index, when being circulated to side line extraction place temperature to 68 ℃, the extraction trichlorosilane reaches 99.99% back and gets into the trichlorosilane storage tank, finishes the trichlorosilane extraction herein during temperature variation.
4), when horizontal reboiler temperature reaches 96 ℃ at the bottom of the tower, rely on tower self pressure that high boiling material such as four phosphorus chloride, methyl-monosilane, boron trichloride silicon tetrachloride are delivered to the silicon tetrachloride tundish.
The positively effect of the technical scheme of the utility model is:
The high-efficient spiral-screen column tower body and the column internals of the utility model are 304 materials, and efficient structured packing of interior dress and sieve plate are to guarantee the side line liquid phase extraction of quality product and trichlorosilane.
The utility model has improved the boiling point of each cut through system is carried out compression rectification, makes it boiling-point difference apart from widening, and separation and purification efficient is more efficient.And through after the utility model technology; Water of condensation circulation cryogenic refrigeration systems can be used industrial circulating water, has significantly reduced facility investment and the process heat exchange efficiency is greatly improved, and in the utility model, has used floating head condenser as overhead condenser simultaneously; Horizontal reboiler substitutes vertical reboiler; Reduce structure deteriorate rate and potential safety hazard, changed the convention of the condenser tube sheet weld leakiness of trichlorosilane industry, improved service life of equipment.
The advantage of the utility model is to design through reasonably optimizing; And utilize trichlorosilane separating technology and device solves thereof in the efficient thermal coupling rectification and purification high-boiling and low-boiling components perplex the chlorosilane industry always high-boiling and low-boiling components handle a difficult problem, reduced the waste of trichlorosilane and discharged the environmental pollution that brings with high-boiling and low-boiling components.99% dichloro-dihydro silicon and silicon tetrachloride can directly be used in anti-disproportionation system trichlorosilane or the cold and hot hydrogenation system trichlorosilane of silicon tetrachloride.99.99% trichlorosilane can directly be used for the raw materials for production of polysilicon.Have good economic benefit and social benefit.The utility model simple, easy to operate, safety rational in infrastructure, energy consumption is low, the recovery is high, advantage such as pollution-free.
Description of drawings:
Fig. 1 is the structural representation of the utility model.
Embodiment:
Below in conjunction with accompanying drawing the utility model technical scheme is further described.
Can find out by Fig. 1; The tripping device of trichlorosilane in this purification high-boiling and low-boiling components; Mainly comprise head tank 1, fresh feed pump 2, reboiler 3, overhead condenser 5, return tank 6, reflux pump 7 and high-efficient spiral-screen column 4, wherein, the discharge end of head tank 1 is connected with the feed end of fresh feed pump 2 through pipeline; The discharge end of fresh feed pump 2 is connected with the feed end of high-efficient spiral-screen column 4 through pipeline; High-efficient spiral-screen column 4 tops are provided with overhead condenser 5, and high-efficient spiral-screen column 4 belows are connected with reboiler 3 with trichlorosilane jar 9 respectively through pipeline, and the outlet of overhead condenser 5 is connected with the import of return tank 6 through pipeline; Return tank 6 is connected with dichloro-dihydro silicon storage tank 8 with reflux pump 7 respectively through pipeline, and reflux pump 7 is connected with dichloro-dihydro silicon storage tank 8, silicon tetrachloride storage tank 10 and reboiler 3 respectively through pipeline.
Be provided with efficient structured packing and sieve plate in the said high-efficient spiral-screen column 4.
Operational condition is that the cat head working pressure of high-efficient spiral-screen column 4 is 200-205kpa, and tower top temperature is 41.8-42.5C, and side line extraction place temperature is 67.6-68.5C, and column bottom temperature is 95.8-96.3C, and the number of plies of sieve plate is 58 layers.
Use the method for trichlorosilane in the tripping device purification high-boiling and low-boiling components, its step is following:
The first step, the high-boiling and low-boiling components that contains trichlorosilane get in the high-efficient spiral-screen columns 4 through fresh feed pump 2 via head tank 1; Cat head material vapour line links to each other with overhead condenser 5; Liquid phase is back to high-efficient spiral-screen column 4 cats head through reflux pump 7 after the condensation, and reboiler 3 uses thermal oil that heat is provided.
Dichloro-dihydro silicon, boron trichloride and methyl phosphuret-(t)ed hydrogen low-boiler in second step, the raw material are qualified in total reflux; Technic index temperature 41.8C, pressure 200kpa is via reflux pump 7 a part of extraction to dichloro-dihydro silicon storage tanks 8; Major part is back to high-efficient spiral-screen column 4, reflux ratio 25:1.
The 3rd step, in the extraction of dichloro-dihydro silicon after can not satisfy technic index, when being circulated to side line extraction place temperature to 68C, the extraction trichlorosilane reaches 99.99% back and gets into trichlorosilane storage tank 9, finishes the trichlorosilane extraction herein during temperature variation.
The 4th step, when reboiler 3 temperature reach 96C, rely on self pressure of high-efficient spiral-screen column 4 that high boiling material such as four phosphorus chloride, methyl-monosilane, boron trichloride silicon tetrachloride are delivered to silicon tetrachloride tundish 10.
Claims (5)
1. the tripping device of trichlorosilane in the high-boiling and low-boiling components of purifying; Mainly comprise head tank (1), fresh feed pump (2), reboiler (3), overhead condenser (5), return tank (6), reflux pump (7) and high-efficient spiral-screen column (4); It is characterized in that: the discharge end of head tank (1) is connected with the feed end of fresh feed pump (2) through pipeline; The discharge end of fresh feed pump (2) is connected with the feed end of high-efficient spiral-screen column (4) through pipeline; High-efficient spiral-screen column (4) top is provided with overhead condenser (5); High-efficient spiral-screen column (4) below is connected with reboiler (3) with trichlorosilane jar (9) respectively through pipeline; The outlet of overhead condenser (5) is connected with the import of return tank (6) through pipeline, and return tank (6) is connected with dichloro-dihydro silicon storage tank (8) with reflux pump (7) respectively through pipeline, and reflux pump (7) is connected with dichloro-dihydro silicon storage tank (8), silicon tetrachloride storage tank (10) and reboiler (3) respectively through pipeline.
2. the tripping device of trichlorosilane in the purification high-boiling and low-boiling components according to claim 1 is characterized in that: high-efficient spiral-screen column is provided with efficient structured packing and sieve plate in (4).
3. the tripping device of trichlorosilane in the purification high-boiling and low-boiling components according to claim 2, it is characterized in that: the number of plies of sieve plate is 55-60 layers.
4. the tripping device of trichlorosilane in the purification high-boiling and low-boiling components according to claim 1 is characterized in that: reboiler (3) is for horizontal.
5. the tripping device of trichlorosilane in the purification high-boiling and low-boiling components according to claim 1 is characterized in that: overhead condenser (5) is a floating head type.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011203477828U CN202246101U (en) | 2011-09-16 | 2011-09-16 | Trichlorosilane separation device for purification of substance with high/low boiling point |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011203477828U CN202246101U (en) | 2011-09-16 | 2011-09-16 | Trichlorosilane separation device for purification of substance with high/low boiling point |
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| CN202246101U true CN202246101U (en) | 2012-05-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2011203477828U Expired - Fee Related CN202246101U (en) | 2011-09-16 | 2011-09-16 | Trichlorosilane separation device for purification of substance with high/low boiling point |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104474730A (en) * | 2014-11-20 | 2015-04-01 | 新疆中泰化学股份有限公司 | VCM (Vinyl Chloride Monomer) rectification separation device special for high-boiling residues and separation method |
-
2011
- 2011-09-16 CN CN2011203477828U patent/CN202246101U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104474730A (en) * | 2014-11-20 | 2015-04-01 | 新疆中泰化学股份有限公司 | VCM (Vinyl Chloride Monomer) rectification separation device special for high-boiling residues and separation method |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120530 Termination date: 20130916 |