CN201809177U - Rectifying equipment for purifying trichlorosilane - Google Patents
Rectifying equipment for purifying trichlorosilane Download PDFInfo
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- CN201809177U CN201809177U CN2010205501390U CN201020550139U CN201809177U CN 201809177 U CN201809177 U CN 201809177U CN 2010205501390 U CN2010205501390 U CN 2010205501390U CN 201020550139 U CN201020550139 U CN 201020550139U CN 201809177 U CN201809177 U CN 201809177U
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The utility model discloses rectifying equipment for purifying trichlorosilane, belonging to the technical field of trichlorosilane rectification and purification. The rectifying equipment comprises a preliminary tower, a trichlorosilane rectification tower and a silicon tetrachloride rectification tower which are respectively guide screen plate towers; and two-stage condensers are respectively arranged at the tops of the towers. The utility model has the advantages of high capacity and efficiency, low pressure drop, simple structure, low manufacturing cost, strong capability of resisting the blockage and the like.
Description
Technical field
The utility model belongs to trichlorosilane rectification and purification technical field, is specifically related to a kind of rectifying device of purify trichlorosilane.
Background technology
Trichlorosilane is the important source material of producing solar level and microelectronics level polysilicon, also is the important intermediate of synthesizing organo-silicon simultaneously.Polysilicon is most important, the most basic functional material of semi-conductor industry, electronics and information industry, solar-energy photo-voltaic cell industry, and organosilicon is a new type chemical material, and Application Areas is extensive.For promoting the sustained and rapid development of China's photovoltaic industry and electronics and information industry, National Development and Reform Committee has listed " catalogue is instructed in the renewable resources industry development " in " technological development of photovoltaic silicon materials ".At present, the technical process of domestic production trichlorosilane is roughly as follows: hydrogen chloride gas after the dehydration and dried silicon powder generate mixed gass such as trichlorosilane, silicon tetrachloride and dichloro-dihydro silicon at fluidized bed type synthetic furnace internal reaction, gas reclaims remaining silica flour through cyclonic separator and sack cleaner, clean gas is delivered to condenser system, the chlorosilane that condensation is got off is delivered to distillation system with liquid form, isolate trichlorosilane and silicon tetrachloride product by rectifying tower, uncooled tail gas is delivered to exhaust gas recovery system.In rectification working process, present domestic main employing normal pressure process for separating and purifying (two towers purify continuously separation).This technology is in when operation, and cat head needs freeze system with 7 ℃ of water-cooleds that involve great expense, and the energy consumption height, product yield is low, product purity is low, can only satisfy the low and middle-end demand, can not satisfy the demand of high purity product.
The utility model content
The technical problems to be solved in the utility model is cutting down the consumption of energy of facing of present trichlorosilane production, reduces and pollutes, and the four problems that improves the quality, enhances production capacities provides a kind of rectifying device of purify trichlorosilane.
For solving the problems of the technologies described above, the technical solution adopted in the utility model is as follows:
The rectifying device of purify trichlorosilane of the present utility model, comprise pre-tower, trichlorosilane rectifying tower and silicon tetrachloride rectifying tower, pre-tower fresh feed pump is connected with pre-tower opening for feed, pre-column overhead is provided with pre-tower first-stage condenser and pre-tower secondary condenser, pre-tower first-stage condenser condensate outlet is connected with pre-tower return tank opening for feed, pre-tower return tank discharge port is connected with pre-tower refluxing opening, and pre-tower secondary condenser condensate outlet is connected with dichloro-dihydro silicon finished product jar; The air outlet of pre-tower secondary condenser is connected with surge tank before the machine by pipeline.
Discharge port connects trichlorosilane feed chute, trichlorosilane fresh feed pump successively at the bottom of the pre-Tata; The trichlorosilane fresh feed pump is connected with trichlorosilane rectifying tower opening for feed.Trichlorosilane rectifying tower top is provided with trichlorosilane rectifying tower first-stage condenser and trichlorosilane rectifying tower secondary condenser, trichlorosilane rectifying tower first-stage condenser all is connected with backflash with the condensate outlet of trichlorosilane rectifying tower secondary condenser, the backflash liquid outlet is connected with trichlorosilane rectifying tower refluxing opening, and another liquid outlet connects trichlorosilane finished product jar.The air outlet of trichlorosilane rectifying tower secondary condenser is connected with surge tank before the machine by pipeline.
Discharge port connects silicon tetrachloride feeding groove, silicon tetrachloride feeding pump successively at the bottom of the trichlorosilane rectifying Tata, and the silicon tetrachloride feeding pump is connected with silicon tetrachloride rectifying tower opening for feed.Silicon tetrachloride rectifying tower top is provided with silicon tetrachloride rectifying tower first-stage condenser and silicon tetrachloride rectifying tower secondary condenser, silicon tetrachloride rectifying tower first-stage condenser all is connected with return tank with the condensate outlet of silicon tetrachloride rectifying tower secondary condenser, the return tank liquid outlet is connected with silicon tetrachloride rectifying tower refluxing opening, and another liquid outlet connects silicon tetrachloride finished product jar; The air outlet of silicon tetrachloride rectifying tower secondary condenser is connected with surge tank before the machine by pipeline.
Described pre-tower is a guide sieve-plate tower, and stage number is 22～26, and pre-tower bottom is provided with pre-tower reboiler.
Described trichlorosilane rectifying tower is a guide sieve-plate tower, and stage number is 38～42, and the trichlorosilane rectifier bottoms is provided with trichlorosilane rectifying tower reboiler.
Described silicon tetrachloride rectifying tower is a guide sieve-plate tower, and stage number is 38～42, and tetrachloro hydrogen silicon rectifier bottoms is provided with silicon tetrachloride rectifying tower reboiler.
The utility model adopts pre-tower, trichlorosilane tower, the three tower cascade connected continuous compression rectification technology of silicon tetrachloride tower, separates most of light impurity component of sloughing in the raw material by pre-tower; By the trichlorosilane tower trichlorosilane is separated with silicon tetrachloride, cat head obtains the trichlorosilane product, and the material of tower still enters the silicon tetrachloride tower; The silicon tetrachloride tower steams the product silicon tetrachloride.The continuous compression rectification technology of this multitower, rectifying tower service temperature and pressure raise one by one, and its energy consumption only is original 1/3, and energy-conservation amplitude reaches 60%, and energy-saving effect is obvious.Owing to be the continuous rectification technology, this technology also makes output be greatly improved in energy-conservation.
Adopt national new and high technology high-efficiency guide sieve-plate tower in the rectifying, guide sieve-plate tower is a kind of new enhanced sieve-tray tower, has characteristics such as production capacity is big, efficient is high, pressure drop is low, simple in structure, cheap, anti-stifled ability is strong.Increase pilot hole on the sieve plate of tower, can improve the flow operating mode of gas on the column plate, liquid, prolonged the movement locus of gas entrainment droplet, reduced entrainment, improved gas flow rate and throughput.
Because the technique scheme that the utility model adopts, the beneficial effect that has is as follows:
1) the energy-efficient rectifying tower that is meant has adopted high-efficiency guide sieve-plate tower, a large amount of sieve apertures and small part pilot hole have been offered on this Tata plate, gas by sieve aperture on column plate with the liquid cross-flow, pass the liquid layer vertical uplift, gas by Linde sieve tray, advance along the column plate level, with the liquid of momentum transfer to horizontal flow on the column plate, thereby promote liquid uniform and stable advancing on column plate, liquid level drop and backmixing of liquid phase on the original column plate have been overcome, improve throughput and tray efficiency, solved problems such as stifled tower, liquid flooding.
2) the continuous compression rectification of multitower is meant and adopts pre-tower, trichlorosilane tower and the continuous compression rectification of silicon tetrachloride tower three towers, and three pressure towers raise gradually, produce dichloro-dihydro silicon, trichlorosilane, silicon tetrachloride product respectively according to mixture boiling point difference.Through pressurization, the boiling-point difference of trichlorosilane and silicon tetrachloride increases, and is easier to separate, and the overhead water cooler just can satisfy processing requirement with ordinary cycle water, and compression rectification greatly reduces the production cost of trichlorosilane.
Description of drawings
Fig. 1 is a structural representation of the present utility model.
Embodiment
As shown in Figure 1, the rectifying device of purify trichlorosilane of the present utility model comprises pre-tower 3, trichlorosilane rectifying tower 10 and silicon tetrachloride rectifying tower 17, and pre-tower fresh feed pump 1 is connected with pre-tower opening for feed.Pre-tower 3 cats head are provided with pre-tower first-stage condenser 4 and pre-tower secondary condenser 5, pre-tower first-stage condenser 4 condensate outlets are connected with pre-tower return tank 6 opening for feeds, pre-tower return tank 6 discharge ports are connected with pre-tower 3 refluxing openings, and pre-tower secondary condenser 5 condensate outlets are connected with dichloro-dihydro silicon finished product jar 22.The air outlet of pre-tower secondary condenser 5 is connected with surge tank 25 before the machine by pipeline.
Discharge port connects trichlorosilane feed chute 7, trichlorosilane fresh feed pump 8 successively at the bottom of the pre-Tata; Trichlorosilane fresh feed pump 8 is connected with trichlorosilane rectifying tower 10 opening for feeds, trichlorosilane rectifying tower 10 tops are provided with trichlorosilane rectifying tower first-stage condenser 11 and trichlorosilane rectifying tower secondary condenser 12, the condensate outlet of trichlorosilane rectifying tower first-stage condenser 11 and trichlorosilane rectifying tower secondary condenser 12 all is connected with backflash 13, backflash 13 liquid outlets are connected with trichlorosilane rectifying tower refluxing opening, and another liquid outlet connects trichlorosilane finished product jar 23; The air outlet of trichlorosilane rectifying tower secondary condenser 12 is connected with surge tank 25 before the machine by pipeline.
Discharge port connects silicon tetrachloride feeding groove 14 successively at the bottom of the trichlorosilane rectifying Tata, silicon tetrachloride feeding pump 15, silicon tetrachloride feeding pump 15 is connected with silicon tetrachloride rectifying tower 17 opening for feeds, silicon tetrachloride rectifying tower 17 tops are provided with silicon tetrachloride rectifying tower first-stage condenser 18 and silicon tetrachloride rectifying tower secondary condenser 19, the condensate outlet of silicon tetrachloride rectifying tower first-stage condenser 18 and silicon tetrachloride rectifying tower secondary condenser 19 all is connected with return tank 20, return tank 20 liquid outlets are connected with silicon tetrachloride rectifying tower refluxing opening, and another liquid outlet connects silicon tetrachloride finished product jar 24; The air outlet of silicon tetrachloride rectifying tower secondary condenser 13 is connected with surge tank 25 before the machine by pipeline.
Described pre-tower is a guide sieve-plate tower, and stage number is 22～26, and pre-tower bottom is provided with pre-tower reboiler 2.
Described trichlorosilane rectifying tower is a guide sieve-plate tower, and stage number is 38～42, and the trichlorosilane rectifier bottoms is provided with trichlorosilane rectifying tower reboiler 9.
Described silicon tetrachloride rectifying tower is a guide sieve-plate tower, and stage number is 38～42, and tetrachloro hydrogen silicon rectifier bottoms is provided with silicon tetrachloride rectifying tower reboiler 16, and reboiler 16 discharge port bottoms emit the high boiling material raffinate, remove raffinate storage tank 21.
Principle of work of the present utility model is as follows:
As shown in Figure 1, the trichlorosilane concentration of sending here from synthesizing section is that about 85% thick synthetic liquid is thrown pre-tower 3 top opening for feeds into by pre-tower fresh feed pump 1, described pre-tower is a guide sieve-plate tower, stage number is 22～26, cat head pressure is 60～70KPa, tower top temperature is 40～50 ℃, and reflux ratio is 0.1～0.3.Pre-tower bottom reboiler 2 adopts 500Kpa saturation steam indirect heating liquid crude trichlorosilane, pre-cat head is provided with the condensed in two stages device, it is 5～7 ℃ that the first-stage condenser tube side feeds temperature, pressure is the refrigerated water of 400～500 Kpa, it is-25～-30 ℃ that the secondary condenser tube side feeds temperature, and pressure is the chilled brine of 400～500 Kpa.The liquid that gets off from 4 condensations of one-level condenser advances pre-tower return tank 6, utilizes the potential difference of return tank, and liquid enters in the tower as phegma.Lower boiling dichloro-dihydro silicon is difficult for being condensed at pre-top of tower, enters secondary condenser 5 with gas form, with lower temperature its condensation is got off, and enters dichloro-dihydro silicon product storage tank by pipeline.
Liquid after pre-tower removes dichloro-dihydro silicon enters trichlorosilane rectifying tower 10 middle part opening for feeds by trichlorosilane tower feed chute 7, trichlorosilane tower fresh feed pump 8 successively at the bottom of tower, described trichlorosilane rectifying tower is a guide sieve-plate tower, stage number is 38～42, cat head pressure is 180～200KPa, tower top temperature is 60～70 ℃, and reflux ratio is 10～14.Trichlorosilane rectifying tower reboiler 9 usefulness chucks feed 500KPa steam indirect heating material, strict control column bottom temperature.Be provided with the condensed in two stages device at trichlorosilane rectifying tower cat head, it is 20～25 ℃ that the first-stage condenser tube side feeds temperature, and pressure is the process water of 400～500 Kpa, and it is 5～7 ℃ that the secondary condenser tube side feeds temperature, and pressure is the refrigerated water of 400～500 Kpa.Trichlorosilane rectifying tower cat head material steam enters first-stage condenser 11, secondary condenser 12, phlegma flows into backflash 13, liquid utilizes most of backflow of potential difference to enter the trichlorosilane rectifying tower as phegma in the backflash 13, and small portion removes the trichlorosilane storage tank as product.
High boiling substance enters silicon tetrachloride feeding groove 14 at the bottom of by tower at the bottom of the trichlorosilane rectifying Tata, squeezes into silicon tetrachloride rectifying tower 17 middle part opening for feeds by silicon tetrachloride feeding pump 15.Described tetrachloro hydrogen silicon rectifying tower is a guide sieve-plate tower, and stage number is 38～42, and cat head pressure is 200～230KPa, and tower top temperature is 80～90 ℃, and reflux ratio is 8～12.Silicon tetrachloride rectifying tower reboiler 16 feeds 500KPa steam heating, strict control tower bottom temp by chuck.Be provided with the condensed in two stages device at silicon tetrachloride rectifying tower cat head, it is 20～25 ℃ that the first-stage condenser tube side feeds temperature, and pressure is the process water of 400～500 Kpa, and it is 5～7 ℃ that the secondary condenser tube side feeds temperature, and pressure is the refrigerated water of 400～500 Kpa.Silicon tetrachloride rectifying tower overhead gas removes silicon tetrachloride column overhead condenser 18,19, and phlegma flows into return tank 20, utilizes the potential difference major part to go into cat head as phegma, and small portion removes tank field silicon tetrachloride storage tank as product.
Some high-boiling-point impurity in the liquid at the bottom of the silicon tetrachloride Tata generally accumulates in reboiler discharge port bottom, therefore, emits the high boiling material raffinate in the discharge port bottom, removes raffinate storage tank 21.
Claims (3)
1. the rectifying device of a purify trichlorosilane, it is characterized in that: comprise pre-tower (3), trichlorosilane rectifying tower (10) and silicon tetrachloride rectifying tower (17), pre-tower fresh feed pump (1) is connected with pre-tower opening for feed, pre-tower (3) cat head is provided with pre-tower first-stage condenser (4) and pre-tower secondary condenser (5), pre-tower first-stage condenser (4) condensate outlet is connected with pre-tower return tank (6) opening for feed, pre-tower return tank (6) discharge port is connected with pre-tower (3) refluxing opening, and pre-tower secondary condenser (5) condensate outlet is connected with dichloro-dihydro silicon finished product jar (22); The air outlet of pre-tower secondary condenser (5) is connected with surge tank (25) before the machine by pipeline;
Discharge port connects trichlorosilane feed chute (7), trichlorosilane fresh feed pump (8) successively at the bottom of the pre-Tata; Trichlorosilane fresh feed pump (8) is connected with trichlorosilane rectifying tower (10) opening for feed, trichlorosilane rectifying tower (10) top is provided with trichlorosilane rectifying tower first-stage condenser (11) and trichlorosilane rectifying tower secondary condenser (12), the condensate outlet of trichlorosilane rectifying tower first-stage condenser (11) and trichlorosilane rectifying tower secondary condenser (12) all is connected with backflash (13), backflash (13) liquid outlet is connected with trichlorosilane rectifying tower refluxing opening, and another liquid outlet connects trichlorosilane finished product jar (23); The air outlet of trichlorosilane rectifying tower secondary condenser (12) is connected with surge tank (25) before the machine by pipeline;
Discharge port connects silicon tetrachloride feeding groove (14) successively at the bottom of the trichlorosilane rectifying Tata, silicon tetrachloride feeding pump (15), silicon tetrachloride feeding pump (15) is connected with silicon tetrachloride rectifying tower (17) opening for feed, silicon tetrachloride rectifying tower (17) top is provided with silicon tetrachloride rectifying tower first-stage condenser (18) and silicon tetrachloride rectifying tower secondary condenser (19), the condensate outlet of silicon tetrachloride rectifying tower first-stage condenser (18) and silicon tetrachloride rectifying tower secondary condenser (19) all is connected with return tank (20), return tank (20) liquid outlet is connected with silicon tetrachloride rectifying tower refluxing opening, and another liquid outlet connects silicon tetrachloride finished product jar (24); The air outlet of silicon tetrachloride rectifying tower secondary condenser (13) is connected with surge tank (25) before the machine by pipeline.
2. the rectifying device of purify trichlorosilane according to claim 1, it is characterized in that: described pre-tower is a guide sieve-plate tower, and stage number is 22～26, and pre-tower bottom is provided with pre-tower reboiler (2).
3. the rectifying device of purify trichlorosilane according to claim 1 and 2, it is characterized in that: described trichlorosilane rectifying tower is a guide sieve-plate tower, and stage number is 38～42, and the trichlorosilane rectifier bottoms is provided with trichlorosilane rectifying tower reboiler (9).
4.The rectifying device of purify trichlorosilane according to claim 3 is characterized in that: described silicon tetrachloride rectifying tower is a guide sieve-plate tower, and stage number is 38～42, and the silicon tetrachloride rectifier bottoms is provided with silicon tetrachloride rectifying tower reboiler (16).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010205501390U CN201809177U (en) | 2010-09-30 | 2010-09-30 | Rectifying equipment for purifying trichlorosilane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010205501390U CN201809177U (en) | 2010-09-30 | 2010-09-30 | Rectifying equipment for purifying trichlorosilane |
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| CN201809177U true CN201809177U (en) | 2011-04-27 |
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| CN2010205501390U Expired - Fee Related CN201809177U (en) | 2010-09-30 | 2010-09-30 | Rectifying equipment for purifying trichlorosilane |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616788A (en) * | 2011-10-27 | 2012-08-01 | 内蒙古神舟硅业有限责任公司 | Trichlorosilane purification and control system |
| CN102795628A (en) * | 2012-08-03 | 2012-11-28 | 东华工程科技股份有限公司 | Improved method for preparing trichlorosilane by using low-pressure synthetic technology |
| CN102794070A (en) * | 2012-07-25 | 2012-11-28 | 新疆大全新能源有限公司 | Processing method for trichlorosilane gas |
| CN103435044A (en) * | 2013-07-19 | 2013-12-11 | 新特能源股份有限公司 | Method for purifying and separating chlorosilane from polysilicon tail gas |
| CN103920300A (en) * | 2013-01-16 | 2014-07-16 | 北京先锋创新科技发展有限公司 | Energy-saving and consumption-reducing method for distillation process |
-
2010
- 2010-09-30 CN CN2010205501390U patent/CN201809177U/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616788A (en) * | 2011-10-27 | 2012-08-01 | 内蒙古神舟硅业有限责任公司 | Trichlorosilane purification and control system |
| CN102794070A (en) * | 2012-07-25 | 2012-11-28 | 新疆大全新能源有限公司 | Processing method for trichlorosilane gas |
| CN102794070B (en) * | 2012-07-25 | 2014-12-10 | 新疆大全新能源有限公司 | Processing method for trichlorosilane gas |
| CN102795628A (en) * | 2012-08-03 | 2012-11-28 | 东华工程科技股份有限公司 | Improved method for preparing trichlorosilane by using low-pressure synthetic technology |
| CN102795628B (en) * | 2012-08-03 | 2014-01-15 | 东华工程科技股份有限公司 | Improved method for preparing trichlorosilane by using low-pressure synthetic technology |
| CN103920300A (en) * | 2013-01-16 | 2014-07-16 | 北京先锋创新科技发展有限公司 | Energy-saving and consumption-reducing method for distillation process |
| CN103435044A (en) * | 2013-07-19 | 2013-12-11 | 新特能源股份有限公司 | Method for purifying and separating chlorosilane from polysilicon tail gas |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110427 Termination date: 20150930 |
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| EXPY | Termination of patent right or utility model |