CN101538045A - Trichlorosilane differential pressure coupling rectification system and operation method thereof - Google Patents
Trichlorosilane differential pressure coupling rectification system and operation method thereof Download PDFInfo
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- CN101538045A CN101538045A CN200910068557A CN200910068557A CN101538045A CN 101538045 A CN101538045 A CN 101538045A CN 200910068557 A CN200910068557 A CN 200910068557A CN 200910068557 A CN200910068557 A CN 200910068557A CN 101538045 A CN101538045 A CN 101538045A
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Abstract
The invention relates to a trichlorosilane differential pressure coupling rectification system and an operation method thereof. The system comprises a low pressure rectifying tower, a pressurizing rectifying tower, a tower kettle reboiler, an overhead condenser and an auxiliary condenser; a condensation reboiler is arranged between the low pressure rectifying tower and the pressurizing rectifying tower, a vapor phase material outlet on the top of the pressurizing rectifying tower is connected with a heating medium inlet of the condensation reboiler, and a heating medium outlet returns to the top of the pressurizing rectifying tower; a liquid phase material outlet at the bottom of the low pressure rectifying tower is connected with a heated medium inlet of the condensation reboiler, and a heated medium outlet returns to the bottom of the low pressure rectifying tower. Raw materials are fed through different towers, so that two sets of process flow can be adopted; the process flow A adopts a low pressure tower as a front tower for removing lightness, and a feeding pump is added for feeding a pressurizing tower; the process flow B adopts the pressurizing tower as the front tower for removing lightness, and the feeding pump is not needed to be added for feeding the low pressure tower. The invention greatly reduces the production cost and energy consumption, and saved energy by about 40% in rectification. The technology remarkably improves the market competitiveness of the polysilicon material.
Description
Technical field
The present invention relates to the distillation technology field, particularly relate to trichlorosilane differential pressure coupling rectification system and working method.
Background technology
Polysilicon is a main raw material of making products such as unicircuit substrate, solar cell.Polysilicon can be used to prepare silicon single crystal, and its deep processed product is widely used in the semi-conductor industry, as the base mateiral of devices such as artificial intelligence, control automatically, information processing, opto-electronic conversion.
The polysilicon of solar level and electronic-grade can be prepared by metallurgical-grade polysilicon, method is that solid-state metallurgical grade silicon is converted into liquid chlorosilanes such as trichlorosilane, then it is carried out rectification and purification and remove wherein impurity, with hydrogen the chlorosilane of purifying is reduced to elemental silicon again, wherein elemental silicon is the form of polysilicon.Main at present employing rectificating method is reduced to foreign matter content and meets solar level and electronic-grade requirement.Existing trichlorosilane rectifying is the conventional rectification technology, and, reflux ratio many because of theoretical stage makes the power consumption of polysilicon industry very high greatly.
Summary of the invention
Purpose of the present invention is the differential pressure coupling rectification technology that provides trichlorosilane to purify for production of polysilicon, and it adopts two tower serial process, and rectifying tower all adopts pressurized operation, when producing high-purity polycrystalline silicon, energy expenditure is dropped to minimum.
Technology of the present invention is as follows:
Trichlorosilane differential pressure coupling rectification system of the present invention comprises low-pressure distillation tower 2, compression rectification tower 5, tower still reboiler 7, overhead condenser 3 and auxiliary condenser 6; Be provided with a condensation reboiler 4 between two rectifying tower sections, the vapor-phase material outlet of compression rectification column overhead is connected to condensation reboiler 4 heating mediums inlet, and the heating medium outlet turns back to compression rectification tower 5 cats head again; Liquid phase material outlet at the bottom of low-pressure distillation tower 2 towers is connected to condensation reboiler 4 heated mediums inlet, and the heated medium outlet is returned at the bottom of low-pressure distillation tower 2 towers again.
Adopt system of the present invention, raw material can adopt different tower chargings, so can adopt two cover technical process, technical process A adopts lower pressure column to take off gently as preceding tower, and the pressurizing tower charging need add fresh feed pump; Process flow B adopts pressurizing tower to take off gently as preceding tower, and the lower pressure column charging can need not to add fresh feed pump.
The working method of the A technology of employing low-pressure distillation tower (2) charging is as follows:
After trichlorosilane raw material (1) separates through low-pressure distillation tower (2), cat head light constituent A (9) is divided into backflow material A (11) and extraction material A (10) according to certain reflux ratio behind condenser (3), take off light liquid A (12) at the bottom of the tower and be divided into two portions, a part forms the steam A (13) that boils again and returns lower pressure column (2) after condensation reboiler (4) heating, another part is squeezed into pressurizing tower (5) by pump (8), at the bottom of tower, form the height liquid A (14) that boils, a part is returned pressurizing tower (5) after reboiler (7) heating, part extraction, the trichlorosilane gas phase A (15) that cat head forms enters the heating medium inlet of condensation reboiler (4), form feed liquid A (16) after institute's heat requirement and enter auxiliary condenser (6) again and become condensation feed liquid A (17) for the condensation reboiler provides, condensation feed liquid A (a 17) part is returned pressurizing tower (5) top, and a part is as trichlorosilane product A (18) extraction.
Under low-pressure distillation Tata still thermal load and the suitable situation of compression rectification column overhead thermal load, auxiliary condenser (6) can need not to open.
Lower pressure column working pressure scope is 0.1～0.3MPa, and pressurizing tower working pressure scope is 0.4～0.8MPa, and two tower pressure differential ranges are 0.2～0.5MPa; The medial temperature of heating medium will be higher than 20～60 ℃ of the medial temperatures of heat-eliminating medium in the condensation reboiler.
The working method of the B technology of employing compression rectification tower (5) charging is as follows:
After trichlorosilane raw material (1) separates through compression rectification tower (5), cat head light constituent B (19) enters the heating medium inlet of condensation reboiler (4), for the condensation reboiler becomes condensation feed liquid B (23) after institute's heat requirement is provided, a part is returned pressurizing tower (5) top, a part of extraction behind auxiliary condenser (6) again.The tower still takes off and returns pressurizing tower (5) after light liquid B (a 21) part heats through tower still reboiler (7), and another part utilizes the pressure difference of two towers, directly enters lower pressure column (2) as charging and separates.The trichlorosilane gas phase B (27) of low pressure cat head refluxes through overhead condenser (a 3) back part, another part is as trichlorosilane product B (28) extraction, tower still heavy constituent B (a 24) part enters at the bottom of the tower heated medium of condensation reboiler (4) and goes into the interruption-forming steam B (22) that boils again and return lower pressure column (2), another part extraction.
Utilize the pressure reduction charging between pressurizing tower and the lower pressure column, need not to be provided with the lower pressure column fresh feed pump.
Lower pressure column working pressure scope is 0.1～0.3MPa, and pressurizing tower working pressure scope is 0.4～0.8Mpa, and two tower pressure differential ranges are 0.2～0.5MPa; The medial temperature of heating medium will be higher than 20～60 ℃ of the medial temperatures of heat-eliminating medium in the condensation reboiler.
Distinctive feature of the present invention is: the gaseous phase materials of the cat head that will pressurize is as the heating medium of condensation reboiler, can save the heating energy loss of tower still reboiler, can save the energy waste of overhead condenser again, and the working pressure of two rectifying tower and pressure reduction are all lower among the flow process A, utilize the working pressure of pressurizing tower that feed liquid is directly squeezed into lower pressure column among the flow process B, saved one group of lower pressure column fresh feed pump and corresponding utility appliance.
Compared with prior art, the present invention has following advantage:
[1] load of pressurization overhead condensation can be complementary with the load of low pressure tower bottom reboiler, realizes thermal coupling rectifying, the coupling heat exchange.
[2] energy expenditure is the main energy consumption place in the distillation operation, and the present invention has compared with prior art realized minimum energy expenditure with differential pressure thermal coupling means substantially.
[3] part technology is taken into account the characteristics that the energy-conservation and differential pressure of differential pressure is economized pump.
Form the characteristics approaching, that temperature is approaching according to the full tower of trichlorosilane rectifying, the present invention proposes a kind of trichlorosilane differential pressure coupling rectification technology and is expected to significantly reduce production costs and energy consumption, Finestill energy-saving about 40%.This technology significantly improves the market competitiveness of polycrystalline silicon material, promotes the development of photovoltaic and information material industrial chain.
Description of drawings
Fig. 1 is the flow process A synoptic diagram of the hot coupling rectification process of trichlorosilane differential pressure.
Fig. 2 is the flow process B synoptic diagram of the hot coupling rectification process of trichlorosilane differential pressure.
Embodiment
Below in conjunction with accompanying drawing technology and equipment provided by the present invention is further detailed.
System of the present invention is as follows:
Trichlorosilane differential pressure coupling rectification system of the present invention comprises low-pressure distillation tower 2, compression rectification tower 5, tower still reboiler 7, overhead condenser 3 and auxiliary condenser 6; Be provided with a condensation reboiler 4 between two rectifying tower sections, the vapor-phase material outlet of compression rectification column overhead is connected to condensation reboiler 4 heating mediums inlet, and the heating medium outlet turns back to compression rectification tower 5 cats head again; Liquid phase material outlet at the bottom of low-pressure distillation tower 2 towers is connected to condensation reboiler 4 heated mediums inlet, and the heated medium outlet is returned at the bottom of low-pressure distillation tower 2 towers again.
Example 1:
The working method of the A technology of employing low-pressure distillation tower (2) charging is as follows:
As shown in Figure 1, after trichlorosilane raw material (1) separates through low-pressure distillation tower (2), light constituent A (9) is divided into backflow material A (11) and extraction material A (10) according to certain reflux ratio at cat head behind condenser (3), take off light liquid A (12) at the bottom of the tower and be divided into two portions, a part enters tower still condensation reboiler (4) heating back and forms the height liquid A (13) that boils and return lower pressure column (2), another part enters after pressurizing tower (5) rectifying at the tower still and forms the height liquid A (14) that boils, form the heating medium inlet that trichlorosilane gas phase A (15) enters condensation reboiler (4) at cat head, formed feed liquid A (16) after institute's heat requirement and enter auxiliary condenser (6) and become condensation feed liquid A (17) by the condensation reboiler provides, condensation feed liquid A (a 17) part is returned pressurizing tower (5) top, and a part is as trichlorosilane product A (18) extraction.
In operating process when if the material A (13) in the heating medium exit of condensation reboiler (4) satisfies the trim the top of column temperature of pressurizing tower (5), then auxiliary condenser (6) can be opened.
Technology and equipment of the present invention is applicable to the rectifying of trichlorosilane in the polysilicon production process, in order to illustrate that better the present invention in the advantage aspect saving energy and reduce the cost, chooses an application example and is illustrated.
Process the purification of trichlorosilane in 2000 tons of/year production of polysilicon, feed composition is as follows:
Rectifying workshop section raw material feed composition: the dichloro-dihydro silicone content is 1%; Trichlorosilane content is 98%; Silicon tetrachloride content is 1%.
The lower pressure column working pressure is 0.2KPa, and tower top temperature is 50.7 ℃, and the charging reflux ratio is 14, and the tower theoretical stage is 180; The pressurizing tower tower top pressure is 0.55MPa, and tower top temperature is 88.5 ℃, and the charging reflux ratio is 14, and the tower theoretical stage is 180.
Behind said process, foreign matter content meets the requirement of polycrystalline silicon solar level and electronic-grade silicon production in the high-purity trichlorosilane product of main products.
Each tower load is as shown in the table in the trichlorosilane purification process, because rectifying adopts differential pressure coupled method, so the heating load of lower pressure column and the cooling load of pressurizing tower are complementary, data heat when not setting up the condensation reboiler or cool off needed thermal load in the bracket:
| Cooling load M*KCAL/HR | Heating load M*KCAL/HR | Add up to M*KCAL/HR | |
| Lower pressure column | 1.2537 | (1.2723) | 1.2537(2.5260) |
| Pressurizing tower | (1.2584) | 1.2751 | 1.2751(2.5335) |
| Add up to | 1.2537(2.5121) | 1.2751(2.5474) | 2.5288(5.0595) |
After adding the condensation reboiler, the total thermal load of pressurizing tower and condensing tower is 2.5288M*KCAL/HR, and total thermal load is not 5.0595M*KCAL/HR when not adding the condensation reboiler, conserve energy 50.01%.
Example 2:
The working method of the B technology of employing compression rectification tower (5) charging is as follows:
As shown in Figure 2, the working method of flow process B is: after trichlorosilane raw material (1) separates through compression rectification tower (5), cat head light constituent B (19) enters the heating medium inlet of the condensation reboiler (4) of lower pressure column still, for the condensation reboiler becomes condensation feed liquid B (23) after institute's heat requirement is provided, behind auxiliary condenser (6), a part is returned pressurizing tower (5) top, a part of extraction.The tower still takes off light liquid B (21) and forms the steam (20) that boils again through tower still reboiler (7) heating back and return pressurizing tower (5), and another part utilizes the pressure difference of two towers, directly enters lower pressure column (2) as charging and separates.Behind trichlorosilane gas phase B (27) the process overhead condenser (3) of low pressure cat head, a part refluxes, another part is as the product extraction, heavy constituent B (24) part of tower still enters at the bottom of the tower heated medium of condensation reboiler (4) goes into the interruption-forming steam B (22) that boils again and returns lower pressure column (2), and another part is as the high boiling material extraction.
Technology and equipment of the present invention is applicable to the rectifying of trichlorosilane in the polysilicon production process, in order to illustrate that better the present invention in the advantage aspect saving energy and reduce the cost, chooses an application example and is illustrated.
Process the purification of trichlorosilane in 2000 tons of/year production of polysilicon, feed composition is as follows:
Rectifying workshop section raw material feed composition: the dichloro-dihydro silicone content is 1%; Trichlorosilane content is 98%; Silicon tetrachloride content is 1%.
The lower pressure column working pressure is 0.2MPa, and tower top temperature is 53 ℃, and the charging reflux ratio is 15, and the tower theoretical stage is 180; The pressurizing tower tower top pressure is 0.55MPa, and tower top temperature is 88.5 ℃, and the charging reflux ratio is 14, and the tower theoretical stage is 180.
Behind said process, foreign matter content meets the requirement of polycrystalline silicon solar level and electronic-grade silicon production in the high-purity trichlorosilane product of main products.
Each tower load is as shown in the table in the trichlorosilane purification process, because rectifying adopts differential pressure coupled method, so the cooling load of the heating load of lower pressure column and pressurizing tower is complementary:
| Cooling load M*KCAL/HR | Heating load M*KCAL/HR | Add up to M*KCAL/HR | |
| Lower pressure column | 1.2218 | (1.2716) | 1.2218(2.4934) |
| Pressurizing tower | (1.2049) | 1.2715 | 1.2715(2.4764) |
| Add up to | 1.2218(2.4267) | 1.2715(2.5431) | 2.4933(4.9698) |
After adding the condensation reboiler, the total thermal load of pressurizing tower and condensing tower is 2.4933M*KCAL/HR, and total thermal load is not 4.9698M*KCAL/HR when not adding the condensation reboiler, conserve energy 49.83%.
Trichlorosilane differential pressure coupling rectification system and working method that the present invention proposes, be described by embodiment, person skilled obviously can be changed or suitably change and combination system and method as herein described in not breaking away from content of the present invention, spirit and scope, realizes technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (5)
1. trichlorosilane differential pressure coupling rectification system comprises low-pressure distillation tower (2), compression rectification tower (5), tower still reboiler (7), overhead condenser (3) and auxiliary condenser (6); It is characterized in that being provided with between two rectifying tower sections a condensation reboiler (4), the vapor-phase material outlet of compression rectification column overhead is connected to condensation reboiler (4) heating medium inlet, and the heating medium outlet turns back to compression rectification tower (5) cat head again; Liquid phase material outlet at the bottom of low-pressure distillation tower (2) tower is connected to condensation reboiler (4) heated medium inlet, and the heated medium outlet is returned at the bottom of low-pressure distillation tower (2) tower again.
2. the working method of the trichlorosilane differential pressure coupling rectification system of claim 1, after it is characterized in that trichlorosilane raw material (1) separates through low-pressure distillation tower (2), cat head light constituent A (9) is divided into backflow material A (11) and extraction material A (10) according to certain reflux ratio behind condenser (3), take off light liquid A (12) at the bottom of the tower and be divided into two portions, a part forms the steam A (13) that boils again and returns lower pressure column (2) after condensation reboiler (4) heating, another part is squeezed into pressurizing tower (5) by pump (8), at the bottom of tower, form the height liquid A (14) that boils, a part is returned pressurizing tower (5) after reboiler (7) heating, part extraction, the trichlorosilane gas phase A (15) that cat head forms enters the heating medium inlet of condensation reboiler (4), form feed liquid A (16) after institute's heat requirement and enter auxiliary condenser (6) again and become condensation feed liquid A (17) for the condensation reboiler provides, condensation feed liquid A (a 17) part is returned pressurizing tower (5) top, and a part is as trichlorosilane product A (18) extraction.
3. the working method of trichlorosilane differential pressure coupling rectification system as claimed in claim 2 is characterized in that under low-pressure distillation Tata still thermal load and the suitable situation of compression rectification column overhead thermal load, and auxiliary condenser (6) can need not to open.
4. the working method of the trichlorosilane differential pressure coupling rectification system of claim 1, after it is characterized in that trichlorosilane raw material (1) separates through compression rectification tower (5), cat head light constituent B (19) enters the heating medium inlet of condensation reboiler (4), for the condensation reboiler becomes condensation feed liquid B (23) after institute's heat requirement is provided, a part is returned pressurizing tower (5) top, a part of extraction behind auxiliary condenser (6) again.The tower still takes off and returns pressurizing tower (5) after light liquid B (a 21) part heats through tower still reboiler (7), and another part utilizes the pressure difference of two towers, directly enters lower pressure column (2) as charging and separates.The trichlorosilane gas phase B (27) of low pressure cat head refluxes through overhead condenser (a 3) back part, another part is as trichlorosilane product B (28) extraction, tower still heavy constituent B (a 24) part enters at the bottom of the tower heated medium of condensation reboiler (4) and goes into the interruption-forming steam B (22) that boils again and return lower pressure column (2), another part extraction.
5. as the working method of claim 2 or 4 described trichlorosilane differential pressure coupling rectification systems, it is characterized in that lower pressure column working pressure scope is 0.1～0.3MPa, pressurizing tower working pressure scope is 0.4～0.8Mpa, and two tower pressure differential ranges are 0.2～0.5MPa; The medial temperature of heating medium will be higher than 20～60 ℃ of the medial temperatures of heat-eliminating medium in the condensation reboiler.
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| CN102086409A (en) * | 2010-08-16 | 2011-06-08 | 中国海洋石油总公司 | Cracked gasoline high and low pressure thermal coupling separation technology |
| CN102134080A (en) * | 2011-04-12 | 2011-07-27 | 天津大学 | Heat-pump energy-saving separating device for extracting trichlorosilane by adopting static mixing booster and method |
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