CN218741065U - Recovery system for silicon powder-containing emptying gas in cold hydrogenation of polycrystalline silicon - Google Patents
Recovery system for silicon powder-containing emptying gas in cold hydrogenation of polycrystalline silicon Download PDFInfo
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- CN218741065U CN218741065U CN202223156037.2U CN202223156037U CN218741065U CN 218741065 U CN218741065 U CN 218741065U CN 202223156037 U CN202223156037 U CN 202223156037U CN 218741065 U CN218741065 U CN 218741065U
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Abstract
The utility model discloses a cold hydrogenation of polycrystalline silicon contains gaseous recovery system of silica flour unloading belongs to polycrystalline silicon production waste gas recycle technical field, including one-level filter, condenser, vapour and liquid separator and secondary filter, the import of one-level filter's gaseous phase exit linkage condenser, the exit linkage vapour and liquid separator's of condenser feed inlet, vapour and liquid separator's gaseous phase exit linkage secondary filter's import, secondary filter's gaseous phase exit linkage multistage pressure gas conveying line has solved the gas of bleeding in the cold hydrogenation workshop section of prior art and has directly been sent to exhaust-gas treatment system and handle, has the extravagant problem of chlorosilane and hydrogen for polycrystalline silicon manufacturing cost is high.
Description
Technical Field
The utility model belongs to the technical field of polycrystalline silicon production waste gas recycle, concretely relates to cold hydrogenation of polycrystalline silicon contains recovery system of silica flour unloading gas.
Background
At present, a high-pressure silicon powder feeding tank is used in a cold hydrogenation section in polysilicon production, high-pressure hydrogen is used for material pressing, silicon powder in a storage tank is pressed into a hydrogenation furnace for reaction, after the silicon powder in the previous tank is completely emptied, the high-pressure hydrogen in the storage tank needs to be decompressed from high pressure of about 3MPa to a low pressure state of less than 0.1MPa, then the next tank of silicon powder is added, in the existing process, after the silicon powder in the tank is emptied, a valve of a silicon powder discharging pipeline is closed, the high-pressure gas in the tank is fed into a silicon powder filter for filtering and recovering the silicon powder, and the obtained waste gas is directly decompressed into a tail gas leaching device for treatment.
In addition, a silicon powder collecting tank is connected to the lower part of the cyclone separator in the cold hydrogenation chemical industry section, and a silicon powder collecting tank is also connected to the lower part of the silicon powder filter. When the cyclone separator or the silicon powder filter needs to discharge the silicon powder, the silicon powder collecting tank at the lower part needs to be filled with hydrogen to form high pressure, so that the pressure difference between the cyclone separator, the silicon powder filter and the silicon powder collecting tank is reduced, and the excessive abrasion of a pipeline in the silicon powder discharging process is avoided. In the operation process, the pressure difference between the cyclone separator and the silicon powder filter and a silicon powder collecting tank connected with the lower part is generally controlled within the range of 0.3 to 0.5MPa (and the normal operating pressure of the cyclone separator and the silicon powder filter is about 2.6 MPa). In the process of silicon powder blanking, the pressure of the silicon powder collecting tank rises, the pressure difference is reduced, and in order to ensure that the silicon powder blanking is smoother, high-pressure hydrogen (containing silicon powder and chlorosilane) in the silicon powder collecting tank needs to be emptied. In addition, after the silicon powder in the cyclone separator and the silicon powder filter is completely discharged, high-pressure hydrogen containing the silicon powder and chlorosilane in the silicon powder collecting tank needs to be discharged and decompressed to be below 0.1MPa, then nitrogen is used for replacement, then the silicon powder is pressed into a waste storage tank to be cooled and then discharged, and the high-pressure hydrogen containing the silicon powder and chlorosilane is filtered by the silicon powder filter and then directly discharged to a tail gas leaching device.
Therefore, in the traditional treatment process, the chlorosilane is directly sent to the post-treatment system for centralized treatment, so that part of the chlorosilane is wasted, and meanwhile, the treatment pressure of the post-treatment system is increased.
SUMMERY OF THE UTILITY MODEL
The utility model discloses aim at solving among the prior art polycrystalline silicon production cold-hydrogenation workshop section produced bleed gas and directly send to exhaust-gas treatment system and handle, have the extravagant problem of chlorosilane and hydrogen for polycrystalline silicon manufacturing cost is high at present, also leads to the problem that exhaust-gas treatment system pressure is great, treatment cost is higher simultaneously.
In order to achieve the above purpose, the technical solution of the present invention is as follows:
the utility model provides a recovery system that polycrystalline silicon cold hydrogenation contains silicon powder unloading gas, includes one-level filter, condenser, vapour and liquid separator and secondary filter, the import of one-level filter's gaseous phase exit linkage condenser, the exit linkage vapour and liquid separator's of condenser feed inlet, vapour and liquid separator's gaseous phase exit linkage secondary filter's import, secondary filter's gaseous phase exit linkage multistage pressure gas conveying pipeline.
Furthermore, the multistage pressure gas conveying pipeline connected with the gas phase outlet of the secondary filter comprises a three-stage pressure gas conveying pipeline which is respectively a gas conveying pipeline with the pressure of more than 0.6MPa, a gas conveying pipeline with the pressure of 0.1 to 0.6MPa and a gas conveying pipeline with the pressure of less than 0.1 MPa.
Further, pressure gauges are arranged at a gas phase outlet of the secondary filter, a valve I, a valve II and a valve III are respectively arranged on the gas conveying pipeline with the pressure of more than 0.6MPa, the gas conveying pipeline with the pressure of 0.1 to 0.6MPa and the gas conveying pipeline with the pressure of less than 0.1MPa, and the pressure gauges are respectively in control connection with the valve I, the valve II and the valve III.
Further, the gas conveying pipeline with the pressure greater than 0.6MPa is connected with a buffer tank I at the front end of a supplementary hydrogen compressor of the cold hydrogenation section; the gas conveying pipeline of 0.1 to 0.6MPa is connected with a buffer tank II at the front end of a tail gas recovery and regeneration hydrogen compressor; the gas conveying pipeline less than 0.1MPa is connected with a leaching device of the waste gas treatment system.
Further, the filtering precision of the primary filter is 8-15 μm.
Further, the precision of the secondary filter is 1-5 μm.
Furthermore, the material inlet end of the primary filter is connected with the gas phase outlet of the silicon powder feeding tank at the front end of the hydrogenation furnace and is also connected with the gas phase outlet of the silicon powder collecting tank connected with the rear end of the cyclone separator.
The utility model has the advantages that:
1. the utility model discloses in, adopt this recovery system to carry out the prefilter to the gas of releasing of collection, detach most great granule silica flour particle, carry out cooling treatment to the gaseous phase again, make the chlorosilane cooling in the industrial gas be liquid, isolate gaseous phase (mainly for hydrogen) and liquid phase (mainly for chlorosilane) through vapour and liquid separator again, the commodity circulation that contains chlorosilane is collected after gas-liquid separation's liquid phase export is discharged, the gaseous phase that obtains is handled further through secondary filter further again, the silica flour of intercepting less granule, obtain pure hydrogen, hydrogen has certain pressure this moment (gas pressure generally is greater than 0.6 MPa), carry out the hierarchical utilization with this part hydrogen that has pressure.
2. In the utility model, according to the characteristics of the polysilicon production process, the multistage pressure gas conveying pipeline connected with the gas phase outlet of the secondary filter is designed into a three-stage pressure gas conveying pipeline which is respectively a gas conveying pipeline with the pressure of more than 0.6MPa, a gas conveying pipeline with the pressure of 0.1 to 0.6MPa and a gas conveying pipeline with the pressure of less than 0.1MPa, wherein the gas conveying pipeline with the pressure of more than 0.6MPa is used for conveying hydrogen with the pressure of more than or equal to 7 kilograms to a buffer tank I at the front end of a supplementary hydrogen compressor of a cold hydrogenation section; the 0.1 to 0.6MPa gas conveying pipeline is connected with 1~7 kg of hydrogen and is used for conveying the hydrogen to a buffer tank II at the front end of a tail gas recovery and regeneration hydrogen compressor; the gas delivery line less than 0.1MPa is used for delivering hydrogen gas with the pressure less than 1 kilogram to a leaching device connected with a waste gas treatment system. Of course, in actual production, the control parameters of the corresponding gas can be adjusted or the number of hydrogen conveying pipelines can be increased or decreased appropriately according to the hydrogen pressure requirement of the production line.
3. The utility model discloses in, be equipped with the pressure gauge in the gas phase exit of secondary filter, be greater than 0.6MPa gas transmission pipeline, 0.1 to 0.6MPa gas transmission pipeline and be less than and be equipped with valve I, valve II, valve III on the 0.1MPa gas transmission pipeline respectively, the pressure gauge respectively with valve I, valve II, valve III control connection, realize carrying out automatic control to corresponding valve and adjust.
4. The utility model discloses in, the filter fineness of the one-level filter of front end is less than rear end secondary filter's filter fineness, obtains purer hydrogen in order to guarantee the filter effect.
5. In the embodiment, the cooling medium adopted by the condenser is circulating water with the temperature of 7-12 ℃, the industrial gas passing through the condenser 2 is cooled to about 20 ℃, so that chlorosilane in the industrial gas is cooled to be in a liquid state, and the circulating water after heat exchange can be used for other links of polycrystalline silicon production.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Fig. 2 is a schematic structural diagram of another embodiment.
Fig. 3 is a schematic structural diagram of yet another embodiment.
Fig. 4 is a schematic structural view of another preferred embodiment.
FIG. 5 is a schematic structural view of example 6.
Wherein, 1, a first-stage filter; 2. a condenser; 3. a gas-liquid separator; 4. a secondary filter; 5. a gas delivery line greater than 0.6 MPa; 6. gas delivery pipelines of 0.1 to 0.6 MPa; 7. a gas delivery line less than 0.1 MPa; 8. a pressure gauge; 9. a valve I; 10. a valve II; 11. a valve III; 12. a buffer tank I; 13. a buffer tank II; 14. leaching the device; 15. a hydrogenation furnace; 16. a silicon powder feeding tank; 17. a cyclone separator; 18. a silicon powder collection tank; 19. an exhaust gas inlet pipe; 20. a gas recovery line; 21. an exhaust gas discharge line; 22. a hydrogen storage tank; 1.1, a gas phase outlet I;2.1, an inlet I;2.2, an outlet; 3.1, a feed inlet; 3.2, a gas phase outlet II;3.3, a liquid phase outlet; 4.1, an inlet II;4.2, a gas phase outlet III;16.1, a gas phase outlet IV;18.1 and a gas phase outlet IV.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited thereto.
Example 1
The embodiment is the most basic embodiment, and a recovery system for silicon powder-containing vent gas in cold hydrogenation of polycrystalline silicon belongs to the technical field of recycling of waste gas in production of polycrystalline silicon, and refers to fig. 1, and includes a first-stage filter 1, a condenser 2, a gas-liquid separator 3 and a second-stage filter 4, wherein a gas-phase outlet I1.1 of the first-stage filter 1 is connected to an inlet I2.1 of the condenser 2, an outlet I2.2 of the condenser 2 is connected to a feed inlet 3.1 of the gas-liquid separator 3, a gas-phase outlet II3.2 of the gas-liquid separator 3 is connected to an inlet II4.1 of the second-stage filter 4, and a gas-phase outlet III4.2 of the second-stage filter 4 is connected to a multi-stage pressure gas conveying pipeline, as shown in fig. 1, the system includes two-stage pressure gas conveying pipelines such as a gas recovery pipeline 20 and a waste gas discharge pipeline 21, the gas recovery pipeline 20 is used for conveying hydrogen with higher pressure into a hydrogen storage tank 22, and the waste gas discharge pipeline 21 is used for conveying hydrogen with lower pressure into a leaching device 14.
In the embodiment, silicon powder discharge gas generated in a cold hydrogenation section in polysilicon production firstly enters a primary filter 1 through a waste gas inlet pipe 19 for primary filtration, most of large-particle silicon powder is intercepted, the gas is discharged from a gas-phase outlet I1.1 and then enters a condenser 2, the temperature is generally reduced to about 20 ℃, chlorosilane is condensed into liquid, then the liquid chlorosilane is separated through a gas-liquid separator 3, the obtained liquid chlorosilane is discharged from a liquid-phase outlet 3.3 of the gas-liquid separator 3 and collected, the gas phase (mainly hydrogen) obtained after treatment of the gas-liquid separator 3 is continuously sent to a secondary filter 4 for further filtration to obtain pure hydrogen, the hydrogen has certain pressure, the obtained hydrogen is further recycled through a multistage pressure gas conveying pipeline, and finally the hydrogen with lower pressure is sent to a waste gas treatment system for treatment, so that the hydrogen and the chlorosilane in the waste gas can be further utilized.
Example 2
Compared with the embodiment 1, the present embodiment is different in that the multistage pressure gas conveying pipeline connected to the gas phase outlet III4.2 of the two-stage filter 4 includes a three-stage pressure gas conveying pipeline, and referring to fig. 2, the three-stage pressure gas conveying pipeline is a gas conveying pipeline 5 with a pressure greater than 0.6MPa, a gas conveying pipeline 6 with a pressure ranging from 0.1MPa to 0.6MPa, and a gas conveying pipeline 7 with a pressure less than 0.1 MPa.
Preferably, the gas conveying pipeline 5 with the pressure of more than 0.6MPa is connected with a buffer tank I12 at the front end of a supplementary hydrogen compressor of the cold hydrogenation section; the 0.1 to 0.6MPa gas conveying pipeline 6 is connected with a buffer tank II13 at the front end of a tail gas recovery and regeneration hydrogen compressor; the gas delivery line 7 less than 0.1MPa is connected with a leaching device 14 of the waste gas treatment system.
Preferably, a pressure gauge 8 is arranged at a gas phase outlet III4.2 of the secondary filter 4, a valve I9, a valve II10 and a valve III11 are respectively arranged on the gas delivery pipeline 5 with the pressure of more than 0.6MPa, the gas delivery pipeline 6 with the pressure of 0.1 to 0.6MPa and the gas delivery pipeline 7 with the pressure of less than 0.1MPa, referring to fig. 3, the pressure gauge 8 is respectively in control connection with the valve I9, the valve II10 and the valve III11, namely when the pressure gauge 8 detects the pressure at the gas phase outlet III4.2 of the secondary filter 4, the valves on the corresponding pipelines are controlled to be opened, and meanwhile, the valves on other pipelines are controlled to be closed, so that automatic control is realized, the operation is convenient, and the control is accurate.
Example 3
This example is different from example 1-2 in that the primary filter 1 preferably has a filtration accuracy of 8 to 15 μm.
Example 4
This embodiment is different from embodiments 1 to 3 in that the precision of the secondary filter 4 is preferably 1 to 5 μm.
Example 5
The recycling system of the embodiment is further optimized on the embodiment 1, and referring to fig. 4, the difference is that the end of the feeding port 3.1 of the primary filter 1 is connected with a gas phase outlet IV16.1 of a silicon powder feeding tank 16 at the front end of the hydrogenation furnace 15 and is also connected with a gas phase outlet V18.1 of a silicon powder collecting tank 18 connected with the rear end of the cyclone separator 17.
Example 6
In this embodiment, a recovery system for silicon powder-containing vent gas produced by cold hydrogenation of 20 ten thousand tons of trichlorosilane per year is taken as an example, and the technical scheme is further explained, belonging to the technical field of recycling of waste gas in polysilicon production.
The recovery system specifically comprises a primary filter 1, a condenser 2, a gas-liquid separator 3 and a secondary filter 4, referring to fig. 5, wherein a gas-phase outlet I1.1 of the primary filter 1 is connected with an inlet I2.1 of the condenser 2, an outlet I2.2 of the condenser 2 is connected with a feed inlet 3.1 of the gas-liquid separator 3, a gas-phase outlet 3.2 of the gas-liquid separator 3 is connected with an inlet II4.1 of the secondary filter 4, a gas-phase outlet III4.2 of the secondary filter 4 is connected with a three-stage pressure gas conveying pipeline, and the three-stage pressure gas conveying pipeline is a gas conveying pipeline 5 with the pressure of more than 0.6MPa, a gas conveying pipeline 6 with the pressure of 0.1 to 0.6MPa and a gas conveying pipeline 7 with the pressure of less than 0.1 MPa.
In this embodiment, a gas phase outlet III4.2 of the secondary filter 4 is provided with a pressure gauge 8, the gas delivery pipeline 5 with a pressure greater than 0.6MPa, the gas delivery pipeline 6 with a pressure ranging from 0.1MPa to 0.6MPa, and the gas delivery pipeline 7 with a pressure less than 0.1MPa are respectively provided with a valve I9, a valve II10, and a valve III11, and the pressure gauge 8 is respectively in control connection with the valve I9, the valve II10, and the valve III 11.
In this embodiment, the gas delivery line 5 greater than 0.6MPa is connected to a buffer tank I12 at the front end of a make-up hydrogen compressor of the cold hydrogenation section; the 0.1 to 0.6MPa gas conveying pipeline 6 is connected with a buffer tank II13 at the front end of a tail gas recovery and regeneration hydrogen compressor; the gas delivery line 7 less than 0.1MPa is connected with a leaching device 14 of the waste gas treatment system.
In the embodiment, the medium in the condenser 2 is circulating water with the temperature of 7-12 ℃, and the industrial gas passing through the condenser 2 is cooled to about 20 ℃, so that chlorosilane in the industrial gas is cooled to be in a liquid state.
In this embodiment, the filtering precision of the primary filter 1 is 10 μm; the precision of the secondary filter 4 is 1 μm.
In the embodiment, the end of the feeding hole 3.1 of the primary filter 1 is connected with the gas phase outlet IV16.1 of the silicon powder feeding tank 16 at the front end of the hydrogenation furnace 15, and is also connected with a gas phase outlet V18.1 of a silicon powder collecting tank 18 connected with the rear end of the cyclone separator 17.
In this embodiment, the valves I9, II10, and III11 may be any one of a regulating valve and a shut-off valve.
In the embodiment, by adopting the recovery system, hydrogen gas containing silicon powder and silane, which is generated by the silicon powder feeding tank 16 and the silicon powder collecting tank 18, is discharged, primary filtration is performed in the first-stage filter 1, silane is cooled down after passing through the condenser 2, and then chlorosilane liquid is separated and collected through the gas-liquid separator 3, and after passing through the second-stage filter 4, the chlorosilane liquid is recovered in two stages, wherein hydrogen with the pressure of more than or equal to 7 kilograms is recovered to the buffer tank I12 connected with the front end of the cold-hydrogenation supplementary hydrogen compressor through the gas conveying pipeline 5 with the pressure of more than or equal to 0.6 MPa; and (2) sending 1-7 kg of hydrogen to a buffer tank II13 in front of a tail gas recycling and regenerating hydrogen compressor through a gas conveying pipeline 6 with the pressure of 0.1-0.6 MPa for recycling, realizing the respective recycling of silane and hydrogen and the graded recycling of hydrogen, and sending the hydrogen with the pressure of less than 1 kg to a leaching device 14 of a waste gas treatment system for treatment through a gas conveying pipeline 7 with the pressure of less than 0.1 MPa. The production line can recover about 10000Nm of hydrogen 3 A day, 1.5 yuan/Nm in terms of hydrogen cost 3 In addition, the cost can be reduced by 495 ten thousand yuan per year for hydrogen calculated according to 330 days of operation in one year; the recoverable silane amount is about 10 tons/day, the cost of the chlorosilane is 3500 yuan/ton based on the cost of the silicon tetrachloride, and the cost can be reduced by 1155 ten thousand yuan/year based on 330 days of operation in one year.
Claims (7)
1. The utility model provides a recovery system of silicon powder unloading gas is contained in cold hydrogenation of polycrystalline silicon which characterized in that: including one-level filter (1), condenser (2), vapour and liquid separator (3) and secondary filter (4), the import of the gaseous phase exit linkage condenser (2) of one-level filter (1), feed inlet (3.1) of the exit linkage vapour and liquid separator (3) of condenser (2), the import of gaseous phase exit linkage secondary filter (4) of vapour and liquid separator (3), the gaseous phase exit linkage multistage pressure gas conveying pipeline of secondary filter (4).
2. The recovery system for silicon powder-containing vent gas in polysilicon cold hydrogenation according to claim 1, characterized in that: the multistage pressure gas conveying pipeline connected with the gas phase outlet of the secondary filter (4) comprises a three-stage pressure gas conveying pipeline which is a gas conveying pipeline (5) with the pressure of more than 0.6MPa, a gas conveying pipeline (6) with the pressure of 0.1 to 0.6MPa and a gas conveying pipeline (7) with the pressure of less than 0.1 MPa.
3. The recovery system for silicon powder-containing vent gas in polysilicon cold hydrogenation according to claim 2, characterized in that: and a gas phase outlet of the secondary filter (4) is provided with a pressure gauge (8), the gas conveying pipelines (5) with the pressure of more than 0.6MPa, the gas conveying pipelines (6) with the pressure of 0.1 to 0.6MPa and the gas conveying pipelines (7) with the pressure of less than 0.1MPa are respectively provided with a valve I (9), a valve II (10) and a valve III (11), and the pressure gauge (8) is respectively in control connection with the valve I (9), the valve II (10) and the valve III (11).
4. The recovery system of silicon powder-containing vent gas in the cold hydrogenation of polysilicon according to claim 3, characterized in that: the gas conveying pipeline (5) with the pressure of more than 0.6MPa is connected with a buffer tank I (12) at the front end of a supplementary hydrogen compressor of a cold hydrogenation section; the 0.1 to 0.6MPa gas conveying pipeline (6) is connected with a buffer tank II (13) at the front end of the tail gas recovery and regeneration hydrogen compressor; the gas conveying pipeline (7) less than 0.1MPa is connected with a leaching device (14) of the waste gas treatment system.
5. The recovery system for silicon powder-containing vent gas in polysilicon cold hydrogenation according to claim 1, characterized in that: the filtering precision of the primary filter (1) is 8-15 mu m.
6. The recovery system for silicon powder-containing vent gas in polysilicon cold hydrogenation according to claim 1, characterized in that: the precision of the secondary filter (4) is 1-5 mu m.
7. The recovery system for silicon powder-containing vent gas in polysilicon cold hydrogenation according to claim 1, characterized in that: the end of a feed inlet (3.1) of the first-stage filter (1) is connected with a gas phase outlet of a silicon powder feeding tank (16) at the front end of the hydrogenation furnace (15), and is also connected with a gas phase outlet of a silicon powder collecting tank (18) connected with the rear end of the cyclone separator (17).
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| CN202223156037.2U CN218741065U (en) | 2022-11-28 | 2022-11-28 | Recovery system for silicon powder-containing emptying gas in cold hydrogenation of polycrystalline silicon |
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| CN202223156037.2U CN218741065U (en) | 2022-11-28 | 2022-11-28 | Recovery system for silicon powder-containing emptying gas in cold hydrogenation of polycrystalline silicon |
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Assignee: Sichuan Yongxiang Energy Technology Co.,Ltd. Assignor: SICHUAN YONGXIANG NEW ENERGY Co.,Ltd. Contract record no.: X2023510000014 Denomination of utility model: A Recovery System for Vented Gas from Cold Hydrogenation of Polycrystalline Silicon Containing Silicon Powder Granted publication date: 20230328 License type: Common License Record date: 20230816 |
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