CN116803903A - Natural circulation vertical silicon tetrachloride vaporization system - Google Patents
Natural circulation vertical silicon tetrachloride vaporization system Download PDFInfo
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- CN116803903A CN116803903A CN202310690492.0A CN202310690492A CN116803903A CN 116803903 A CN116803903 A CN 116803903A CN 202310690492 A CN202310690492 A CN 202310690492A CN 116803903 A CN116803903 A CN 116803903A
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- Prior art keywords
- silicon tetrachloride
- vaporizer
- separation tank
- liquid separation
- gas
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- 239000005049 silicon tetrachloride Substances 0.000 title claims abstract description 117
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 238000009834 vaporization Methods 0.000 title claims abstract description 32
- 230000008016 vaporization Effects 0.000 title claims abstract description 31
- 239000006200 vaporizer Substances 0.000 claims abstract description 45
- 239000001257 hydrogen Substances 0.000 claims abstract description 39
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 238000000926 separation method Methods 0.000 claims abstract description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007791 liquid phase Substances 0.000 claims abstract description 15
- 150000002431 hydrogen Chemical class 0.000 claims description 14
- 238000000034 method Methods 0.000 abstract description 13
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 8
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 8
- 229920005591 polysilicon Polymers 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 2
- 239000005052 trichlorosilane Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000011874 heated mixture Substances 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention discloses a natural circulation vertical silicon tetrachloride vaporization system, and belongs to the technical field of polysilicon production. The system comprises a silicon tetrachloride vaporizer and a silicon tetrachloride gas-liquid separation tank, wherein the bottom of the silicon tetrachloride vaporizer is connected with a hydrogen feeding pipeline, the top of the silicon tetrachloride vaporizer is connected with the middle of the silicon tetrachloride gas-liquid separation tank through a silicon tetrachloride vaporizer outlet pipeline, the output end of the bottom of the silicon tetrachloride gas-liquid separation tank is connected with the bottom of the silicon tetrachloride vaporizer, and the upper part of the silicon tetrachloride gas-liquid separation tank is also connected with a liquid phase silicon tetrachloride pipeline. Aiming at the defects of high silicon tetrachloride vaporization temperature and serious vibration of a kettle type heat exchanger in the cold hydrogenation process, the method and the device can effectively reduce energy consumption and ensure the stable operation of the device.
Description
Technical Field
The invention relates to the technical field of polysilicon production, in particular to a natural circulation vertical silicon tetrachloride vaporization system.
Background
Under the conditions that the energy source is increasingly stressed and the environmental pressure is increasingly increased, the development and the utilization of renewable energy sources are valued by various governments, and the search for a pollution-free green energy source becomes urgent. Compared with other energy sources, solar energy has the advantages of cleanness, safety, wide sources, sufficient resources and the like, so that solar photovoltaic power generation is one of the best ways for fundamentally realizing sustainable energy development. Currently, polysilicon is the main raw material for producing solar photovoltaic cells, and its market share is around 90%.
The main technical route for producing the polysilicon at home and abroad is an improved Siemens method, 19-24 tons of trichlorosilane is consumed for producing 1 ton of polysilicon, 15-20 tons of silicon tetrachloride is produced as a byproduct, and the silicon tetrachloride reacts with humid air to generate silicic acid and hydrogen chloride, so that the silicon tetrachloride is directly discharged to seriously pollute the environment and damage the health of human bodies. For the recovery of the byproducts, the cold hydrogenation technology is adopted to convert the byproducts into trichlorosilane, so that the closed cycle of materials in the device is realized, the process flow is optimized, and the effect of zero emission of pollutants is achieved.
The vaporization of the silicon tetrachloride is an important component of the cold hydrogenation technology, and the reasonable vaporization mode of the silicon tetrachloride is selected, so that the vaporization temperature can be effectively reduced, the service life of equipment is prolonged, and the method has important significance for continuous operation of the device.
The traditional vaporization mode mainly comprises electric heating and conduction oil heating, and because the reaction pressure of the cold hydrogenation device is generally maintained at 2-3 MPa, the liquid silicon tetrachloride is completely vaporized at the operation pressure and needs higher temperature, and the energy consumption needed by adopting the electric heating mode is higher. In addition, the raw material silicon tetrachloride generally contains a small amount of metal chloride and other impurities, and the impurities are easy to adhere to the surface of the electric heater, so that the heat transfer efficiency of the vaporizer is reduced. Most of the existing polysilicon enterprises use heat conduction oil as a heat source to heat silicon tetrachloride, but the investment of the heat conduction oil device is large, the heat conduction oil needs to be replaced regularly, and the operation and maintenance costs are high. Meanwhile, the use process of the heat conduction oil needs to be strictly sealed, and once leakage occurs, huge pollution is generated on the whole cold hydrogenation device, and the heat conduction oil is difficult to clean.
At present, the optimized heating mode is to mix and heat liquid-phase silicon tetrachloride and hydrogen first, and because the process is carried out under constant pressure, the partial pressure of the silicon tetrachloride can be reduced by adding the hydrogen, and then the boiling point temperature of the silicon tetrachloride is reduced, so that the final vaporization temperature of the silicon tetrachloride is determined by the hydrogen amount in the mixture, and the production energy consumption is obviously reduced. Patent CN107337211a discloses a vaporization method and vaporization device for silicon tetrachloride in a polysilicon cold hydrogenation method, liquid phase silicon tetrachloride and hydrogen are respectively added into a kettle type vaporizer for mixing under constant pressure, and the silicon tetrachloride is heated by steam to be completely vaporized. The vaporization method and the vaporization device can consume less electric energy, but when the two are mixed and contacted in the heat exchanger, a large amount of liquid-phase silicon tetrachloride is instantaneously vaporized, so that the vaporization device is severely vibrated and is unfavorable for the stable operation of the reaction.
Disclosure of Invention
The invention aims to provide a natural circulation vertical silicon tetrachloride vaporization system, which aims at the defects of high silicon tetrachloride vaporization temperature and serious vibration of a kettle type heat exchanger in a cold hydrogenation process, and by adopting the method and the device, the energy consumption can be effectively reduced, and the stable operation of the device is ensured.
The aim of the invention can be achieved by the following technical scheme:
the natural circulation vertical silicon tetrachloride vaporization system comprises a silicon tetrachloride vaporizer and a silicon tetrachloride gas-liquid separation tank, wherein the bottom of the silicon tetrachloride vaporizer is connected with a hydrogen feeding pipeline, the top of the silicon tetrachloride vaporizer is connected with the middle of the silicon tetrachloride gas-liquid separation tank through a silicon tetrachloride vaporizer outlet pipeline, the output end of the bottom of the silicon tetrachloride gas-liquid separation tank is connected with the bottom of the silicon tetrachloride vaporizer, and the upper part of the silicon tetrachloride gas-liquid separation tank is also connected with a liquid phase silicon tetrachloride pipeline.
The technical scheme of the invention is as follows: the position where the liquid-phase silicon tetrachloride pipeline is connected with the silicon tetrachloride gas-liquid separation tank is higher than the position where the outlet pipeline of the silicon tetrachloride vaporizer is connected with the silicon tetrachloride gas-liquid separation tank.
The technical scheme of the invention is as follows: the hydrogen feed line is connected to a hydrogen distributor.
The technical scheme of the invention is as follows: the hydrogen distributor is positioned at the position from the bottom end socket of the silicon tetrachloride vaporizer to the lower end tube plate.
The technical scheme of the invention is as follows: the distribution pipes in the distributor are uniformly arranged and are provided with 300 to 400 air outlet holes upwards.
The specific working process is as follows: the method comprises the steps of preheating raw material silicon tetrachloride, conveying the preheated raw material silicon tetrachloride to a silicon tetrachloride gas-liquid separation tank, enabling a large amount of silicon tetrachloride circulating liquid to enter a silicon tetrachloride vaporizer under the action of a driving force density difference, enabling preheated hydrogen to enter the vaporizer through a hydrogen distributor, adopting steam as a heat source, finally extracting silicon tetrachloride and hydrogen from the top of the vaporizer in a gas-liquid two-phase mode, conveying the silicon tetrachloride and the hydrogen to the silicon tetrachloride gas-liquid separation tank, realizing gas-liquid two-phase separation in the tank, conveying a gas phase from the top of the tank to downstream equipment for reaction, and enabling the liquid phase to circulate into the vaporizer for heating vaporization.
The invention has the beneficial effects that:
(1) A hydrogen distributor is arranged at the bottom of the vaporizer to realize uniform mixing of silicon tetrachloride and hydrogen in the vaporizer;
(2) Reducing the vaporization temperature of the silicon tetrachloride by adopting a mode of mixing and vaporizing hydrogen in a liquid phase of the silicon tetrachloride;
(3) 1.0MPag saturated steam is used as a heat source, so that the energy consumption is obviously reduced, and the process flow is simplified;
(4) The system has high safety and lower equipment investment;
(5) Small holes are uniformly distributed on the hydrogen distributor to control the flow rate of hydrogen so as to avoid a great amount of hydrogen from entering the vaporizer to produce severe vibration of equipment.
Drawings
FIG. 1 is a process flow diagram of a natural circulation vertical silicon tetrachloride vaporization system provided by the invention.
Wherein, 1-liquid phase silicon tetrachloride pipeline; 2-silicon tetrachloride vaporizer inlet line; 3-hydrogen feed line; a 4-silicon tetrachloride vaporizer outlet line; a 5-silicon tetrachloride gas phase outlet line; 6-silicon tetrachloride vaporizer; 7-silicon tetrachloride gas-liquid separation tank.
Fig. 2 is a schematic diagram of a hydrogen distributor structure.
Detailed Description
The invention is further illustrated below with reference to examples, but the scope of the invention is not limited thereto:
according to the natural circulation vertical silicon tetrachloride vaporization system shown in fig. 1, the system comprises a silicon tetrachloride vaporizer 6 and a silicon tetrachloride gas-liquid separation tank 7, wherein the bottom of the silicon tetrachloride vaporizer 6 is connected with a hydrogen feeding pipeline 3, the top of the silicon tetrachloride vaporizer 6 is connected with the middle part of the silicon tetrachloride gas-liquid separation tank 7 through a silicon tetrachloride vaporizer outlet pipeline 4, the output end of the bottom of the silicon tetrachloride gas-liquid separation tank 7 is connected with the bottom of the silicon tetrachloride vaporizer 6, and the upper part of the silicon tetrachloride gas-liquid separation tank 7 is also connected with a liquid-phase silicon tetrachloride pipeline 1.
The position of the liquid-phase silicon tetrachloride pipeline 1 connected with the silicon tetrachloride gas-liquid separation tank 7 is higher than the position of the silicon tetrachloride vaporizer outlet pipeline 4 connected with the silicon tetrachloride gas-liquid separation tank 7. The hydrogen feed line 3 is connected to a hydrogen distributor. The hydrogen distributor is positioned at the position from the bottom end socket to the lower end tube plate of the silicon tetrachloride vaporizer 6. The distribution pipes in the distributor are uniformly arranged and are provided with 300 to 400 air outlet holes upwards.
The specific working process is as follows: raw material silicon tetrachloride is preheated and then conveyed to a silicon tetrachloride gas-liquid separation tank 7 in a liquid phase form, silicon tetrachloride liquid in the separation tank enters a bottom end enclosure of a silicon tetrachloride vaporizer 6 from the bottom through a pipeline 2, meanwhile, raw material hydrogen is conveyed into the silicon tetrachloride vaporizer 6 through a pipeline 3, a hydrogen distributor is positioned at the position from the bottom end enclosure of the vaporizer to a lower tube plate, and distribution pipes in the distributor are uniformly arranged and upwards provided with 302 phi 15 gas outlet holes, so that hydrogen is uniformly bubbled and ejected in the silicon tetrachloride liquid phase, and vaporization effect of the vaporizer is enhanced. The steam is used as a heat source, the mixture of the silicon tetrachloride and the hydrogen is heated in the vaporizer 6, the heated mixture returns to the silicon tetrachloride gas-liquid separation tank 7 from the top of the tube side of the vaporizer 6, gas-liquid two-phase separation is realized in the separation tank 7, and the silicon tetrachloride and the hydrogen mixed gas are conveyed to the reactor from the top of the separation tank 7 through a pipeline 5 for reaction.
The device has the advantages that the vaporization temperature of the silicon tetrachloride can be flexibly adjusted according to the use amount of the hydrogen, and the partial pressure of the silicon tetrachloride in the gas phase can be reduced by adding the hydrogen under the constant pressure of the system, so that the vaporization temperature of the silicon tetrachloride is reduced. Each polysilicon production unit can flexibly adjust the vaporization temperature of silicon tetrachloride by adopting proper hydrogen consumption according to the vapor grade of the enterprise. In addition, in order to further reduce the vibration problem of the vaporizer, the flow rate of hydrogen can be adjusted by changing the number of pore channels in the hydrogen distributor, so that the vibration phenomenon caused by the instant vaporization of a large amount of silicon tetrachloride when gas-liquid two phases are contacted is avoided, and the cold hydrogenation device is always in a stable operation state.
Claims (5)
1. A natural circulation vertical silicon tetrachloride vaporization system is characterized in that: the system comprises a silicon tetrachloride vaporizer (6) and a silicon tetrachloride gas-liquid separation tank (7), wherein the bottom of the silicon tetrachloride vaporizer (6) is connected with a hydrogen feeding pipeline (3), the top of the silicon tetrachloride vaporizer (6) is connected with the middle of the silicon tetrachloride gas-liquid separation tank (7) through a silicon tetrachloride vaporizer outlet pipeline (4), the output end of the bottom of the silicon tetrachloride gas-liquid separation tank (7) is connected with the bottom of the silicon tetrachloride vaporizer (6), and the upper part of the silicon tetrachloride gas-liquid separation tank (7) is also connected with a liquid-phase silicon tetrachloride pipeline (1).
2. The natural circulation vertical silicon tetrachloride vaporization system of claim 1, wherein: the position of the liquid-phase silicon tetrachloride pipeline (1) connected with the silicon tetrachloride gas-liquid separation tank (7) is higher than the position of the silicon tetrachloride vaporizer outlet pipeline (4) connected with the silicon tetrachloride gas-liquid separation tank (7).
3. The natural circulation vertical silicon tetrachloride vaporization system of claim 1, wherein: the hydrogen feeding pipeline (3) is connected with a hydrogen distributor.
4. The natural circulation vertical silicon tetrachloride vaporization system of claim 3, wherein: the hydrogen distributor is positioned at the position from the bottom end socket to the lower end tube plate of the silicon tetrachloride vaporizer (6).
5. The natural circulation vertical silicon tetrachloride vaporization system of claim 3, wherein: the distribution pipes in the distributor are uniformly arranged and are provided with 300 to 400 air outlet holes upwards.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310690492.0A CN116803903A (en) | 2023-06-09 | 2023-06-09 | Natural circulation vertical silicon tetrachloride vaporization system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310690492.0A CN116803903A (en) | 2023-06-09 | 2023-06-09 | Natural circulation vertical silicon tetrachloride vaporization system |
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| CN116803903A true CN116803903A (en) | 2023-09-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202310690492.0A Pending CN116803903A (en) | 2023-06-09 | 2023-06-09 | Natural circulation vertical silicon tetrachloride vaporization system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117654065A (en) * | 2024-02-02 | 2024-03-08 | 浙江赛勒新能源材料有限公司 | Silicon tetrachloride vaporization system and vaporization process for polysilicon cold hydrogenation device |
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- 2023-06-09 CN CN202310690492.0A patent/CN116803903A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117654065A (en) * | 2024-02-02 | 2024-03-08 | 浙江赛勒新能源材料有限公司 | Silicon tetrachloride vaporization system and vaporization process for polysilicon cold hydrogenation device |
| CN117654065B (en) * | 2024-02-02 | 2024-04-26 | 浙江赛勒新能源材料有限公司 | Silicon tetrachloride vaporization system and vaporization process for polysilicon cold hydrogenation device |
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