CN216155481U - Hydrogen impurity removal system for polycrystalline silicon production and polycrystalline silicon production system - Google Patents
Hydrogen impurity removal system for polycrystalline silicon production and polycrystalline silicon production system Download PDFInfo
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- CN216155481U CN216155481U CN202120971611.6U CN202120971611U CN216155481U CN 216155481 U CN216155481 U CN 216155481U CN 202120971611 U CN202120971611 U CN 202120971611U CN 216155481 U CN216155481 U CN 216155481U
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Abstract
The utility model provides a hydrogen impurity removal system for polycrystalline silicon production and a polycrystalline silicon production system, wherein the impurity removal system comprises an elution tower and a condenser, the lower part of the elution tower is used for storing boiling trichlorosilane, and is provided with an air inlet pipe, and the air inlet pipe is used for introducing hydrogen into the boiling trichlorosilane so as to enable the internal water diversion thereof to react with the trichlorosilane; the upper part of the leaching tower is provided with a spraying structure for atomizing trichlorosilane, gas phase escaping from the boiling trichlorosilane is contacted with the atomized trichlorosilane, and the residual water in the escaping gas phase reacts with the trichlorosilane to obtain dehydrated gas phase; the condenser is connected with the top of the leaching tower and is used for condensing the dehydrated gas phase so as to liquefy the vaporized trichlorosilane therein and obtain the hydrogen with impurities removed. By adopting the method for drying the hydrogen, the moisture in the hydrogen for producing the polysilicon can be dried to be below 1PPm on the premise of not introducing external impurities.
Description
Technical Field
The utility model relates to the technical field of gas purification, in particular to a hydrogen impurity removal system for polycrystalline silicon production and a polycrystalline silicon production system.
Background
Hydrogen is an important chemical raw material and an important fuel, a common preparation method of the hydrogen comprises hydrogen production by a water electrolysis method or hydrogen production by a water gas method, and the prepared hydrogen contains a trace amount of oxygen and moisture impurities regardless of the method, and the quality of the hydrogen is seriously influenced by the existence of the impurities.
In the process of generating trichlorosilane which is a raw material for producing polycrystalline silicon, hydrogen is firstly used as the raw material to synthesize hydrogen chloride, and then the hydrogen chloride reacts with silicon powder to synthesize trichlorosilane, and the existence of oxygen and moisture can influence the conversion rate of trichlorosilane synthesis and the operation efficiency of a system. Therefore, it is important to remove impurities from the hydrogen gas to obtain high-quality hydrogen gas.
In the prior art, water in hydrogen is removed by adopting a cooler in a fluidized manner, or hydrogen containing water vapor is contacted with an adsorbent and trichlorosilane, so that water is adsorbed and absorbed in the adsorbent and the trichlorosilane, and the water is removed and the dew point is reduced. However, the cooling water removal efficiency is limited, and only a part of the water in the hydrogen gas can be removed. When the solid adsorbent or the liquid trichlorosilane is used, external impurities are inevitably brought in, and the quality of the final product polycrystalline silicon is influenced.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem of providing a hydrogen impurity removal system for polysilicon production, which improves the removal rate of water in hydrogen and does not introduce external impurities, and correspondingly provides a polysilicon production system aiming at the defects in the prior art.
The technical scheme adopted for solving the technical problem of the utility model is as follows:
the utility model provides a hydrogen impurity removal system for polysilicon production, which comprises a leaching tower and a condenser,
the lower part of the leaching tower is used for storing the boiled trichlorosilane, and is provided with an air inlet pipe, and the air inlet pipe is used for introducing hydrogen for polycrystalline silicon production into the boiled trichlorosilane so as to enable the internal water diversion thereof to react with the trichlorosilane;
the upper part of the leaching tower is provided with a spraying structure for atomizing and spraying trichlorosilane, gas phase escaping from boiling trichlorosilane is contacted with the atomized trichlorosilane, and residual water in the escaping gas phase is reacted with the trichlorosilane to obtain dehydrated gas phase;
the condenser is connected with the first gas guide pipe at the top of the leaching tower and is used for condensing the dehydrated gas phase so as to liquefy the vaporized trichlorosilane therein, thereby obtaining the purified hydrogen for producing the polycrystalline silicon.
Optionally, a return pipe is arranged between the condenser and the spraying structure and used for guiding the liquefied trichlorosilane into the spraying structure.
Optionally, a catalytic reactor is also included,
and the outlet of the catalytic reactor is connected with the air inlet pipe of the leaching tower and is used for carrying out catalytic oxidation on the hydrogen for producing the polycrystalline silicon before the hydrogen is introduced into the leaching tower so as to convert oxygen in the hydrogen into water.
Optionally, a first discharging pipe is arranged at the bottom of the leaching tower, and a first opening and closing valve is arranged on the first discharging pipe.
Optionally, the system further comprises a flash tank, wherein the flash tank is connected with the first discharge pipe and is used for receiving the solid-phase-containing trichlorosilane discharged from the leaching tower and performing flash evaporation on the trichlorosilane to obtain trichlorosilane vapor.
Optionally, the system further comprises a pressurizer, and the pressurizer is respectively connected with the outlet of the flash tank and the inlet of the elution tower, and is used for receiving the trichlorosilane vapor fed from the flash tank, pressurizing and liquefying the trichlorosilane vapor, and feeding the trichlorosilane vapor back to the elution tower.
Optionally, a second discharging pipe is arranged at the bottom of the flash tank, and a second opening and closing valve is arranged on the second discharging pipe.
Optionally, the device further comprises a reflux pump, wherein the reflux pump is arranged between the spraying structure and the condenser and is used for pressing trichlorosilane liquefied by the condenser into the spraying structure.
Optionally, a reboiler is arranged at the lower part of the elution tower and is used for heating trichlorosilane at the lower part of the elution tower to a temperature above the boiling point of trichlorosilane.
The utility model also provides a polycrystalline silicon production system which comprises a reduction furnace and a material providing unit, wherein the material providing unit comprises the hydrogen impurity removal system for polycrystalline silicon production.
According to the utility model, the intermediate product trichlorosilane in the production of polycrystalline silicon is used as the drying agent for removing impurities from hydrogen, the trichlorosilane in the leaching tower reacts with water in the hydrogen to generate precipitate, HCl and hydrogen, and a small amount of HCl introduced by the dried hydrogen and vaporized trichlorosilane are both raw materials or byproducts in the polycrystalline silicon generation reaction, so that the introduction of external impurities is reduced to the maximum extent, and the quality of the final product polycrystalline silicon is ensured.
And because the water content of the hydrogen for producing the polycrystalline silicon is very low, the utility model leads the hydrogen into the boiling trichlorosilane in the leaching tower, so that the hydrogen is fully contacted with the trichlorosilane in a bubbling mode to ensure that the internal water distribution of the hydrogen is contacted and reacted with the trichlorosilane in a boiling state, gas phase (the hydrogen removing part of the water and trichlorosilane steam generated by the boiling trichlorosilane) escaped from the boiling trichlorosilane is contacted with the trichlorosilane atomized by a spraying structure, and the water in the gas phase can be repeatedly contacted and reacted with the vaporized and atomized trichlorosilane under the action of the lower pressure of the atomized trichlorosilane. Trichlorosilane steam mixed in the dried hydrogen is condensed by a condenser, so that clean hydrogen can be obtained.
Drawings
Fig. 1 is a schematic structural diagram of a hydrogen impurity removal system for polycrystalline silicon production according to embodiment 1 of the present invention.
In the figure: 1. an air inlet pipe; 2. leaching the tower; 21. a spraying structure; 3. a reboiler; 4. a first air duct; 5. a first discharging pipe; 6. a condenser; 7. a return pipe; 8. a second air duct; 9. a catalytic reactor; 10. a flash tank; 11. a pressurizer; 12. a second discharge pipe; 13. a reflux pump; 14. a demister.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are only some embodiments, but not all embodiments, of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the scope of the present invention.
In the description of the present invention, it should be noted that the indication of orientation or positional relationship, such as "on" or the like, is based on the orientation or positional relationship shown in the drawings, and is only for convenience and simplicity of description, and does not indicate or imply that the device or element referred to must be provided with a specific orientation, constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "connected," "disposed," "mounted," "fixed," and the like are to be construed broadly, e.g., as being fixedly or removably connected, or integrally connected; either directly or indirectly through intervening media, or may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood in specific cases for those skilled in the art.
The utility model provides a hydrogen impurity removal system for polysilicon production, which comprises a leaching tower and a condenser,
the lower part of the leaching tower is used for storing the boiled trichlorosilane, and is provided with an air inlet pipe, and the air inlet pipe is used for introducing hydrogen for polycrystalline silicon production into the boiled trichlorosilane so as to enable the internal water diversion thereof to react with the trichlorosilane;
the upper part of the leaching tower is provided with a spraying structure for atomizing and spraying trichlorosilane, gas phase escaping from boiling trichlorosilane is contacted with the atomized trichlorosilane, and residual water in the escaping gas phase is reacted with the trichlorosilane to obtain dehydrated gas phase;
the condenser is connected with the first gas guide pipe at the top of the leaching tower and is used for condensing the dehydrated gas phase so as to liquefy the vaporized trichlorosilane therein, thereby obtaining the purified hydrogen for producing the polycrystalline silicon.
The utility model also provides a polycrystalline silicon production system which comprises a reduction furnace and a material providing unit, wherein the material providing unit comprises the hydrogen impurity removal system for polycrystalline silicon production.
Example 1:
as shown in fig. 1, the embodiment provides a hydrogen impurity removal system for polysilicon production, which includes a leaching tower 2, a condenser 6, a catalytic reactor 9, a flash tank 10 and a pressurizer 11.
The lower part of the leaching tower 2 is used for storing boiled trichlorosilane (31.8 ℃), and is provided with an air inlet pipe 1, and the air inlet pipe 1 is used for introducing hydrogen for polycrystalline silicon production into the boiled trichlorosilane so as to enable internal water diversion to react with the trichlorosilane;
the upper part of the leaching tower 2 is provided with a spraying structure 21 for atomizing and spraying trichlorosilane, gas phase escaping from boiling trichlorosilane is contacted with the atomized trichlorosilane, and residual water in the escaping gas phase is reacted with the trichlorosilane to obtain dehydrated gas phase;
the condenser 6 is connected with the first gas guide pipe 4 at the top of the leaching tower 2 and is used for condensing the gas phase subjected to water removal so as to liquefy the vaporized trichlorosilane therein, thereby obtaining the purified hydrogen for producing the polycrystalline silicon.
The hydrogen source for producing the polysilicon is hydrogen produced by electrolyzing water, hydrogen obtained by electrolyzing salt water and hydrogen produced by water gas.
Therefore, by adopting the intermediate product trichlorosilane in the production of polycrystalline silicon as the drying agent for removing impurities from hydrogen, the trichlorosilane in the leaching tower 2 reacts with water in the hydrogen to generate precipitate, HCl and hydrogen, and a small amount of HCl introduced by the dried hydrogen and the vaporized trichlorosilane are both raw materials or byproducts in the polycrystalline silicon generation reaction, so that the introduction of external impurities is reduced to the maximum extent, and the quality of the final product polycrystalline silicon is ensured.
And because the water content of the hydrogen for producing the polycrystalline silicon is very low, the utility model leads the hydrogen into the boiling trichlorosilane in the leaching tower 2, so that the hydrogen is fully contacted with the trichlorosilane in a bubbling mode to ensure that the internal water distribution of the hydrogen is contacted with the trichlorosilane in a boiling state for reaction, gas phase (the hydrogen removing part of the water and the trichlorosilane steam generated by the boiling trichlorosilane) escaped from the boiling trichlorosilane is contacted with the trichlorosilane atomized by the spraying structure 21, and under the action of the lower pressure of the atomized trichlorosilane, the water energy in the gas phase can be repeatedly contacted with the vaporized and atomized trichlorosilane for reaction, and the practice shows that the utility model can dry the water content in the hydrogen for producing the polycrystalline silicon to be less than 1 PPm. Trichlorosilane steam mixed in the dried hydrogen is condensed by a condenser, so that clean hydrogen can be obtained.
In this embodiment, the reflux pump 13 is arranged between the spraying structure 21 and the condenser 6, and because the spraying structure 21 has a large atomization pressure drop, the reflux pump 13 is used for pressurizing so as to press the trichlorosilane liquefied by the condenser 6 into the spraying structure 21.
In this embodiment, the condenser 6 is provided with a second gas-guide tube 8 for guiding out the purified hydrogen for polysilicon production. The second gas-guide tube 8 is provided with a demister 14 for removing trichlorosilane mist entrained in the hydrogen.
In this embodiment, a return pipe 7 is disposed between the condenser 6 and the spraying structure 21, and is used for guiding liquefied trichlorosilane into the spraying structure 21. On one hand, the trichlorosilane is recycled, and on the other hand, the introduction of external impurities is further reduced.
In this embodiment, an outlet of the catalytic reactor 9 is connected to an air inlet pipe of the elution tower 2, and is used for performing catalytic oxidation on the hydrogen for producing polycrystalline silicon before the hydrogen is introduced into the elution tower 2, so that oxygen in the hydrogen is converted into water. Thereby further reducing impurities in the hydrogen gas which affect the quality of the polysilicon.
In this embodiment, the bottom of the leaching tower 2 is provided with a first discharging pipe 5, and the first discharging pipe 5 is provided with a first opening and closing valve.
In this embodiment, the set value is 25% to 35%.
Solid phase SiO produced by reaction of water in hydrogen for producing polycrystalline silicon and trichlorosilane2All enter into trichlorosilane at the lower part of the leaching tower 2. Due to SiO2The particles are extremely fine and exist in the trichlorosilane liquid in a suspension mode, and when the number of suspended particles is more and more, the flowability of the trichlorosilane is poorer and more, the practice of the applicant shows that when the ratio of the suspended particles to the liquid trichlorosilane is more than about 30 percent, the trichlorosilane containing solid phase is difficult to discharge. Therefore, when off-line sampling detects solid phase SiO in the trichlorosilane containing the solid phase2And when the ratio of the trichlorosilane to the liquid phase reaches a set value, opening a first opening and closing valve to discharge the trichlorosilane containing the solid phase, and adding new trichlorosilane into the leaching tower 2.
In this embodiment, the flash tank 10 is connected to the first discharge pipe 5, and is configured to receive the solid-phase-containing SiO discharged from the leaching tower 22And carrying out flash evaporation on the trichlorosilane, wherein the flash evaporation pressure is 50KPa, so as to obtain trichlorosilane steam.
Thus, through flash evaporation, trichlorosilane and SiO can be prepared2And the trichlorosilane can be returned to the polysilicon production system for recycling, so that the production cost is reduced. And compared with other liquid absorbents such as the adoption of silicon tetrachloride as a drying agent, which is a byproduct in a polysilicon production system (the silicon tetrachloride reacts with water to generate H)4SiO4Gelling, which causes difficulty in recovering silicon tetrachloride), trichlorosilane is conveniently recovered as a drying agent, the recovery efficiency is greatly improved, and the recovery cost is reduced.
In this embodiment, the system further comprises a pressurizer 11, and the pressurizer 11 is connected to an outlet of the flash tank and an inlet of the elution tower, and is configured to receive trichlorosilane vapor sent from the flash tank 10, pressurize and liquefy the trichlorosilane vapor, and send the trichlorosilane vapor back to the elution tower 2.
And the trichlorosilane steam obtained by flash evaporation is pressurized and liquefied and then returned to the leaching tower 2 to be used as a drying agent, so that on one hand, the cyclic utilization of trichlorosilane is realized, and on the other hand, the introduction of external impurities is further reduced.
In this embodiment, a second discharging pipe 12 is disposed at the bottom of the flash tank 10, and a second on-off valve is disposed on the second discharging pipe. When the solid phase SiO2 is observed to remain in the flash tank 10, the second on-off valve is opened to discharge the solid phase through the second discharge pipe 12.
In this embodiment, a reboiler 3 is disposed at the lower portion of the elution tower 2, and the reboiler 3 is completely immersed in the trichlorosilane liquid, and is used to heat the trichlorosilane at the lower portion of the elution tower 2 to a temperature above the boiling point (31.8 ℃).
The process flow of the hydrogen impurity removal system for polycrystalline silicon production in the embodiment is as follows:
crude hydrogen enters a catalytic reactor 9, oxygen in the hydrogen and the hydrogen are subjected to oxidation reaction under the action of a catalyst to generate water, the reacted gas enters an elution tower 2 through an air inlet pipe 1 and contacts trichlorosilane boiling at the tower bottom of the elution tower 2 in a bubbling mode to remove part of moisture in the hydrogen, and the unremoved moisture and the hydrogen flow from the tower bottom to the top togetherRepeatedly contacts with trichlorosilane steam in the leaching tower 2 and atomized silicon tetrachloride sprayed from the top of the tower in the moving process, and the water in the hydrogen reacts with the trichlorosilane to generate SiO2Hydrogen chloride and hydrogen, SiO produced by the reaction2And (3) enriching in the tower kettle, wherein the hydrogen with the moisture removed and part of trichlorosilane steam are ejected from the elution tower and enter a condenser 6 through a first gas guide pipe 4, the trichlorosilane is condensed into liquid and returns to the elution tower 2 through a return pipe 7, and the hydrogen with the impurities removed passes through a second gas guide pipe 8 to reach a hydrogen chloride synthesis process. The tower kettle of the leaching tower 2 is provided with a reboiler 3, and part of trichlorosilane is gasified through steam heating.
When suspended substance SiO in trichlorosilane in tower kettle2When the mass ratio of the SiO-containing solid phase to the trichlorosilane liquid reaches 30 percent, a first opening and closing valve is opened to enable the SiO-containing solid phase to be SiO2The trichlorosilane liquid is discharged to a flash tank 10 through a first discharge pipe 5, the flash tank 10 carries out flash evaporation on the liquid-solid mixture fed into the flash tank, and the obtained trichlorosilane vapor is pressurized and liquefied through a pressurizer 11 and then returns to the leaching tower 2 for recycling. When only solid phase remains in the flash tank 10, a second on-off valve is opened to enable SiO to be discharged2The powder is discharged through a second discharge conduit 12.
Example 2
The embodiment provides a polycrystalline silicon production system, which comprises a reduction furnace and a material providing unit, wherein the material providing unit comprises the hydrogen impurity removal system for polycrystalline silicon production in embodiment 1.
It will be understood that the above embodiments are merely exemplary embodiments taken to illustrate the principles of the present invention, which is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the utility model, and these modifications and improvements are also considered to be within the scope of the utility model.
Claims (9)
1. A hydrogen impurity removal system for polysilicon production is characterized by comprising a leaching tower (2) and a condenser (6),
the lower part of the leaching tower (2) is used for storing the boiled trichlorosilane, and is provided with an air inlet pipe;
a spray structure (21) is arranged at the upper part of the leaching tower (2), and a return pipe (7) is arranged between the condenser (6) and the spray structure (21) and is used for guiding liquefied trichlorosilane into the spray structure (21);
the condenser (6) is connected with the first gas-guide tube (4) at the top of the leaching tower (2).
2. The hydrogen impurity removal system for polysilicon production according to claim 1, further comprising a catalytic reactor (9),
the outlet of the catalytic reactor (9) is connected with the air inlet pipe of the leaching tower (2).
3. The hydrogen impurity removal system for polycrystalline silicon production according to claim 1, wherein a first discharge pipe (5) is arranged at the bottom of the leaching tower (2), and a first opening and closing valve is arranged on the first discharge pipe (5).
4. The hydrogen impurity removal system for polysilicon production according to claim 3, further comprising a flash tank (10), wherein the flash tank (10) is connected to the first discharge pipe (5).
5. The hydrogen impurity removal system for polycrystalline silicon production according to claim 4, further comprising a pressurizer (11), wherein the pressurizer (11) is respectively connected with the outlet of the flash tank (10) and the inlet of the leaching tower (2), and is used for receiving trichlorosilane vapor fed from the flash tank (10), pressurizing and liquefying the trichlorosilane vapor and feeding the trichlorosilane vapor back to the leaching tower (2).
6. The hydrogen impurity removal system for polysilicon production as recited in claim 4, wherein a second discharge pipe (12) is disposed at the bottom of the flash tank (10), and a second on-off valve is disposed on the second discharge pipe.
7. The hydrogen impurity removal system for polycrystalline silicon production according to any one of claims 1 to 6, further comprising a reflux pump (13), wherein the reflux pump (13) is arranged between the spraying structure (21) and the condenser (6) and is used for pressing trichlorosilane liquefied by the condenser (6) into the spraying structure (21).
8. The hydrogen impurity removal system for polycrystalline silicon production according to any one of claims 1 to 6, wherein a reboiler (3) is arranged at the lower part of the elution tower (2) and is used for heating trichlorosilane at the lower part of the elution tower (2) to a temperature above the boiling point of trichlorosilane.
9. A polycrystalline silicon production system comprises a reduction furnace and a material providing unit, and is characterized in that the material providing unit comprises the hydrogen impurity removal system for polycrystalline silicon production according to any one of claims 1 to 8.
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| CN202120971611.6U CN216155481U (en) | 2021-05-08 | 2021-05-08 | Hydrogen impurity removal system for polycrystalline silicon production and polycrystalline silicon production system |
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| CN202120971611.6U CN216155481U (en) | 2021-05-08 | 2021-05-08 | Hydrogen impurity removal system for polycrystalline silicon production and polycrystalline silicon production system |
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