CN113244766A - Single crystal furnace tail gas purification and recovery system and method - Google Patents
Single crystal furnace tail gas purification and recovery system and method Download PDFInfo
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- 238000011084 recovery Methods 0.000 title claims description 25
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/18—Noble gases
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/10—Single element gases other than halogens
- B01D2257/104—Oxygen
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
- Y02A50/2351—Atmospheric particulate matter [PM], e.g. carbon smoke microparticles, smog, aerosol particles, dust
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- Biomedical Technology (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The invention discloses a method for purifying and recovering tail gas of a single crystal furnace, which comprises the following steps: s1, removing dust, namely filtering and removing dust from the tail gas of the monocrystalline silicon furnace to remove solid impurities; s2, cooling and separating, namely cooling the tail gas subjected to dust removal to separate out non-condensable gas and condensate; and S3, recovering argon, and performing decarbonization, deoxidation and purification treatment on the non-condensable gas to obtain high-purity argon. The invention also discloses a system for purifying and recovering the tail gas of the single crystal furnace. The invention can recover the argon in the tail gas of the monocrystalline silicon furnace, and the recovered high-purity argon can be introduced into the monocrystalline silicon furnace for recycling, thereby reducing the production cost of monocrystalline silicon, reducing hydrocarbon substances in the tail gas and reducing environmental pollution.
Description
Technical Field
The invention belongs to the technical field of monocrystalline silicon production, and particularly relates to a system and a method for purifying and recovering tail gas of a monocrystalline furnace.
Background
In the process of preparing the monocrystalline silicon by the czochralski method, in order to reduce the influence of impurities such as SiO, graphite heating rods and the like in silicon raw materials on the production process of the monocrystalline silicon and obtain perfect monocrystalline silicon, the impurities gasified due to high temperature are generally required to be carried out by the flowing of inert gas, and the specific process is as follows: argon is introduced from the top of the single crystal furnace and is pumped out by a vacuum pump, so that dynamic balance is achieved, and the inside of the single crystal furnace is kept in a sub-vacuum state. Therefore, in the production process of single crystal silicon, the off-gas discharged from the single crystal silicon furnace usually contains a large amount of argon gas.
In the existing monocrystalline silicon production process, most of the treatment of the tail gas of the monocrystalline silicon furnace is only to carry out simple dust removal treatment and then directly discharge the tail gas, and the direct discharge of methane and high hydrocarbon substances in the tail gas not only causes resource waste such as a large amount of argon and the like, but also can cause environmental pollution.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art, and provides a system and a method for purifying and recovering the tail gas of a single crystal furnace, which can recycle argon and hydrocarbon substances in the tail gas and are beneficial to reducing the production cost of single crystal silicon.
According to one aspect of the invention, the invention discloses a method for purifying and recovering tail gas of a single crystal furnace, which adopts the following technical scheme:
a method for purifying and recovering tail gas of a single crystal furnace comprises the following steps:
s1 dust removal: filtering and dedusting the tail gas of the monocrystalline silicon furnace to remove solid impurities;
s2 cooling and separating: cooling the tail gas after dust removal, and separating out non-condensable gas and condensate;
s3 argon recovery: and (4) decarbonizing, deoxidizing and purifying the non-condensable gas to obtain high-purity argon.
Preferably, the obtained high-purity argon is introduced into the single crystal furnace after the step S3, so that the argon is recycled.
Preferably, the step S2 further comprises subjecting the non-condensable gas to an adsorption treatment to obtain an adsorbate, and the subsequent treatment of the adsorbate comprises S4 oil gas recovery: and resolving the adsorbate, and then compressing and cooling to recover the oily waste liquid.
Preferably, in step S1, the dust content in the filtered and dedusted tail gas has an accuracy of < 0.3 ppm.
Preferably, in step S2, the cooling step uses water at 7 ℃ as a cooling medium, and further includes compressing the tail gas after dust removal to 0.5-1MPa before the cooling step.
Preferably, in step S3,
the carbon removal refers to the catalytic oxidation of a carbon source in the non-condensable gas by adopting a palladium metal catalyst, wherein the reaction temperature is 350-500 ℃;
the deoxidation is to use a carbon-supported carbon deoxidizer to consume oxygen in the non-condensable gas at the temperature of 280-350 ℃.
Compared with the traditional process, the method for purifying and recovering the tail gas of the monocrystalline silicon furnace disclosed by the invention not only can recover and recycle the argon in the tail gas and reduce the production cost of monocrystalline silicon, but also can recover hydrocarbon substances in the tail gas and reduce the pollution of the tail gas emission to the environment.
According to another aspect of the invention, a system for purifying and recovering tail gas of a single crystal furnace is disclosed, which adopts the following technical scheme:
an exhaust gas purification and recovery system comprising:
the dust removal device is used for receiving the tail gas of the monocrystalline silicon furnace and removing solid impurities in the tail gas;
the cooling separation device is connected with a tail gas output port of the dust removal device and is used for cooling the tail gas after dust removal to obtain non-condensable gas and condensate;
the adsorption device is connected with a non-condensable gas output port of the cooling and separating device and is used for carrying out adsorption treatment on the non-condensable gas obtained by condensation;
the carbon removal device is connected with the adsorption device and is used for oxidizing the carbon source in the tail gas after adsorption treatment;
the oxygen removal tower is connected with the carbon removal device and is used for consuming oxygen in the carbon-removed gas;
and the purification tower is connected with the deoxygenation tower and is used for removing carbon dioxide in the deoxygenated gas to obtain high-purity argon.
Preferably, the dust removing device adopts a filter with an M-shaped 14-core pulse filter core.
Preferably, the adsorption device comprises an adsorber and a control valve, the control assembly comprises a first control valve and a second control valve,
the inlet of the adsorber is connected with the non-condensable gas outlet of the cooling and separating device, and the first control valve is arranged between the inlet of the adsorber and the non-condensable gas outlet of the cooling and separating device;
the second control valve is arranged at the outlet of the adsorber and used for controlling the gas after adsorption treatment to be discharged;
and a desorption pipeline is arranged at the inlet of the adsorber to discharge desorption products of the adsorber.
Preferably, the adsorbers are in a plurality of groups, the plurality of groups of adsorbers are arranged in parallel, each group of adsorbers is provided with a control component corresponding to the adsorber,
the control assembly further comprises a fourth control valve and a fifth control valve, and the fourth control valve and the fifth control valve are respectively arranged between each absorber and the first pressure equalizing pipeline and between each absorber and the second pressure equalizing pipeline so as to control the communication between the absorbers in each group.
Preferably, the carbon removing apparatus includes:
the reactor is connected with the outlet of the absorber, and a palladium metal catalyst is arranged in the reactor and used for catalytic oxidation of a carbon source in the gas after adsorption treatment;
preferably, the carbon removing apparatus further comprises:
the preheater is arranged between the adsorber and the reactor and is used for primarily heating the gas treated by the adsorber.
Preferably, the system further comprises:
and the second cooler is arranged between the deoxygenation tower and the purification tower and is used for cooling the gas after the deoxygenation treatment.
Preferably, the system further comprises:
the refrigerator is connected with the desorption pipeline of the adsorber and is used for compressing and condensing desorption products;
and the oil collecting tank is connected with the refrigerating machine and is used for storing the oily waste liquid generated by compression and condensation of the refrigerating machine.
The tail gas purification and recovery system disclosed by the invention can be used for purification and recovery treatment of the tail gas of the single crystal furnace, and can be used for respectively recycling argon and oil in the tail gas. The purity of the recovered argon can reach more than 99.999 percent, the argon can be recycled, and the tail gas treatment cost is reduced. Through oil gas recovery, the discharged tail gas can meet the national environmental protection standard, and the pollution is reduced.
Drawings
FIG. 1 is a process flow diagram of a method for purifying and recovering tail gas of a single crystal furnace in an embodiment of the invention;
FIG. 2 is a schematic structural diagram of a system for purifying and recovering tail gas of a single crystal furnace in an embodiment of the invention;
fig. 3 is a schematic structural diagram of an adsorption apparatus according to an embodiment of the present invention.
In the figure: 1-furnace tail gas pipeline; 2-overpressure release valve; 3-a filter; 4-a first cooler; 5-oil removal tank; 6-reciprocating compressor; 7-a compression return line; 8-an adsorber; 9-a first control valve; 10-a second control valve; 11-a resolving line; 12-a third control valve; 13-a first pressure equalization line; 14-a second pressure equalization line; 15-a fourth control valve; 16-a fifth control valve; 17-a pressure regulating mechanism; 18-a reactor; 19-a preheater; 20-a heater; 21-on-line oxygen analyzer; 22-a deoxygenation tower; 23-a purification column; 24-a second cooler; 25-a monocrystalline silicon furnace; 26-a freezer; 27-a vacuum pump; 28-oil collecting tank; 29-evacuation line; 30-fire-resistant cap.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention will be further clearly and completely described below with reference to the accompanying drawings and specific examples of the present invention.
In the prior art, the consumption of argon is high in the treatment process of the tail gas of the monocrystalline silicon furnace, and the tail gas contains methane and hydrocarbon substances, so that the problems of resource waste and the like are caused. Therefore, the invention provides a method for purifying and recovering tail gas of a single crystal furnace, which comprises the following steps:
s1 dust removal: filtering and dedusting the tail gas of the monocrystalline silicon furnace to remove solid impurities;
s2 cooling and separating: cooling the tail gas after dust removal, and separating out non-condensable gas and condensate;
s3 argon recovery: and (4) decarbonizing, deoxidizing and purifying the non-condensable gas to obtain high-purity argon.
Correspondingly, the invention also provides a system for purifying and recovering the tail gas of the single crystal furnace, which comprises:
the dust removal device is used for receiving the tail gas of the monocrystalline silicon furnace and removing solid impurities in the tail gas;
the cooling separation device is connected with a tail gas output port of the dust removal device and is used for cooling the tail gas after dust removal to obtain non-condensable gas and condensate;
the adsorption device is connected with a non-condensable gas output port of the cooling and separating device and is used for carrying out adsorption treatment on the non-condensable gas obtained by condensation;
the carbon removal device is connected with the adsorption device and is used for oxidizing the carbon source in the tail gas after adsorption treatment;
the oxygen removal tower is connected with the carbon removal device and is used for consuming oxygen in the carbon-removed gas;
and the purification tower is connected with the deoxygenation tower and is used for removing carbon dioxide in the deoxygenated gas to obtain high-purity argon.
Example 1
As shown in fig. 1, the embodiment discloses a method for purifying and recovering tail gas of a single crystal furnace, which comprises the following steps:
s1 dust removal: and filtering and dedusting the tail gas of the monocrystalline silicon furnace to remove solid impurities.
Specifically, the tail gas of the monocrystalline silicon furnace is introduced into a precision dust removal filter with the dust removal precision of less than 0.3ppm for filtering and dust removal so as to remove solid impurities such as dust particles in the tail gas.
S2 cooling and separating: and cooling the tail gas after dust removal, and separating out non-condensable gas and condensate.
Specifically, the cooling separation is to use water at 7 ℃ as a cooling medium, condense hydrocarbon substances in the dedusted tail gas into liquid (namely, oil-containing waste liquid), and obtain non-condensable gas, wherein the non-condensable gas mainly contains argon, methane, oxygen and the like.
It should be noted that before the cooling in step S2, the method further includes compressing and pressurizing the dedusted tail gas to 0.5-1.0MPa, preferably 0.5MPa, where the pressurization can improve the subsequent tail gas recovery and treatment efficiency.
S3 argon recovery: and (3) performing decarbonization, deoxidation and purification treatment on the non-condensable gas to obtain the high-purity argon gas.
In the step S3, the obtained high-purity argon gas can be fed into a single crystal furnace, so that the argon gas can be recycled.
Specifically, at the temperature of 350-; then, under the condition of 280-350 ℃, the carbon-containing substance in the carbon-supported deoxidizer and the oxygen in the gas after carbon removal treatment are used for oxidation reaction to consume the oxygen therein, and the obtained gas mainly comprises argon and carbon dioxide; then, carbon dioxide in the deoxidized gas is removed by using a carbon dioxide adsorbent (such as calcium hydroxide) to obtain high-purity argon. High-purity argon can be introduced into the monocrystalline silicon furnace again to realize cyclic utilization.
It should be noted that the method of this embodiment further includes:
the step S2 further comprises the step of subjecting the non-condensable gas to adsorption treatment to obtain adsorbate, and the subsequent treatment of the adsorbate comprises S4 oil gas recovery: the adsorbate is resolved, and the resolved gaseous stance is compressed and cooled to recover the oily waste liquid.
Specifically, the non-condensable gas obtained by condensation separation is introduced into an adsorber containing activated carbon to adsorb impurities (mainly hydrocarbon substances which are not fully condensed) in the non-condensable gas; the adsorption saturated adsorber is vacuumized to separate out the adsorbed substances such as hydrocarbons on the activated carbon to obtain the desorption gas, the desorption gas is condensed to condense the hydrocarbon substances in the desorption gas into liquid (namely oil-containing waste liquid), and the condensed gas is directly discharged, or a fire-resisting cap is passed before discharging to further ensure to remove the substances such as hydrocarbons in the discharged gas, so as to avoid environmental pollution.
Compared with the traditional process, the method for purifying and recovering the tail gas of the monocrystalline silicon furnace disclosed by the embodiment can be used for recycling the argon in the tail gas, recovering hydrocarbon substances in the tail gas and reducing the pollution of the tail gas emission to the environment.
Example 2
As shown in fig. 2, this embodiment discloses a system for purifying and recovering tail gas of a single crystal silicon furnace, which can be used in the method described in embodiment 1, and the system includes a dust removing device, a cooling and separating device, an adsorption device, a carbon removing device, a deoxygenating tower 22, and a purification tower 23, and specifically includes the following components:
and the dust removal device is used for receiving the tail gas of the monocrystalline silicon furnace and removing solid impurities in the tail gas.
Specifically, the inlet of the dust removal device is connected with a tail gas pipeline 1 of the monocrystalline silicon furnace. An overpressure vent valve 2 is optionally arranged on the tail gas pipeline to avoid overpressure of the system. The dust removing device includes a filter 3 and a vacuum pump (not shown in the figure), and the filtered gas is pumped out by the vacuum pump. The filter 3 preferably adopts a filter with a filter screen containing a filter element, for example, the filter element adopts an M-shaped 14-core pulse filter element, compared with the traditional filter device (containing a vacuum pump), the filter with the M-shaped 14-core pulse filter element adopted in the embodiment has the dust removal precision of less than 0.3ppm, can prevent extremely small silicon dioxide particles (the particle size is less than or equal to 2 microns) in tail gas from entering the pump cavity of the vacuum pump to be mixed and deposited with pump oil, so that the lubricating effect of the pump oil of the vacuum pump is influenced, the failure rate of the vacuum pump can be reduced, and the operation stability of the vacuum pump and the filter can be improved. It should be noted that the dust removing device of this embodiment further includes a purging tank (not shown), the purging tank is communicated with the filter and is used for performing reverse pulse purging on the filter 3, solid impurities adsorbed on the filter element that is purged are temporarily stored in the bottom space of the filter, and the solid impurities are cleaned when the system is stopped.
And the cooling separation device is connected with a tail gas output port of the dust removal device and used for cooling the tail gas after dust removal to obtain non-condensable gas and condensate.
Specifically, the cooling separation device includes first cooler 4 and deoiling jar 5, the entry of first cooler 4 and the exit linkage of filter 3, first cooler 4 adopts 7 ℃ water as coolant, and the tail gas after the filter 3 is handled is after 7 ℃ water cooling in first cooler 4, and high boiling point material such as high hydrocarbon material wherein condenses into liquid (promptly the oily waste in this embodiment), and noncondensable gases such as argon, methane, oxygen are let in deoiling jar 5 to get rid of the liquid that smugglies in the noncondensable gas, obtain crude argon.
It should be noted that the system of the present embodiment further includes a pressure boosting device:
and the supercharging device is arranged between the filter 3 and the first cooler 4, namely the inlet of the supercharging device is connected with the tail gas output port of the filter, and the outlet of the supercharging device is connected with the inlet of the first cooler 4, and is used for increasing the pressure of the tail gas (the pressure is generally 7-12KPa) after filtering and dedusting to 0.5-1.0 MPa. The supercharging device in this embodiment preferably employs a reciprocating compressor 6, preferably two reciprocating compressors arranged in parallel, one for each.
It should be noted that, in consideration of the throughput of the following devices such as the adsorption device, the compression return line 7 is provided before the reciprocating compressor 6 and after the degreasing tank 5, and a part of the crude argon gas may be returned to the reciprocating compressor 6 for cyclic compression in the case where the crude argon gas discharged from the degreasing tank 5 exceeds the throughput of the following devices such as the adsorption device, so as to improve the stability of the system operation.
And the adsorption device is connected with a non-condensable gas output port of the cooling and separating device and is used for carrying out adsorption treatment on the non-condensable gas obtained by condensation.
In particular, as shown in fig. 3, the adsorption device comprises an adsorber 8 and a control assembly comprising a first control valve 9 and a second control valve 10. The inlet of the adsorber 8 is connected with the non-condensable gas outlet of the cooling and separating device (namely, the gas outlet of the oil removing tank 5), and the first control valve 9 is arranged on a pipeline between the inlet of the adsorber 8 and the non-condensable gas outlet of the cooling and separating device (namely, the gas outlet of the oil removing tank 5). A second control valve 10 is provided at the outlet of the adsorber 8 for controlling the discharge of the gas after the adsorption treatment. The adsorber 8 is filled with an adsorbent, preferably an activated carbon adsorbent. When the adsorption of the adsorbent reaches saturation, the adsorbent can be regenerated through desorption. In this embodiment, it is preferable that the vacuum pump 27 is used to suck the adsorber 8 from the inlet of the adsorber 8 to desorb the adsorbed substances from the adsorbent, and accordingly, a desorption line 11 is further provided at the inlet of the adsorber 8, the vacuum pump is provided on the desorption line 11, the control valve further includes a third control valve 12, and the third control valve 12 is provided on the desorption line 11 to control the desorption line 11 to be closed during the adsorption process of the adsorber 8 and to be opened during the desorption process to discharge the desorbed products of the adsorbent.
Further, as shown in fig. 3, the adsorbers 8 are provided in plural groups, plural groups of adsorbers are arranged in parallel, and each group of adsorbers is provided with a corresponding control unit (that is, each adsorber 8 is provided with a first control valve 9, a second control valve 10, a third control valve 12, an analysis line 11, and the like). A first pressure equalizing pipeline 13 and a second pressure equalizing pipeline 14 are arranged between the outlets of the adsorbers of each group to communicate the adsorbers 8 of each group, the control assembly further comprises a fourth control valve 15 and a fifth control valve 16, the fourth control valve 15 and the fifth control valve 16 are respectively arranged between the adsorbers 8 of each group and the first pressure equalizing pipeline 13 and the second pressure equalizing pipeline 14, the communication between the adsorbers 8 of each group and the first pressure equalizing pipeline 13 and the second pressure equalizing pipeline 14 is controlled through the fourth control valve 15 and the fifth control valve 16 corresponding to the adsorbers 8 of each group, and the communication relation between the adsorbers 8 of each group is controlled to adjust the adsorbers of each group to reach the required pressure. It should be noted that each of the above-mentioned groups of adsorbers 8 may be provided with only one adsorber, or may be provided with a plurality of adsorbers connected in series to form one group, in this embodiment, each group is preferably provided with one adsorber, and the adsorbers 8 are preferably provided in a tower shape, that is, an adsorption tower.
In some alternative embodiments, the adsorption process preferably employs a VPSA (i.e., pressure swing adsorption vacuum desorption) process, i.e., six groups of adsorbers are arranged in parallel, each group includes an adsorption column, each adsorption column is designated as A, B, C, D, E, F, and each adsorption column always sequentially comprises during operation: adsorption, primary pressure equalizing and reducing, secondary pressure equalizing and reducing, analysis, primary pressure equalizing and increasing, secondary pressure equalizing and increasing and the like. When the adsorption device is used, the A-F towers can be used for adsorption one by one, and the adsorption tower saturated in adsorption is regenerated, so that the adsorption device keeps the adsorption treatment effect. After a period of normal operation, the towers A-F are respectively in the processes shown in figure 3 (at this time, A is in the adsorption process, B is in the secondary pressure equalizing and boosting process, C is the primary pressure equalizing and boosting process, D is in the analysis process, E is in the secondary pressure equalizing and reducing process, and F is in the primary pressure equalizing and reducing process), namely, the six adsorption towers are staggered with each other in the arrangement of the execution program to form a closed cycle so as to ensure the stable operation of the adsorption device, and the six adsorption towers are staggered with each other in different working states in the arrangement of the execution program through different combination states of closing or closing of control valves in a control assembly. The following describes the "adsorption-regeneration" cycle of the adsorption column a in detail, taking the adsorption column a as an example:
adsorption: namely an adsorption tower A, introducing crude argon (with the pressure of 0.5-1.0MPa) output by a cooling separation device into the adsorption tower A, after adsorption treatment by activated carbon adsorbent, the impurities (including uncondensed high hydrocarbon substances) in the crude argon are adsorbed, the gas after adsorption treatment mainly comprises argon, methane, oxygen and the like, most of the gas is discharged through the second control valve 10 corresponding to the adsorption tower a, and is introduced into the next process (i.e., the carbon removal process) after being regulated at a stable pressure, and a small part of the gas is cooperatively matched with the fourth control valve 15 corresponding to the adsorption tower a and other control valves (for example, the fourth control valve 15 corresponding to the adsorption tower B is in different closed or closed states), so that the small part of the gas in the adsorption tower a enters the adsorption tower B in the secondary pressure equalizing and boosting process through the first pressure equalizing pipeline 13, and is used for boosting the pressure of the adsorption tower B.
Primary pressure equalizing and reducing: after the adsorption tower runs for a period of time in the adsorption process, the adsorbent tends to be saturated and needs to be regenerated, and the commonly used adsorbent regeneration method is to perform back purging on the adsorbent to resolve adsorbed impurities. In this embodiment, a vacuum suction method is used for desorption, but the pressure in the adsorption tower during the adsorption process is relatively high, which is not beneficial to direct suction desorption, so that depressurization and then vacuum suction are required, and in this embodiment, the system is to introduce the gas in the adsorption tower a that has completed the adsorption process into other adsorption towers that have completed the desorption process, and preferably into the adsorption tower B that has completed the secondary pressure rise process (i.e., the adsorption tower B shown in fig. 3). The process not only can lower the pressure of the adsorption tower A, but also can raise the pressure of the adsorption tower B, and simultaneously recovers the argon in the dead space of the bed layer in the adsorption tower B, so that the argon is fully recycled. The adsorption tower A after the primary pressure equalizing and reducing enters a secondary pressure equalizing and reducing process from the adsorption process, namely, the adsorption tower A is in a state of an adsorption tower F shown in figure 3.
Secondary pressure equalizing and reducing: the gas of adsorption tower A after will having accomplished once decompression communicates with the adsorption tower of accomplishing analytic process, and analytic process is vacuum suction, and the pressure of this adsorption tower is less than adsorption tower A this moment, and adsorption tower A's gas flow direction is to this absorption tower after the analysis to the realization is to adsorption tower A secondary pressure-equalizing decompression, simultaneously, makes this absorption tower after the analysis carry out a pressure-equalizing pressure-boosting process. In this embodiment, the second pressure equalization and depressurization preferably means that the pressure is reduced to a normal pressure state, and the adsorbed impurities begin to be desorbed from the adsorbent.
And (3) analysis: the adsorption tower a is communicated with the desorption pipeline 11, and the vacuum pump 27 on the desorption pipeline 11 is started to carry out vacuum suction on the adsorption tower a, so that impurities adsorbed by the adsorbent in the adsorption tower a are quickly desorbed and discharged to the next process (oil gas recovery process) through the desorption pipeline 11.
Primary voltage equalizing and boosting: and (3) introducing the gas in the adsorption tower which finishes the primary pressure equalizing and reducing process into the adsorption tower A which finishes the analysis process, so that the adsorption tower which finishes the primary pressure equalizing and reducing process carries out the secondary pressure equalizing and reducing process, and the adsorption tower A is boosted (namely the adsorption tower A carries out the primary pressure equalizing and boosting process).
Secondary voltage equalizing and boosting: and (3) introducing the gas in the adsorption tower completing the adsorption process into the adsorption tower A which is subjected to primary pressure equalizing and boosting, so that the adsorption tower completing the adsorption process is subjected to primary pressure equalizing and depressurizing process, the adsorption tower A is subjected to secondary pressure equalizing and boosting process, and the adsorption tower A subjected to secondary pressure boosting is used for the next adsorption-regeneration cycle. This embodiment system, in the actual operation in-process, the connecting line and the first pipeline 13 intercommunication of equalizing pressure with each adsorption tower and next process to set up pressure adjustment mechanism 17, treat the adsorption tower that carries out the adsorption process through the gas after handling with the absorption earlier and carry out steady voltage regulation, adjust the pressure in this adsorption tower to adsorption pressure earlier before getting into the adsorption process promptly, in order to avoid switching the fluctuation that causes when different adsorption towers carry out the adsorption treatment and influence the adsorption treatment effect.
In this embodiment, the adsorption tower after adsorption is depressurized twice, the adsorption tower after desorption is pressurized twice, and the process of depressurizing twice and pressurizing twice is to utilize the gas in the adsorption tower with higher pressure to enter the adsorption tower with lower pressure, and the process is a pressure equalizing process, so that the purpose of depressurizing and pressurizing can be achieved, and the dead space gas (mainly argon gas recovery) in the beds in the adsorption towers can be fully recovered through the process.
And the carbon removal device is connected with the adsorption device and is used for oxidizing the carbon source in the tail gas after adsorption treatment.
Specifically, the carbon removal device comprises a reactor 18, an inlet of the reactor 18 is connected with an outlet of the adsorber 8, and a palladium metal catalyst is arranged in the reactor 18 and used for catalytically oxidizing carbon sources (mainly methane and carbon monoxide) in the gas subjected to adsorption treatment into carbon dioxide, so that the purpose of carbon removal is achieved. The reaction temperature in the reactor 8 of this example was 350-500 ℃.
It should be noted that the decarbonizing device of the present embodiment further includes:
and a preheater 19 provided between the adsorber 8 and the reactor 18 for preliminarily preheating the gas after the adsorption treatment. The preheater 19 may employ a heat exchanger, and uses high-temperature gas (mainly containing argon, oxygen, carbon dioxide, etc.) discharged after the reaction in the reactor as a heat source. The preheater 19 of the embodiment can preheat the gas at about 120 ℃, which is effective for the heat of the reacted gas and reduces the energy consumption.
It should be noted that the carbon removing apparatus of the present embodiment may further include:
and a heater 20 provided between the preheater 19 and the reactor 18 for heating the gas after the adsorption treatment. In view of the heat loss during the gas transportation in the pipeline in the actual operation, the heating temperature of the heater 20 should be slightly higher than the reaction temperature in the reactor 18, therefore, the heating temperature of the heater 20 is preferably set to 600 ℃ to 700 ℃, and the heater 20 can be an electric heater.
And an on-line oxygen analyzer 21 disposed on a connection line between the adsorption tower 8 and the preheater 19 to detect the oxygen content in the adsorbed gas. Optionally, in order to ensure that the oxygen content is sufficient to sufficiently oxidize the carbon source, an oxygen supply line (not shown) may be provided to determine whether oxygen needs to be supplied to ensure sufficient oxidation of methane, carbon monoxide, etc. to carbon dioxide based on the oxygen content of the gas (i.e., crude argon) after the adsorption treatment detected by the on-line oxygen analyzer 21. The oxygen supply line may be disposed at the front end of the on-line oxygen analyzer 21, or may be at another position, and this embodiment is not further limited. In the present embodiment, since the amount of oxygen in the off-gas of the silicon single crystal furnace is sufficient to oxidize carbon sources such as methane and carbon monoxide therein, an oxygen supply line may not be provided.
And the deoxygenation tower 22 is connected with the decarbonization device and is used for consuming oxygen in the decarbonized gas.
Specifically, a sufficient amount of a carbon-supported deoxidizing agent (mainly containing C, Ba, Cu, Fe, Ni, Ca, Mg, and other trace elements, such as 3093 carbon deoxidizing agent) is provided in the deoxidizing tower 22, and the oxygen contained in the carbon-supported deoxidizing agent is consumed by the combustion reaction of carbon in the carbon-supported deoxidizing agent and oxygen in the gas discharged from the reactor 18, thereby achieving the purpose of deoxidation. Practice proves that the dew point D.P of the gas after the deoxidation treatment is-70 ℃, and the oxygen content is less than or equal to 1 ppm. The reaction temperature in the deoxygenator column 22 is preferably 280-350 ℃. In order to ensure the deoxidation effect, a plurality of the deoxidation towers 22 may be provided in series, and in the present embodiment, two deoxidation towers are preferably connected in series.
And a purification column 23 connected to the deoxygenation column 22 for removing carbon dioxide from the deoxygenated gas to obtain high-purity argon gas.
Specifically, a second cooler 24 is provided between the purification column 23 and the deoxygenation column 22 to cool the higher temperature (280-. The second cooler 24 can adopt circulating water as a cooling medium, and the gas temperature can be reduced to 70-80 ℃ after the cooling treatment of the second cooler 24. A carbon dioxide adsorbent, such as calcium hydroxide, is arranged in the purification tower 23, and the carbon dioxide adsorbent is used for adsorbing and removing carbon dioxide in the deoxidized gas to obtain high-purity argon, and the high-purity argon can reach more than 99.999% through detection. High-purity argon can be introduced into the monocrystalline silicon furnace 25 to realize recycling.
Further, in order to avoid the pollution of the desorption product of the adsorber to the environment, the system further comprises:
the refrigerator 26 is connected to the desorption line 11 of the adsorber 8 and removes hydrocarbon substances (i.e., oil) from the desorption product. Specifically, the desorbed product generated in the desorption process of the adsorber 8 is pumped by the vacuum pump 27, enters the refrigerator 26 through the desorption pipeline 11, is compressed and frozen by the refrigerator 26, and condenses the hydrocarbon substances in the desorbed product into liquid, namely oil-containing waste liquid, so as to ensure that the uncondensed gas reaches the emission standard (the total hydrocarbon content of non-methane is less than or equal to 120 mg/m)3). The freezer 26 may employ a mechanism known in the art for achieving cryogenic refrigeration by changing the pressure change of the refrigerant gas using a compressor.
And an oil collecting tank 28 connected to the refrigerator 26 for storing the oil-containing waste liquid generated by compression and condensation of the refrigerator 26. The uncondensed gas (i.e. the tail gas reaching the standard) is discharged through an evacuation line 29 provided on the oil collecting tank 28, and a fire-proof cap 30 is provided on the evacuation line to ensure the safety of the discharge.
The system for purifying and recovering the tail gas of the monocrystalline silicon furnace disclosed by the embodiment can be used for purifying and recovering the tail gas of the monocrystalline silicon furnace, and respectively recycling argon and oil in the tail gas. The purity of the recovered argon can reach more than 99.999 percent, the argon can be recycled, and the tail gas treatment cost is reduced. Through oil gas recovery, the discharged tail gas can meet the national environmental protection standard, and the pollution is reduced.
It will be understood that the foregoing is only a preferred embodiment of the invention, and that the invention is not limited thereto. It will be apparent to those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention, and these changes and modifications are to be considered as within the scope of the invention.
Claims (14)
1. A method for purifying and recovering tail gas of a single crystal furnace comprises the following steps,
s1 dust removal: filtering and dedusting the tail gas of the monocrystalline silicon furnace to remove solid impurities;
s2 cooling and separating: cooling the tail gas after dust removal, and separating out non-condensable gas and condensate;
s3 argon recovery: and (4) decarbonizing, deoxidizing and purifying the non-condensable gas to obtain high-purity argon.
2. The method for purifying and recycling the tail gas of the single crystal furnace according to claim 1, wherein the step S3 further comprises the step of introducing the obtained high-purity argon gas into the single crystal furnace to recycle the argon gas.
3. The method for purifying and recovering the tail gas of the single crystal furnace according to claim 1, further comprising the step of adsorbing the non-condensable gas to obtain an adsorbate in the step S2, and then the treatment of the adsorbate comprises S4 oil gas recovery: and resolving the adsorbate, and then compressing and cooling to recover the oily waste liquid.
4. The method for purifying and recovering the tail gas of the single crystal furnace according to any one of claim 3, wherein in step S2, water with the temperature of 7 ℃ is used as a cooling medium for the cooling, and the method further comprises compressing the tail gas after dust removal to 0.5-1.0MPa before the cooling.
5. The method for purifying and recovering the tail gas of the single crystal furnace according to any one of claims 1 to 4, wherein in the step S1, the precision of the filtering and dust removal is less than 0.3 ppm.
6. The method for purifying and recovering the off-gas of the single crystal furnace according to any one of claims 1 to 4, wherein in step S3,
the carbon removal refers to the catalytic oxidation of a carbon source in the non-condensable gas by adopting a palladium metal catalyst, wherein the reaction temperature is 350-500 ℃;
the deoxidation is to use a carbon-supported carbon deoxidizer to consume oxygen in the non-condensable gas at the temperature of 280-350 ℃.
7. A tail gas purification and recovery system is characterized by comprising:
the dust removal device is used for receiving the tail gas of the monocrystalline silicon furnace and removing solid impurities in the tail gas;
the cooling separation device is connected with a tail gas output port of the dust removal device and is used for cooling the tail gas after dust removal to obtain non-condensable gas and condensate;
the adsorption device is connected with a non-condensable gas output port of the cooling and separating device and is used for carrying out adsorption treatment on the non-condensable gas obtained by condensation;
the carbon removal device is connected with the adsorption device and is used for oxidizing the carbon source in the tail gas after adsorption treatment;
the deoxygenation tower (22) is connected with the decarbonization device and is used for consuming oxygen in the decarbonized gas;
and a purification tower (23) connected to the deoxygenation tower (22) for removing carbon dioxide from the deoxygenated gas to obtain high-purity argon gas.
8. The single crystal furnace tail gas purification and recovery system according to claim 7, wherein the dust removal device adopts a filter (3) with an M-shaped 14-core pulse filter core.
9. The single crystal furnace tail gas purification and recovery system according to claim 7, characterized in that the adsorption device comprises an adsorber (8) and a control component, the control component comprises a first control valve (9) and a second control valve (10),
the inlet of the adsorber (8) is connected with the outlet of the cooling separation device, and the first control valve (9) is arranged between the inlet of the adsorber and the outlet of the cooling separation device;
the second control valve (10) is arranged at the outlet of the adsorber (8) and is used for controlling the gas after adsorption treatment to be discharged;
and a desorption pipeline (11) is also arranged at the inlet of the adsorber (8) to discharge the desorption product of the adsorber.
10. The single crystal furnace tail gas purification and recovery system as claimed in claim 9, wherein the adsorbers (8) are in a plurality of groups, the plurality of groups of adsorbers are arranged in parallel, each group of adsorbers is provided with a control component corresponding to the group of adsorbers,
a first pressure-equalizing line (13) and a second pressure-equalizing line (14) are arranged between the outlets of the adsorbers of each group, the control assembly further comprising a fourth control valve (15) and a fifth control valve (16),
the fourth control valve and the fifth control valve are respectively arranged between each adsorber and the first pressure equalizing pipeline and the second pressure equalizing pipeline so as to control the communication between each group of adsorbers.
11. The single crystal furnace tail gas purification and recovery system of claim 9, wherein the decarbonization device comprises:
and the reactor (18) is connected with the outlet of the absorber (8), and a palladium metal catalyst is arranged in the reactor and used for catalytically oxidizing the carbon source in the gas after the absorption treatment.
12. The single crystal furnace tail gas purification and recovery system of claim 11, wherein the decarbonization device further comprises:
the preheater (19) is arranged between the adsorber (8) and the reactor (18) and is used for primarily heating the gas treated by the adsorber.
13. The single crystal furnace tail gas purification and recovery system according to claim 7, further comprising:
and a second cooler (24) provided between the deoxidation tower (22) and the purification tower (23) and used for cooling the gas after the deoxidation treatment.
14. The single crystal furnace tail gas purification and recovery system according to claim 7, further comprising:
a refrigerator (26) connected with the desorption pipeline of the adsorber (8) and used for compressing and condensing the desorption product;
and the oil collecting tank (28) is connected with the refrigerator (26) and is used for storing the oily waste liquid generated by compression and condensation of the refrigerator.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116657239A (en) * | 2023-08-01 | 2023-08-29 | 上海联风气体有限公司 | Argon recovery equipment of single crystal furnace |
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