CN117346476A - Double-tower combined argon recovery and purification system and method - Google Patents
Double-tower combined argon recovery and purification system and method Download PDFInfo
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- CN117346476A CN117346476A CN202311208147.5A CN202311208147A CN117346476A CN 117346476 A CN117346476 A CN 117346476A CN 202311208147 A CN202311208147 A CN 202311208147A CN 117346476 A CN117346476 A CN 117346476A
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 title claims abstract description 752
- 229910052786 argon Inorganic materials 0.000 title claims abstract description 376
- 238000011084 recovery Methods 0.000 title claims abstract description 43
- 238000000746 purification Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 340
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 165
- 239000007788 liquid Substances 0.000 claims abstract description 106
- 239000002699 waste material Substances 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims description 70
- 239000002808 molecular sieve Substances 0.000 claims description 52
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 52
- 238000001914 filtration Methods 0.000 claims description 37
- 239000001257 hydrogen Substances 0.000 claims description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims description 21
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 229910001868 water Inorganic materials 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 13
- 239000000428 dust Substances 0.000 claims description 13
- 239000002912 waste gas Substances 0.000 claims description 13
- 239000001569 carbon dioxide Substances 0.000 claims description 10
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 10
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 10
- 238000011069 regeneration method Methods 0.000 claims description 10
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 9
- 238000010926 purge Methods 0.000 claims description 9
- 230000008929 regeneration Effects 0.000 claims description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 8
- 150000002431 hydrogen Chemical class 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 230000009977 dual effect Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 238000003303 reheating Methods 0.000 claims description 4
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 238000005496 tempering Methods 0.000 claims description 2
- 238000002309 gasification Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 11
- 239000001301 oxygen Substances 0.000 description 11
- 229910052760 oxygen Inorganic materials 0.000 description 11
- 239000003921 oil Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000002231 Czochralski process Methods 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
- F25J3/028—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases
- F25J3/0285—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases of argon
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
The invention provides a double-tower combined argon recovery and purification system and a double-tower combined argon recovery and purification method, wherein the system comprises a cold box, an argon rectification unit and a nitrogen rectification unit; the argon rectification unit is arranged in the cold box and comprises an argon rectification tower, an argon condenser and a liquid argon inlet, wherein the argon condenser is arranged at the top of the inner cavity of the argon rectification tower, and the liquid argon inlet is arranged at the top of the argon rectification tower and is communicated with the argon condenser; the nitrogen rectification unit is arranged in the cold box and comprises a nitrogen rectification tower, a first conveying pipeline and a second conveying pipeline, wherein the nitrogen rectification tower is communicated with the inlet end of the argon condenser through the first conveying pipeline and the outlet end of the argon condenser through the second conveying pipeline. The nitrogen introduced into the argon condenser can recycle the redundant cold energy of the liquid argon to form liquid nitrogen, and finally the liquid nitrogen is sent back to the nitrogen rectifying tower through the second conveying pipeline, so that the recycled liquid nitrogen can be sold as a byproduct, the economic benefit is increased, and the cold energy waste caused by the normal temperature gasification of the liquid argon is avoided.
Description
Technical Field
The invention relates to the technical field of gas purification and recovery, in particular to a double-tower combined argon recovery and purification system and method.
Background
The Czochralski method (Czochralski method) is the primary method of producing single crystal silicon, with most single crystal silicon worldwide being produced by the Czochralski method. The most common Czochralski process for producing single crystal silicon is a reduced pressure crystal pulling process that is both vacuum-like and flow-like; the decompression process is to continuously and uniformly introduce high-purity argon into the hearth of the single crystal furnace in the silicon single crystal drawing process, and simultaneously vacuum pumpArgon is continuously pumped outwards from the hearth, so that the vacuum degree in the hearth is kept to be about 20 Torr, and the process has the characteristics of a vacuum process and a flowing atmosphere process. The vacuum pump of the vacuum pull process typically employs a slide valve pump, which is a mechanical vacuum pump that maintains a seal with oil. The argon gas carries silicon oxide and impurity volatiles generated due to high temperature during the single crystal pulling process and is discharged to the atmosphere by pumping of a vacuum pump. By analyzing the discharged argon gas, the main impurity components are dust, O 2 、N 2 、CO、CO 2 、CH 4 And (3) waiting for alkane and liquid lubricating oil mist. The recycling of the argon has great practical significance.
In the prior art, the common argon recovery and purification method comprises the following steps: firstly, carrying out crude oil removal on argon recovered from a single crystal furnace, and then carrying out high-precision oil removal and dust removal after compression cooling; then, high-temperature catalysis is carried out to react hydrocarbon such as methane and carbon monoxide with oxygen to produce water and carbon dioxide, and excessive oxygen is ensured in the catalysis reaction (oxygen is added when impurity oxygen is insufficient); after cooling, the excessive oxygen reacts with the added hydrogen to generate water under the action of a catalyst, the excessive hydrogen is ensured to be reacted, and the impurity components in the treated argon are water, carbon dioxide, hydrogen and nitrogen; and then adsorbing water and carbon dioxide by an argon normal-temperature adsorption unit to obtain crude argon containing nitrogen and hydrogen as impurities, and finally introducing an argon rectifying tower to separate hydrogen and nitrogen, thereby obtaining argon. The argon rectifying tower generally needs to add liquid argon to provide cold energy, and because the recovery rate of general argon is 92%, 8% of liquid argon needs to be gasified to compensate for the loss of argon, but generally, the argon rectifying tower generally has 2% of liquid argon to provide cold energy enough, so about 6% of liquid argon can compensate for the loss of argon in a normal temperature gasification mode, and the cold energy waste is caused.
Disclosure of Invention
Based on the above, the invention aims to provide a double-tower combined argon recovery and purification system, which is used for solving the technical problem that in the prior art, when liquid argon is added into an argon rectifying tower to make up for the loss of argon, part of cold energy of the liquid argon is consumed in a normal-temperature gasification mode, so that the cold energy is wasted.
In one aspect, the present invention provides a dual column combined argon recovery purification system comprising:
a cold box;
the argon rectification unit is arranged in the cold box and comprises an argon rectification tower, an argon condenser and a liquid argon adding port, wherein the argon condenser is arranged at the top of an inner cavity of the argon rectification tower, the liquid argon adding port is arranged at the top of the argon rectification tower and is communicated with the argon condenser, and the liquid argon adding port is used for adding liquid argon into the argon condenser;
the nitrogen rectification unit is arranged in the cold box and comprises a nitrogen rectification tower, a first conveying pipeline and a second conveying pipeline, wherein the nitrogen rectification tower is communicated with the inlet end of the argon condenser through the first conveying pipeline, and is communicated with the outlet end of the argon condenser through the second conveying pipeline.
Further, the double-tower combined argon recovery and purification system further comprises an argon rough filtering unit and a nitrogen rough filtering unit which are arranged outside the cold box, and a first main heat exchanger and a second main heat exchanger which are arranged inside the cold box, wherein the argon rough filtering unit is used for recovering waste argon from the single crystal furnace and filtering the waste argon into crude argon only containing nitrogen and hydrogen, and the first main heat exchanger is used for receiving the crude argon from the argon rough filtering unit, cooling the crude argon and sending the cooled crude argon into the argon rectifying tower to prepare pure argon;
the nitrogen rough filtering unit is used for extracting air and removing carbon dioxide and water in the air, and the second main heat exchanger is used for receiving the air from the nitrogen rough filtering unit, cooling the air and sending the cooled air into the nitrogen rectifying tower to prepare nitrogen.
Further, the argon recovery and purification system with double towers is characterized in that the first main heat exchanger and the second main heat exchanger are combined into a whole.
Further, the double-tower combined argon recovery and purification system comprises an argon rough filtering unit, wherein the argon rough filtering unit comprises a first molecular sieve and a first argon conveying pipeline, one end of the first argon conveying pipeline is connected with the outlet end of the first molecular sieve, and the other end of the first argon conveying pipeline is sequentially connected with the first main heat exchanger and the argon rectifying tower;
an expander is arranged in the cold box, a third conveying pipeline is externally connected to the first conveying pipeline, the third conveying pipeline is used for conveying nitrogen produced in the nitrogen rectifying tower into the second main heat exchanger for tempering, then the warmed nitrogen is conveyed into the expander for expanding to produce cold energy, then the expanded nitrogen is returned to the cold end of the second main heat exchanger for recycling cold energy, and finally the nitrogen is conveyed out of the second main heat exchanger as purge gas to enter the first molecular sieve, wherein a first throttle valve for controlling the nitrogen to enter the argon condenser is arranged on the first conveying pipeline, and a molecular sieve regeneration heater is arranged on the third conveying pipeline and is used for heating the purge gas to be introduced into the first molecular sieve.
Further, the argon recovery purification system that two towers are united, wherein, the inner chamber bottom of argon rectification tower is equipped with the reboiler, first argon gas pipeline is kept away from the one end of first molecular sieve is connected the entrance point of reboiler, the exit end of reboiler is equipped with and connects the first back flow at argon rectification tower middle part, the bottom of argon rectification tower is equipped with the intercommunication the second back flow of argon condenser, be equipped with the second choke valve on the first back flow, be equipped with the third choke valve on the second back flow.
Further, the argon recovery purification system that two towers are united, wherein, the top of argon rectification tower is equipped with waste gas discharge pipe and pure argon gas discharge pipe, waste gas discharge pipe passes first main heat exchanger connects first molecular sieve, pure argon gas discharge pipe passes first main heat exchanger stretches out outside the cold box, pure argon gas discharge pipe's end-to-end connection has a pure argon gas compressor.
Further, the argon recovery purification system that the double tower was united, wherein, the argon gas rough filtration unit still includes second argon gas pipeline, second argon gas pipeline's one end be connected in the entrance point of first molecular sieve, the other end are connected with a dust filter, follow on the dust filter second argon gas pipeline is last to be provided with double-film gas holder system, crude argon gas compressor, water-cooler, high accuracy deoiling system, regenerator, crude argon gas heater, carbon monoxide removal reactor, deoxidization reactor and crude argon gas cooler in proper order.
Further, the dual-tower combined argon recovery and purification system further comprises an air conveying pipeline, wherein one end of the air conveying pipeline penetrates through the second main heat exchanger to be connected with the nitrogen rectifying tower, the other end of the air conveying pipeline is connected with an air filter, and an air compressor, an air cooling unit and a second molecular sieve are sequentially arranged on the air conveying pipeline behind the air filter;
the top of nitrogen rectification tower is equipped with nitrogen gas pipeline and liquid nitrogen discharge pipe, nitrogen gas pipeline passes the second main heat exchanger is connected the second molecular sieve, the liquid nitrogen discharge pipe stretches out outside the cold box, be equipped with on the liquid nitrogen discharge pipe and be used for controlling liquid nitrogen exhaust liquid nitrogen valve.
Further, the argon recovery purification system with the combination of the double towers, wherein a third return pipe connected with the top of the nitrogen rectifying tower is arranged at the bottom of the nitrogen rectifying tower, and a fourth throttle valve is arranged on the third return pipe.
The invention also provides a double-tower combined argon recovery and purification method, which is used for the double-tower combined argon recovery and purification system in the technical scheme, and comprises the following steps:
a) Purifying waste argon, filtering the waste argon from the single crystal furnace to obtain crude argon with nitrogen and hydrogen as impurities;
b) Crude argon is rectified, the crude argon is introduced into an argon rectifying tower to be rectified and separated according to the characteristic of different boiling points of argon, nitrogen and hydrogen, so as to obtain liquid argon at the bottom of the argon rectifying tower, and rectifying waste gas is discharged from the top of the argon rectifying tower, wherein the rectifying waste gas comprises hydrogen and nitrogen;
c) Cold energy recovery, namely transferring part of nitrogen in the nitrogen rectifying tower to the argon rectifying tower through a first conveying pipeline to recover redundant cold energy of liquid argon in the argon rectifying tower to form liquid nitrogen, and then conveying the liquid nitrogen back to the nitrogen rectifying tower through a second conveying pipeline;
d) And (3) preparing pure argon, namely extracting liquid argon in the argon rectifying tower and reheating the liquid argon to generate pure argon.
According to the double-tower combined argon recovery and purification system and method, the argon rectification unit and the nitrogen rectification unit are combined, so that the cold energy of liquid argon added into the argon condenser can be fully utilized, and particularly, when a user adds liquid argon into the argon condenser through the liquid argon adding port, the nitrogen rectification tower can send partial nitrogen into the argon condenser through the first conveying pipeline, the nitrogen in the argon condenser can recycle the redundant cold energy of the liquid argon to form liquid nitrogen, and finally, the liquid nitrogen is returned into the nitrogen rectification tower through the second conveying pipeline, so that the recovered liquid nitrogen can be sold as a byproduct, the economic benefit is increased, and the cold energy waste caused by normal-temperature gasification of the liquid argon is avoided.
Drawings
FIG. 1 is a block diagram of an argon recovery purification system in accordance with the present invention;
FIG. 2 is a flow chart of the argon recovery and purification method of the present invention;
description of main reference numerals:
101. a dust filter; 102. a double membrane gas holder system; 103. a crude argon compressor; 104. a water cooler; 105. a high-precision oil removing system; 106. a regenerator; 107. a crude argon heater; 108. a carbon monoxide removal reactor; 109. a deoxygenation reactor; 110. a crude argon cooler; 111. a first molecular sieve; 112. a first primary heat exchanger; 113. an argon rectifying tower; 114. a pure argon compressor; 201. an air filter; 202. an air compressor; 203. an air cooling unit; 204. a second molecular sieve; 205. a second primary heat exchanger; 206. a nitrogen rectifying tower; 300. a cold box; 11. an argon condenser; 12. a liquid argon inlet; 13. a first argon delivery line; 14. an expander; 15. a third delivery conduit; 16. a first throttle valve; 17. a molecular sieve regeneration heater; 18. a reboiler; 19. a first return pipe; 20. a second return pipe; 21. a second throttle valve; 22. a third throttle valve; 23. an exhaust gas discharge pipe; 24. a pure argon gas discharge pipe; 25. a second argon delivery line; 26. a first delivery conduit; 27. a second delivery conduit; 31. an air delivery conduit; 32. a nitrogen gas delivery pipe; 33. a liquid nitrogen discharge pipe; 34. a liquid nitrogen valve; 35. a third return line; 36. a fourth throttle valve; 400. an analyzer.
The invention will be further described in the following detailed description in conjunction with the above-described figures.
Detailed Description
In order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to the appended drawings. Several embodiments of the invention are presented in the figures. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, a dual-tower combined argon recovery and purification system in a first embodiment of the present invention includes a cold box 300, and an argon rectification unit and a nitrogen rectification unit disposed in the cold box 300.
The argon rectification unit comprises an argon rectification tower 113, an argon condenser 11 and a liquid argon adding port 12, wherein the argon condenser 11 is arranged at the top of an inner cavity of the argon rectification tower 113, the liquid argon adding port 12 is arranged at the top of the argon rectification tower 113 and is communicated with the argon condenser 11, and the liquid argon adding port 12 is used for adding liquid argon into the argon condenser 11, so that on one hand, cold energy is provided for the argon condenser 11, and on the other hand, argon loss in the rectification process can be compensated, and the recovery rate of argon is improved;
it should be explained that, the reason why the liquid argon is added into the argon condenser 11 is that the argon has a certain loss in the rectification process, in this embodiment, the recovery rate of the argon is about 92%, 8% of the liquid argon is needed to be added to gasify to compensate the loss of the argon, but usually, the argon rectification column 113 has enough cold energy provided by 2% of the liquid argon, so that about 6% of the liquid argon needs to gasify at normal temperature to compensate the loss of the argon, which results in the waste of cold energy, and in order to reasonably recover the cold energy of the part of the liquid argon, we additionally integrate a nitrogen rectification unit on the basis of the argon rectification unit.
Specifically, the nitrogen rectification unit includes a nitrogen rectification tower 206, a first conveying pipeline 26 and a second conveying pipeline 27, wherein the nitrogen rectification tower 206 is communicated with the inlet end of the argon condenser 11 through the first conveying pipeline 26, and is communicated with the outlet end of the argon condenser 11 through the second conveying pipeline 27. In practical application, a part of nitrogen can be fed into the argon condenser 11 through the first conveying pipeline 26, specifically, the flow of the nitrogen can be controlled through the first throttle valve 16, the nitrogen can recover redundant cold energy of liquid argon to form liquid nitrogen after being fed into the argon condenser 11, then the liquid nitrogen is fed back into the nitrogen rectifying tower 206 through the second conveying pipeline 27, the recovered liquid nitrogen can be sold as a byproduct, the economic benefit is increased, and the cold energy waste caused by normal-temperature gasification of the liquid argon is avoided.
Specifically, in this embodiment, the dual-tower combined argon recovery and purification system further includes an argon rough filtration unit and a nitrogen rough filtration unit that are disposed outside the cold box 300, and a first main heat exchanger 112 and a second main heat exchanger 205 that are disposed inside the cold box 300;
the argon rough filtering unit is used for recovering waste argon from the single crystal furnace and filtering the waste argon into crude argon only containing nitrogen and hydrogen, and the first main heat exchanger 112 is used for receiving the crude argon from the argon rough filtering unit, cooling the crude argon and sending the cooled crude argon into the argon rectifying tower 113 to prepare pure argon;
in another embodiment, the first main heat exchanger 112 and the second main heat exchanger 205 may be combined.
The nitrogen rough filtering unit is used for extracting air and removing carbon dioxide and water from the air, and the second main heat exchanger 205 is used for receiving the air from the nitrogen rough filtering unit and sending the air into the nitrogen rectifying tower 206 after cooling to prepare nitrogen.
Specifically, the argon gas rough filtering unit comprises a first molecular sieve 111 and a first argon gas conveying pipeline 13, one end of the first argon gas conveying pipeline 13 is connected with the outlet end of the first molecular sieve 111, and the other end of the first argon gas conveying pipeline 13 is sequentially connected with the first main heat exchanger 112 and the argon gas rectifying tower 113;
in this embodiment, the first molecular sieve 111 may be composed of two adsorbers, wherein one adsorber regenerates while the other adsorber is performing adsorption, and the regeneration step includes decompression, heating, blowing and replacement, and the two adsorbers are automatically controlled to switch operation by a time program controller.
The purge gas (nitrogen) for regenerating the first molecular sieve 111 is mainly supplied through the nitrogen rectifying tower 206, and it should be noted that by introducing nitrogen, it competes with argon on the adsorbent for adsorption, thereby gradually replacing the argon. The nitrogen is then collected and treated along with the argon therein, and the adsorbent is again ready for the next round of adsorption. The choice of these regeneration methods depends on the design and application scenario of the adsorber. The purpose of the adsorber regeneration is to ensure that the adsorber can continuously and efficiently recover argon, and the adsorbent can be recycled, so that the waste and cost of the argon are reduced.
In practice, since nitrogen leaving the nitrogen rectification column 206 typically has a pressure of 4.0barg or more, but nitrogen in the first molecular sieve 111 typically has a pressure of 0.1 to 0.2barg, a significant portion of the work is wasted if the nitrogen is directly sent to the first molecular sieve 111, and in this embodiment, an expander 14 is provided in the cold box 300 to recover this portion of the cold energy in order to prevent this portion of the work from being wasted.
Specifically, the first conveying pipeline 26 is externally connected with a third conveying pipeline 15, the third conveying pipeline 15 is used for sending the nitrogen gas produced in the nitrogen rectifying tower 206 into the second main heat exchanger 205 to return to the temperature of-150 ℃, then sending the nitrogen gas after the temperature return into the expander 14 to expand to produce cold energy, then sending the expanded nitrogen gas back to the cold end of the second main heat exchanger 205 to recover cold energy for the second main heat exchanger 205, and finally sending the nitrogen gas out of the second main heat exchanger 205 as purge gas to enter the first molecular sieve 111, wherein the first conveying pipeline 26 is provided with a first throttle valve 16 for controlling the nitrogen gas to enter the argon gas condenser 11, and the third conveying pipeline 15 is provided with a molecular sieve regeneration heater 17, and the molecular sieve regeneration heater 17 is used for heating the purge gas to be introduced into the first molecular sieve 111. It can be seen that in this embodiment, the nitrogen in the nitrogen rectification column 206 is transported into the first molecular sieve 111 as purge gas mainly through the third transfer line 15.
Specifically, the bottom of the inner cavity of the argon rectification column 113 is provided with a reboiler 18, one end of the first argon conveying pipeline 13, which is far away from the first molecular sieve 111, is connected with the inlet end of the reboiler 18, the outlet end of the reboiler 18 is provided with a first return pipe 19 connected with the middle part of the argon rectification column 113, the bottom of the argon rectification column 113 is provided with a second return pipe 20 communicated with the argon condenser 11, the first return pipe 19 is provided with a second throttle valve 21, and the second return pipe 20 is provided with a third throttle valve 22. In this embodiment, the heat source of the reboiler 18 is from the crude argon delivered by the first argon delivery pipe 13, and the crude argon is condensed into liquid by liquid argon having a lower pressure than that of the crude argon after entering the reboiler 18; the cold source of the argon condenser 11 is from the cold energy generated by gasifying liquid argon under low pressure, specifically, a part of liquid argon can be added from the liquid argon adding port 12, and the other part of liquid argon can flow back into the argon condenser 11 through the second backflow pipe 20 to provide cold energy for condensation of crude argon rising in the tower, and when the back-flowing liquid argon is gasified by the vapor recovery cold energy, the liquid argon is discharged outwards through the pure argon discharge pipe 24.
In this embodiment, in order to further improve the purity of the liquid argon at the bottom of the argon rectification column 113, the reboiler 18 is used for reheating and boiling the liquid argon at the bottom of the argon rectification column 113, and the liquid argon is partially converted into a gas form and rises to the middle of the argon rectification column 113 through the first return pipe 19 to continue to participate in the rectification process of the argon condenser 11, so as to further improve the separation effect of the liquid argon.
Further, an exhaust gas discharge pipe 23 and a pure argon gas discharge pipe 24 are arranged at the top of the argon gas rectifying tower 113, the exhaust gas discharge pipe 23 penetrates through the first main heat exchanger 112 to be connected with the first molecular sieve 111, the pure argon gas discharge pipe 24 penetrates through the first main heat exchanger 112 to extend out of the cold box 300, and the tail end of the pure argon gas discharge pipe 24 is connected with a pure argon gas compressor 114. It can be understood that in the present embodiment, the non-condensing gas at the top of the argon rectification column 113 is rectification waste gas, which mainly contains nitrogen, hydrogen and a small portion of argon, and can be discharged into the first molecular sieve 111 as a displacement gas through the waste gas discharge pipe 23. Specifically, after the regeneration of the first molecular sieve 111 is completed, the displacement gas (nitrogen, hydrogen and argon) is supplied to the first molecular sieve 111 through the exhaust gas discharge pipe 23 to completely remove the residual argon gas on the adsorber. The returned liquid argon can be sent out of the cold box 300 through the pure argon discharge pipe 24, and can be reheated and gasified when passing through the first main heat exchanger 112, and finally compressed and sent to the single crystal production plant through the pure argon compressor 114.
Specifically, the argon gas rough filtering unit further includes a second argon gas conveying pipeline 25, one end of the second argon gas conveying pipeline 25 is connected to the inlet end of the first molecular sieve 111, the other end of the second argon gas conveying pipeline 25 is connected to a dust filter 101, and a double-film gas holder system 102, a crude argon gas compressor 103, a water cooler 104, a high-precision oil removal system 105, a heat regenerator 106, a crude argon gas heater 107, a carbon monoxide removal reactor 108, a deoxidization reactor 109 and a crude argon gas cooler 110 are sequentially arranged on the second argon gas conveying pipeline 25 behind the dust filter 101. In practical application, the argon rough filtration steps are as follows: firstly, introducing waste argon from a single crystal furnace into a dust filter 101, filtering dust, sending the dust to a double-membrane gas holder system 102, extracting crude argon from the double-membrane gas holder system 102 by a crude argon compressor 103, and removing oil after compression and cooling; after the temperature is raised by the crude argon heater 107, the crude argon is sent to the carbon monoxide removal reactor 108 to remove hydrocarbon such as methane and carbon monoxide, and in the process, excessive oxygen is ensured, if oxygen is lack, air or oxygen-enriched air from the nitrogen rectifying tower 206 can be supplemented, and water and carbon dioxide are generated by reaction; cooling the crude argon gas from which hydrocarbons and carbon monoxide are removed, adding a small excess of hydrogen gas into a deoxidizing reactor 109 to remove oxygen, and reacting to generate water; the crude argon after the two catalytic reactions is sent to the first molecular sieve 111 to remove water and carbon dioxide in the crude argon, and an absorber of the first molecular sieve 111 can be regenerated through nitrogen conveyed by the third conveying pipeline 15 and rectified waste gas conveyed by the waste gas discharge pipe 23; the main impurities in the crude argon leaving the first molecular sieve 111 are hydrogen and nitrogen, then the crude argon is sent into an argon rectifying tower 113 for rectification, the rectified waste gas with high nitrogen and hydrogen content is separated at the top of the argon rectifying tower 113, and pure liquid argon is obtained at the bottom.
In addition, in this embodiment, two analyzers 400 are further disposed on the second argon gas conveying pipe 25 for monitoring the working condition of the argon gas rough filtering unit to prevent the explosion caused by the accumulation of hydrocarbons.
Specifically, the nitrogen rough filtering unit further includes an air conveying pipe 31, one end of the air conveying pipe 31 passes through the second main heat exchanger 205 to be connected with the nitrogen rectifying tower 206, the other end is connected with an air filter 201, and an air compressor 202, an air cooling unit 203 and a second molecular sieve 204 are sequentially arranged on the air conveying pipe 31 behind the air filter 201;
the top of the nitrogen rectifying tower 206 is provided with a nitrogen conveying pipeline 32 and a liquid nitrogen discharge pipe 33, the nitrogen conveying pipeline 32 passes through the second main heat exchanger 205 to be connected with the second molecular sieve 204, the liquid nitrogen discharge pipe 33 extends out of the cold box 300, and the liquid nitrogen discharge pipe 33 is provided with a liquid nitrogen valve 34 for controlling liquid nitrogen discharge. In practical application, the nitrogen rough filtration comprises the following steps: firstly, air in the environment is introduced into an air filter 201, impurities such as dust are filtered and sent into an air compressor 202 for compression, the pressure and density of the air are increased, then the air is introduced into an air cooling unit 203 for cooling, a coolant in the air cooling unit 203 absorbs heat, the air is cooled and condensed into liquid, the cooled air liquid enters a second molecular sieve 204 to remove water and carbon dioxide therein, finally, the air is sent into a nitrogen rectifying tower 206 for rectification, separation is realized according to the boiling point difference of nitrogen and oxygen, and particularly pure nitrogen is separated from the bottom of the nitrogen rectifying tower 206, crude liquid oxygen is separated from the top of the nitrogen rectifying tower 206, wherein the nitrogen rectifying tower 206 can send partial nitrogen into the second molecular sieve 204 through a nitrogen conveying pipeline 32 to be used as purge gas so as to clear or wash adsorbed substances (oxygen, water and carbon dioxide) on the second molecular sieve 204, and normal operation and adsorption performance of the second molecular sieve 204 are ensured; and the liquid nitrogen returned through the second delivery pipe 27 can be discharged from the nitrogen rectification column 206 through the liquid nitrogen discharge pipe 33.
It should be noted that the gas flowing back into the second molecular sieve 204 must be properly treated and controlled to ensure proper operation and performance of the second molecular sieve 204. This includes controlling the flow, pressure and temperature of the reflux gas, as well as periodic molecular sieve regeneration operations.
Further, a third return pipe 35 connected to the top of the nitrogen rectifying tower 206 is disposed at the bottom of the nitrogen rectifying tower 206, and a fourth throttle valve 36 is disposed on the third return pipe 35. It will be appreciated that the third return line 35 is used to return the crude liquid oxygen to the nitrogen condenser at the top of the nitrogen rectification column 206 to provide refrigeration for the condensation of the air rising within the column.
In summary, according to the dual-tower combined argon recovery and purification system in the above embodiment of the present invention, by combining the argon rectification unit with the nitrogen rectification unit, the cold energy of the liquid argon added into the argon condenser can be fully utilized, specifically, when a user adds the liquid argon into the argon condenser through the liquid argon inlet, the nitrogen rectification tower can send part of the nitrogen into the argon condenser through the first conveying pipeline, the nitrogen in the argon condenser can recycle the redundant cold energy of the liquid argon to form liquid nitrogen, and finally the liquid nitrogen is sent back into the nitrogen rectification tower through the second conveying pipeline, and the recovered liquid nitrogen can be sold as a byproduct, so that economic benefits are increased, and cold energy waste caused by normal temperature gasification of the liquid argon is avoided.
Referring to fig. 2, a method for recovering and purifying argon by combining two towers according to a second embodiment of the present invention is shown, which comprises the following steps:
step S101, purifying waste argon, filtering the waste argon from the single crystal furnace to obtain crude argon with nitrogen and hydrogen as impurities;
step S102, crude argon is rectified, the crude argon is introduced into an argon rectifying tower to be rectified and separated according to the characteristic of different boiling points of argon, nitrogen and hydrogen, so that liquid argon is obtained at the bottom of the argon rectifying tower, and rectified waste gas is discharged at the top of the argon rectifying tower, wherein the rectified waste gas comprises hydrogen and nitrogen;
step S103, cold energy recovery, namely transferring part of nitrogen in the nitrogen rectifying tower to the argon rectifying tower through a first conveying pipeline to recover redundant cold energy of liquid argon in the argon rectifying tower to form liquid nitrogen, and then conveying the liquid nitrogen back to the nitrogen rectifying tower through a second conveying pipeline;
and step S104, preparing pure argon, namely extracting liquid argon in the argon rectifying tower and reheating the liquid argon to generate pure argon.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples merely represent a few embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the invention. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. Accordingly, the scope of protection of the present application is to be determined by the claims appended hereto.
Claims (10)
1. A dual column combined argon recovery purification system comprising:
a cold box;
the argon rectification unit is arranged in the cold box and comprises an argon rectification tower, an argon condenser and a liquid argon adding port, wherein the argon condenser is arranged at the top of an inner cavity of the argon rectification tower, the liquid argon adding port is arranged at the top of the argon rectification tower and is communicated with the argon condenser, and the liquid argon adding port is used for adding liquid argon into the argon condenser;
the nitrogen rectification unit is arranged in the cold box and comprises a nitrogen rectification tower, a first conveying pipeline and a second conveying pipeline, wherein the nitrogen rectification tower is communicated with the inlet end of the argon condenser through the first conveying pipeline, and is communicated with the outlet end of the argon condenser through the second conveying pipeline.
2. The double-tower combined argon recovery and purification system according to claim 1, further comprising an argon rough filtering unit and a nitrogen rough filtering unit which are arranged outside the cold box, and a first main heat exchanger and a second main heat exchanger which are arranged inside the cold box, wherein the argon rough filtering unit is used for recovering waste argon from a single crystal furnace and filtering the waste argon into crude argon only containing nitrogen and hydrogen, and the first main heat exchanger is used for receiving the crude argon from the argon rough filtering unit, cooling the crude argon and sending the cooled crude argon into the argon rectifying tower to prepare pure argon;
the nitrogen rough filtering unit is used for extracting air and removing carbon dioxide and water in the air, and the second main heat exchanger is used for receiving the air from the nitrogen rough filtering unit, cooling the air and sending the cooled air into the nitrogen rectifying tower to prepare nitrogen.
3. The dual column combined argon recovery purification system of claim 2 wherein said first main heat exchanger and said second main heat exchanger are integrated.
4. The double-tower combined argon recovery and purification system according to claim 2, wherein the argon rough filtration unit comprises a first molecular sieve and a first argon conveying pipeline, one end of the first argon conveying pipeline is connected with an outlet end of the first molecular sieve, and the other end of the first argon conveying pipeline is sequentially connected with the first main heat exchanger and the argon rectifying tower;
an expander is arranged in the cold box, a third conveying pipeline is externally connected to the first conveying pipeline, the third conveying pipeline is used for conveying nitrogen produced in the nitrogen rectifying tower into the second main heat exchanger for tempering, then the warmed nitrogen is conveyed into the expander for expanding to produce cold energy, then the expanded nitrogen is returned to the cold end of the second main heat exchanger for recycling cold energy, and finally the nitrogen is conveyed out of the second main heat exchanger as purge gas to enter the first molecular sieve, wherein a first throttle valve for controlling the nitrogen to enter the argon condenser is arranged on the first conveying pipeline, and a molecular sieve regeneration heater is arranged on the third conveying pipeline and is used for heating the purge gas to be introduced into the first molecular sieve.
5. The dual-tower combined argon recovery purification system according to claim 4, wherein a reboiler is arranged at the bottom of an inner cavity of the argon rectification tower, one end, far away from the first molecular sieve, of the first argon conveying pipeline is connected with an inlet end of the reboiler, a first return pipe connected with the middle part of the argon rectification tower is arranged at an outlet end of the reboiler, a second return pipe communicated with the argon condenser is arranged at the bottom of the argon rectification tower, a second throttle valve is arranged on the first return pipe, and a third throttle valve is arranged on the second return pipe.
6. The dual-tower combined argon recovery and purification system as claimed in claim 4, wherein an exhaust gas discharge pipe and a pure argon gas discharge pipe are arranged at the top of the argon rectification tower, the exhaust gas discharge pipe passes through the first main heat exchanger to be connected with the first molecular sieve, the pure argon gas discharge pipe passes through the first main heat exchanger to extend out of the cold box, and the tail end of the pure argon gas discharge pipe is connected with a pure argon gas compressor.
7. The dual-tower combined argon recovery and purification system as claimed in claim 4, wherein the argon rough filtration unit further comprises a second argon conveying pipeline, one end of the second argon conveying pipeline is connected to the inlet end of the first molecular sieve, the other end of the second argon conveying pipeline is connected with a dust filter, and a dual-membrane gas holder system, a rough argon compressor, a water cooler, a high-precision oil removal system, a heat regenerator, a rough argon heater, a carbon monoxide removal reactor, a deoxidization reactor and a rough argon cooler are sequentially arranged on the second argon conveying pipeline after the dust filter.
8. The dual column combined argon recovery and purification system of claim 2, wherein the nitrogen rough filtration unit further comprises an air delivery pipeline, one end of the air delivery pipeline passes through the second main heat exchanger to be connected with the nitrogen rectification column, the other end of the air delivery pipeline is connected with an air filter, and an air compressor, an air cooling unit and a second molecular sieve are sequentially arranged on the air delivery pipeline after the air filter;
the top of nitrogen rectification tower is equipped with nitrogen gas pipeline and liquid nitrogen discharge pipe, nitrogen gas pipeline passes the second main heat exchanger is connected the second molecular sieve, the liquid nitrogen discharge pipe stretches out outside the cold box, be equipped with on the liquid nitrogen discharge pipe and be used for controlling liquid nitrogen exhaust liquid nitrogen valve.
9. The double-tower combined argon recovery and purification system according to claim 1, wherein a third return pipe connected with the top of the nitrogen rectifying tower is arranged at the bottom of the nitrogen rectifying tower, and a fourth throttle valve is arranged on the third return pipe.
10. A double-tower combined argon recovery purification method for a double-tower combined argon recovery purification system as claimed in any one of claims 1 to 9, characterized in that the method comprises the steps of:
a) Purifying waste argon, filtering the waste argon from the single crystal furnace to obtain crude argon with nitrogen and hydrogen as impurities;
b) Crude argon is rectified, the crude argon is introduced into an argon rectifying tower to be rectified and separated according to the characteristic of different boiling points of argon, nitrogen and hydrogen, so as to obtain liquid argon at the bottom of the argon rectifying tower, and rectifying waste gas is discharged from the top of the argon rectifying tower, wherein the rectifying waste gas comprises hydrogen and nitrogen;
c) Cold energy recovery, namely transferring part of nitrogen in the nitrogen rectifying tower to the argon rectifying tower through a first conveying pipeline to recover redundant cold energy of liquid argon in the argon rectifying tower to form liquid nitrogen, and then conveying the liquid nitrogen back to the nitrogen rectifying tower through a second conveying pipeline;
d) And (3) preparing pure argon, namely extracting liquid argon in the argon rectifying tower and reheating the liquid argon to generate pure argon.
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| CN202311208147.5A CN117346476A (en) | 2023-09-18 | 2023-09-18 | Double-tower combined argon recovery and purification system and method |
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