Argon recovery equipment capable of stable distillation and working method thereof
By designing a temperature regulating mechanism, argon lifting unit and stabilization member in the argon recovery equipment, the problem of heat load fluctuations during distillation is solved, and the high purity and stable working conditions of argon are achieved.
Patent Information
- Application Number
- CN202510134646.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-07
- Publication Date
- 2025-05-23
- Estimated Expiration
- 2045-02-07
AI Technical Summary
During the distillation process, existing argon recovery equipment causes heat load fluctuations and unstable working conditions, which affects the purity of argon.
An argon recovery device including a temperature regulating mechanism, an argon lifting unit and a stabilizing member is designed. The temperature regulating mechanism regulates the flow rate of dry nitrogen through the main heat exchanger and the nitrogen compressor. The argon lifting unit uses a refined argon tower and an argon tower reboiler for distillation. The stabilization member is controlled through temperature detection and variable speed operation of the nitrogen compressor to adjust the supply of pure argon to ensure the stability of the distillation process.
Through the design of this equipment, the stability and purity of the argon recovery process are guaranteed, the negative impact of thermal load fluctuations on distillation is avoided, and the high purity of the product argon is ensured.
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Figure CN119548842B_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of argon recovery, and in particular to an argon recovery device capable of stable distillation and a working method thereof. Background Art
[0002] At present, a large amount of crude argon gas is emitted during the production of single crystal silicon by the direct pulling method using a reduced pressure crystal pulling process. Recycling and utilizing this argon gas has great practical significance.
[0003] Patent CN116332139A discloses an argon recovery device with integrated high-purity nitrogen and enhanced efficiency and a method for using the same. After pretreatment, the crude argon gas is cooled by a first heat exchanger to obtain dry crude argon gas, which is then transported to the reboiler of the refined argon tower at the bottom of the refined argon tower for liquefaction. The fluid output from the reboiler of the refined argon tower is depressurized and transported to the upper part of the refined argon tower to participate in distillation.
[0004] Due to the temperature error in the pretreatment process and the changes in the composition of the crude argon gas itself, the composition of the dry crude argon gas will fluctuate to a certain extent. Since the liquefaction temperature points of different gas components are different, the temperature of the dry crude argon gas will fluctuate over a large range. This will cause the heat load of the reboiler of the argon tower to fluctuate greatly, which will make the distillation condition unstable, resulting in the purity of the obtained product argon cannot be guaranteed.
[0005] In addition, due to the temperature deviation of the heat exchange in the first heat exchanger, the reboiler of the argon tower may work unstably, thus affecting the distillation. Summary of the invention
[0006] In order to solve the above technical problems and achieve at least one advantage of the present application, the present application provides an argon recovery device capable of stable distillation, the argon recovery device capable of stable distillation comprising a distillation system, the distillation system comprising:
[0007] A temperature regulating mechanism, the temperature regulating mechanism comprises a temperature regulating component and a conducting pipe group, the temperature regulating component comprises a main heat exchanger, the conducting pipe group comprises a feed pipe and a nitrogen pipe group, the main heat exchanger is installed on the feed pipe, the dry crude argon gas is introduced into the main heat exchanger through the feed pipe and discharged after being cooled in the main heat exchanger, and the nitrogen pipe group comprises a first nitrogen conducting pipe;
[0008] An argon extraction unit, the argon extraction unit comprising:
[0009] Argon tower;
[0010] An argon column reboiler, the argon column reboiler is installed in the refined argon column and is located at the bottom of the column. The argon column reboiler is connected to one end of the feed pipe. The cooled and dried crude argon gas obtained by heat exchange in the main heat exchanger is introduced into the argon column reboiler through the portion of the feed pipe located between the main heat exchanger and the argon column reboiler. The cooled and dried crude argon gas is liquefied in the argon column reboiler to obtain crude liquid argon.
[0011] A refined argon pipe group, the refined argon pipe group comprising a first draft pipe, a pure liquid argon connecting pipe and a pure argon gas connecting pipe, wherein two ends of the first draft pipe are respectively connected to the lower end of the argon tower reboiler and the upper end of the refined argon tower;
[0012] a first valve group, wherein the first valve group comprises a crude liquid argon throttle valve, wherein the crude liquid argon throttle valve is installed on the first draft pipe, wherein the crude liquid argon enters the first draft pipe from the argon column reboiler and flows through the crude liquid argon throttle valve to be introduced into the refined argon column after being depressurized by the crude liquid argon throttle valve, wherein the depressurized crude liquid argon is introduced into the refined argon column and then rectified to obtain pure liquid argon at the bottom of the column and argon-nitrogen mixed gas rising to the top of the column, wherein the pure liquid argon is used as a cold source to liquefy the cooled and dried crude argon gas in the argon column reboiler, and is heat-exchanged with the cooled and dried crude argon gas to be partially vaporized to be a part of the argon-nitrogen mixed gas;
[0013] A stabilization component, the stabilization component comprising:
[0014] A stabilization component, the stabilization component comprising:
[0015] A nitrogen compressor, wherein one end of the first nitrogen conduit is connected to the nitrogen compressor, the main heat exchanger is installed on the first nitrogen conduit, the nitrogen compressor introduces dry nitrogen into the first nitrogen conduit, the dry nitrogen is introduced into the main heat exchanger through the first nitrogen conduit to exchange heat in the main heat exchanger and cool down, and the nitrogen compressor can operate at a variable speed to adjust the flow rate of the dry nitrogen introduced into the main heat exchanger;
[0016] A nitrogen reboiler is installed at the other end of the first nitrogen conduit. The cooled and dried nitrogen obtained by heat exchange in the main heat exchanger is introduced into the nitrogen reboiler through the portion of the first nitrogen conduit located between the nitrogen reboiler and the main heat exchanger. Both ends of the pure liquid argon connecting pipe are respectively connected to the nitrogen reboiler and the lower end of the argon refinement tower. Part of the pure liquid argon in the argon refinement tower is introduced into the nitrogen reboiler through the pure liquid argon connecting pipe. The pure liquid argon and the cooled and dried nitrogen are introduced into the nitrogen reboiler. The dry nitrogen is heat exchanged in the nitrogen reboiler to obtain pure argon and liquid nitrogen. The two ends of the pure argon connecting pipe are respectively connected to the lower end of the refined argon tower and the higher end of the nitrogen reboiler. The refined argon tower is connected to the nitrogen reboiler through the pure argon connecting pipe. The pure argon obtained by heat exchange in the nitrogen reboiler is introduced into the refined argon tower through the pure argon connecting pipe, and cooperates with the pure argon gas obtained by heat exchange and gasification of the dried crude argon gas after cooling in the argon tower reboiler, so as to rectify the crude liquid argon after pressure reduction.
[0017] A temperature detecting component is installed in the portion of the feed pipe located between the main heat exchanger and the argon column reboiler, and is used to detect the temperature of the cooled and dried crude argon gas flowing through the portion of the feed pipe located between the main heat exchanger and the argon column reboiler and directed to the argon column reboiler.
[0018] According to an embodiment of the present application, the argon extraction unit further includes an argon tower condenser evaporator, the argon tower condenser evaporator is installed on the top of the refined argon tower, the refined argon pipe group includes a second drainage pipe, the first valve group includes a pure liquid argon throttle valve, the two ends of the second drainage pipe are respectively connected to the lower end of the refined argon tower and the high end of the argon tower condenser evaporator, the pure liquid argon throttle valve is installed on the second drainage pipe, part of the pure liquid argon in the refined argon tower passes through the second drainage pipe and flows through the pure liquid argon throttle valve to be introduced into the argon tower condenser evaporator after being reduced in pressure by the pure liquid argon throttle valve, and the refined argon pipe The group includes a third drainage pipe, the two ends of which are respectively connected to the high end of the refined argon tower and the high end of the argon tower condenser evaporator, the refined argon tower is connected to the argon tower condenser evaporator through the third drainage pipe, so that the argon-nitrogen mixed gas is supplied from the refined argon tower to the argon tower condenser evaporator, the refined argon pipe group also includes a supplementary pipeline, one end of which is connected to the argon tower condenser evaporator to provide external liquid argon to the argon tower condenser evaporator, and the pure liquid argon and the external liquid argon are heat-exchanged as a whole with the argon-nitrogen mixed gas introduced through the third drainage pipe to obtain pure argon, argon-nitrogen mixed liquid and dirty argon.
[0019] According to one embodiment of the present application, the conducting pipe group includes a pure argon gas pipeline and a dirty argon gas pipeline, the dirty argon gas pipeline includes a dirty argon gas main pipe, one end of the pure argon gas pipeline and one end of the dirty argon gas main pipe are both connected to the argon tower condenser evaporator, the pure argon gas obtained by heat exchange in the argon tower condenser evaporator is discharged through the pure argon gas pipeline, and the dirty argon gas obtained by heat exchange in the argon tower condenser evaporator is discharged through the dirty argon gas main pipe, the main heat exchanger is installed on the pure argon gas pipeline and the dirty argon gas main pipe, the pure argon gas flowing through the pure argon gas pipeline to be introduced into the main heat exchanger and the dirty argon gas flowing through the dirty argon gas main pipe to be introduced into the main heat exchanger are used as cold sources to exchange heat with the dry crude argon gas flowing through the feed pipe to be introduced into the main heat exchanger.
[0020] According to one embodiment of the present application, the refined argon pipe group also includes a reflux pipe, the two ends of which are respectively connected to the lower end of the argon tower condenser evaporator and the upper end of the refined argon tower, and the argon tower condenser evaporator is connected to the refined argon tower through the reflux pipe so that the argon tower condenser evaporator supplies argon-nitrogen mixed liquid to the refined argon tower.
[0021] According to an embodiment of the present application, the argon recovery equipment capable of stable distillation includes a raw material pre-impurity removal system, the raw material pre-impurity removal system includes a heat transfer component, the heat transfer component includes a heat transfer assembly and a phase connection group, the heat transfer assembly includes a heating group, the phase connection group includes a first phase connection, the heating group is installed on the first phase connection, the crude argon gas is introduced into the heating group through the first phase connection after compression and oil and dust removal, the heating group is used to heat the crude argon gas, the raw material pre-impurity removal system includes a catalytic reactor group, the catalytic reactor group is connected to one end of the first phase connection, the heated crude argon gas obtained by heating the heating group is introduced into the catalytic reactor group through the first phase connection, the catalytic reactor group is used to remove carbon monoxide and oxygen in the heated crude argon gas to obtain a crude argon gas containing carbon dioxide, the raw material pre-impurity removal system includes The invention comprises an argon precooling and purification system, wherein the phase pipe group further comprises a second phase pipe, and the two ends of the second phase pipe are respectively connected to the catalytic reactor group and the argon precooling and purification system, and the catalytic reactor group is connected to the argon precooling and purification system through the second phase pipe. The heat transfer component also comprises a water cooler, which is installed on the second phase pipe. The crude argon gas containing carbon dioxide obtained by the treatment of the catalytic reactor group flows through the water cooler and is guided to the argon precooling and purification system after being cooled in the water cooler. The argon precooling and purification system is used to remove water and carbon dioxide from the crude argon gas containing carbon dioxide to obtain dry crude argon gas. The argon precooling and purification system is connected to the other end of the feed pipe, and the dry crude argon gas obtained by the treatment of the argon precooling and purification system is introduced into the main heat exchanger through the feed pipe.
[0022] According to an embodiment of the present application, the first phase pipe includes an inlet pipe and a first discharge pipe, the heating group includes a regenerator and an electric heater, the regenerator is connected to one end of the inlet pipe so as to introduce crude argon gas from the inlet pipe to the regenerator, the regenerator is used to preliminarily heat the introduced crude argon gas, the electric heater is connected to the regenerator through a pipeline so as to introduce the preliminarily heated crude argon gas from the regenerator to the electric heater, the electric heater is used to perform secondary heating on the preliminarily heated crude argon gas, the two ends of the first discharge pipe are respectively connected to the electric heater and the catalytic reactor group, the electric heater is connected to the catalytic reactor group through the first discharge pipe so as to introduce the heated crude argon gas from the electric heater to the catalytic reactor group, the inlet pipe includes a feed pipe and an oxygen supply pipe, one end of the feed pipe is connected to the regenerator, the crude argon gas is introduced into the regenerator through the feed pipe, the feed pipe is radially connected with the oxygen supply pipe, the oxygen supply pipe is used to introduce air or oxygen into the feed pipe.
[0023] According to one embodiment of the present application, the second phase connecting pipe includes a heat recovery pipe and a second discharge pipe, the two ends of the heat recovery pipe are respectively connected to the catalytic reactor group and the regenerator, the catalytic reactor group is connected with the regenerator through the heat recovery pipe to introduce crude argon containing carbon dioxide into the regenerator, so as to serve as a heat source for heating the crude argon introduced into the regenerator, the two ends of the second discharge pipe are respectively connected to the regenerator and the argon precooling purification system, the regenerator is connected with the argon precooling purification system through the second discharge pipe, the water cooler is installed on the second discharge pipe, the crude argon containing carbon dioxide discharged from the regenerator flows into the water cooler through the second discharge pipe and is introduced into the argon precooling purification system after being cooled by the water cooler.
[0024] According to an embodiment of the present application, the refined argon pipe group also includes a liquid nitrogen connecting pipe, the stabilization assembly also includes a nitrogen condenser evaporator, the two ends of the liquid nitrogen connecting pipe are respectively connected to the high end of the nitrogen condenser evaporator and the low end of the nitrogen reboiler, the nitrogen reboiler is connected to the nitrogen condenser evaporator through the liquid nitrogen connecting pipe, the first valve group also includes a liquid nitrogen throttle valve, the liquid nitrogen throttle valve is installed on the liquid nitrogen connecting pipe, the liquid nitrogen obtained by heat exchange in the nitrogen reboiler enters the liquid nitrogen connecting pipe and flows through the liquid nitrogen throttle valve to be introduced into the nitrogen condenser evaporator after being reduced in pressure by the liquid nitrogen throttle valve, the dirty argon gas pipeline also includes a dirty argon gas branch pipe, one end of the dirty argon gas branch pipe is connected to the part of the dirty argon gas main pipe located between the main heat exchanger and the argon tower condenser evaporator, and the dirty argon introduced from the argon tower condenser evaporator into the dirty argon gas main pipe The dirty argon gas is introduced into the nitrogen condensing evaporator through the dirty argon gas branch pipe, and the dirty argon gas and liquid nitrogen are heat-exchanged in the nitrogen condensing evaporator to obtain nitrogen and dirty liquid argon. The nitrogen pipe group also includes a second nitrogen conducting pipe, and the two ends of the second nitrogen conducting pipe are respectively connected to the high end of the nitrogen condensing evaporator and the nitrogen compressor, and the main heat exchanger is installed on the second nitrogen conducting pipe. The nitrogen obtained by heat exchange in the nitrogen condensing evaporator is introduced into the main heat exchanger through the second nitrogen conducting pipe to heat exchange with the dry crude argon gas introduced into the main heat exchanger by the argon precooling purification system and the dry nitrogen introduced into the main heat exchanger by the nitrogen compressor to increase the temperature. The heated nitrogen obtained by heat exchange in the main heat exchanger is introduced into the nitrogen compressor through the part of the second nitrogen conducting pipe located between the main heat exchanger and the nitrogen compressor.
[0025] According to an embodiment of the present application, the refined argon pipe group also includes a dirty liquid argon connecting pipe, the two ends of which are respectively connected to the lower end of the nitrogen condensation evaporator and the upper end of the refined argon tower, the nitrogen condensation evaporator is connected to the refined argon tower through the dirty liquid argon connecting pipe, and the dirty liquid argon obtained by heat exchange in the nitrogen condensation evaporator is introduced into the refined argon tower through the dirty liquid argon connecting pipe.
[0026] In order to solve the above technical problems and achieve at least one advantage of the present application, the present application provides a working method of an argon recovery device capable of stable distillation, and the working method of the argon recovery device capable of stable distillation comprises the following steps:
[0027] The dry crude argon gas is introduced into the main heat exchanger through the feed pipe to exchange heat in the main heat exchanger to obtain the dried crude argon gas after cooling. The dried crude argon gas after cooling is introduced into the argon refinement column to be liquefied in the argon column reboiler in the argon refinement column to obtain crude liquid argon. The crude liquid argon enters the first draft pipe from the argon column reboiler and flows through the crude liquid argon throttle valve to be introduced into the argon refinement column after the pressure is reduced by the crude liquid argon throttle valve. The crude liquid argon after the pressure reduction is introduced into the argon refinement column and then rectified to obtain pure liquid argon placed at the bottom of the column and argon-nitrogen mixed gas rising to the top of the column, wherein the pure liquid argon serves as a cold source to liquefy the dried crude argon gas after cooling in the argon column reboiler. The pure liquid argon exchanges heat with the dried crude argon gas after cooling to be partially vaporized to serve as a part of the argon-nitrogen mixed gas. The argon-nitrogen mixed gas rising in the argon refinement column is in gas-liquid contact with the crude liquid argon gas after pressure reduction flowing downward in the argon refinement column to transfer mass and heat;
[0028] The temperature detecting element detects the temperature of the cooled dry crude argon gas flowing through the portion of the feed pipe between the main heat exchanger and the argon column reboiler and directed to the argon column reboiler. The running speed of the nitrogen compressor is adjusted according to the detected temperature of the cooled dry crude argon gas to regulate the flow rate of the dry nitrogen gas directed to the main heat exchanger. The nitrogen compressor introduces dry nitrogen into the main heat exchanger through the first nitrogen conducting pipe to exchange heat in the main heat exchanger to obtain cooled dry nitrogen gas. Dry nitrogen is introduced into the nitrogen reboiler through the portion of the first nitrogen conducting pipe located between the nitrogen reboiler and the main heat exchanger, part of the pure liquid argon in the refined argon column is introduced into the nitrogen reboiler through the pure liquid argon connecting pipe, pure liquid argon and the cooled dry nitrogen are heat exchanged in the nitrogen reboiler to obtain pure argon and liquid nitrogen, pure argon is introduced into the refined argon column through the pure argon connecting pipe, and cooperates with the pure argon gas obtained by gasification through heat exchange with the cooled dry crude argon in the argon column reboiler, so that the distillation process can be carried out stably.
[0029] The beneficial effects of this application include:
[0030] 1. By utilizing the coordinated effect of the argon refinement tower, the argon tower reboiler and the stabilizing component, according to the amount of pure argon gas vaporized by heat exchange between the pure liquid argon obtained by rectification in the argon refinement tower and the dry crude argon gas after cooling in the argon tower reboiler, the supply amount of dry nitrogen is adaptively adjusted through the stabilizing component to adjust the amount of pure argon gas supplied from the nitrogen reboiler to the argon refinement tower, so as to match the actual working condition of the argon tower reboiler, improve the anti-interference ability of the argon extraction unit, make the evaporation amount during the rectification of the crude liquid argon after pressure reduction remain constant, ensure the stability of the distillation process, and further ensure the purity of the obtained pure argon gas.
[0031] 2. By adding air or oxygen to the crude argon gas, the ratio of carbon monoxide to oxygen is maintained at 2:1, ensuring that the carbon monoxide is fully removed during the subsequent treatment in the catalytic reactor group. Compared with the prior art, there is no need to introduce hydrogen during deoxygenation, which simplifies the argon extraction process, improves the safety of the equipment, and reduces the processing cost.
[0032] 3. By cooling and supercooling the external liquid argon, sufficient cooling capacity is provided for the heat exchange operation in the condenser evaporator of the argon tower. Compared with the uncooled liquid argon, the argon extraction rate is guaranteed while the supplementary amount can be as low as possible, thereby reducing the use of liquid argon. BRIEF DESCRIPTION OF THE DRAWINGS
[0033] Figure 1 The structural flow chart of the argon recovery equipment capable of stable distillation described in the present application is shown.
[0034] Figure 2 The structural flow chart of the raw material pre-impurity removal system of the argon recovery equipment capable of stable distillation described in the present application is shown.
[0035] Figure 3 A partial structural flow chart of the argon recovery equipment capable of stable distillation described in the present application is shown.
[0036] Figure 4 Another partial structural flow chart of the argon recovery equipment capable of stable distillation described in the present application is shown.
[0037] Figure 5 Another partial structural flow chart of the argon recovery equipment capable of stable distillation described in the present application is shown.
[0038] Reference numerals:
[0039] 10. Raw material pre-impurity removal system; 11. Heat transfer component; 111. Heat transfer assembly; 1111. Heating group; 11111. Regenerator; 11112. Electric heater; 1112. Water cooler; 112. Pipe connection group; 1121. First pipe connection; 11211. Inlet pipe; 112111. Feed pipe; 112112. Oxygen supply pipe; 11212. First discharge pipe; 1122. Second pipe connection; 11221. Heat recovery pipe; 11222. Second discharge pipe; 12. Catalytic reactor group; 13. Argon precooling and purification system; 14. First compressor;
[0040] 20. Distillation system; 21. Temperature adjustment mechanism; 211. Temperature adjustment component; 2111. Main heat exchanger; 2112. Temperature adjustment component; 21121. Auxiliary heat exchanger; 21122. Expander; 2113. Subcooler group; 21131. First subcooler; 21132. Second subcooler; 212. Conducting pipe group; 2121. Feed pipe; 2122. Pure argon pipeline; 2123. Sewage argon pipeline; 21231. Sewage argon main pipe; 21232. Sewage argon branch pipe; 2124. Nitrogen pipe group; 21241, first nitrogen conduit; 21242, second nitrogen conduit; 2125, dry air pipeline; 21251, dry air inlet pipe; 21252, dry air outlet pipe; 212521, branch pipeline; 212522, main pipeline; 2126, oxygen-enriched air pipeline; 21261, oxygen-enriched air main pipeline; 21262, liquid nitrogen pipe body; 2127, nitrogen pipeline; 22, argon extraction unit; 221, refined argon tower; 222, argon tower reboiler; 223, refined argon pipe group; 2231 , first drainage pipe; 2232, second drainage pipe; 2233, third drainage pipe; 2234, supplementary pipeline; 2235, reflux pipeline; 2236, pure liquid argon connecting pipe; 2237, pure argon gas connecting pipe; 2238, liquid nitrogen connecting pipe; 2239, dirty liquid argon connecting pipe; 224, first valve group; 2241, crude liquid argon throttle valve; 2242, pure liquid argon throttle valve; 2243, external liquid argon control valve; 2244, liquid nitrogen throttle valve; 225, argon tower condenser evaporator; 226, stabilizing component; 2261, stabilization assembly; 22611, nitrogen compressor; 22612, nitrogen reboiler; 22613, nitrogen condenser evaporator; 2262, temperature detection element; 23, auxiliary unit; 231, nitrogen tower; 232, auxiliary pipeline; 2321, first flow guide pipeline; 2322, second flow guide pipeline; 2323, third flow guide pipeline; 233, nitrogen tower condenser evaporator; 234, second valve group; 2341, oxygen-enriched liquid throttle valve; 2342, dry air throttle valve; 2343, liquid nitrogen control valve;
[0041] 30. Air pretreatment system; 31. Air purification device; 32. Second compressor. DETAILED DESCRIPTION
[0042] The following description is used to disclose the present application so that those skilled in the art can implement the present application. The preferred embodiments described below are only examples, and those skilled in the art can think of other obvious variations. The basic principles of the present application defined in the following description can be applied to other embodiments, variations, improvements, equivalent solutions, and other technical solutions that do not deviate from the spirit and scope of the present application.
[0043] Those skilled in the art should understand that, in the disclosure of the present application, the terms "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship are based on the orientation or position relationship shown in the drawings, which are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. Therefore, the above terms should not be understood as limiting the present application.
[0044] It is to be understood that the term "one" should be understood as "at least one" or "one or more", that is, in one embodiment, the number of an element may be one, while in another embodiment, the number of the element may be multiple, and the term "one" should not be understood as a limitation on the quantity.
[0045] refer to Figure 1 to Figure 2 According to a preferred embodiment of the present application, an argon recovery device capable of stable distillation will be described in detail below. The argon recovery device capable of stable distillation is used to recover crude argon gas, wherein the gas components in the crude argon gas include oxygen, nitrogen, carbon monoxide and argon, wherein the oxygen content is 0~1000ppm, the nitrogen content is 0~0.4%, the carbon monoxide content is 0~2000ppm, and the rest is argon.
[0046] The argon recovery equipment capable of stable distillation includes a raw material pre-impurity removal system 10, and the raw material pre-impurity removal system 10 includes a heat transfer component 11, and the heat transfer component 11 includes a heat transfer assembly 111 and a phase connection group 112, and the heat transfer assembly 111 includes a heating group 1111, and the phase connection group 112 includes a first phase connection 1121, and the heating group 1111 is installed on the first phase connection 1121. After being compressed and deoiled and dusted, the crude argon gas is introduced into the heating group 1111 through the first phase connection 1121, and the heating group 1111 is used to heat the crude argon gas.
[0047] The raw material pre-impurity removal system 10 includes a catalytic reactor group 12, and the catalytic reactor group 12 is connected to one end of the first phase connecting pipe 1121. The heated crude argon gas obtained by heating the heating group 1111 is introduced into the catalytic reactor group 12 through the first phase connecting pipe 1121. The catalytic reactor group 12 is used to remove carbon monoxide and oxygen in the heated crude argon gas to obtain crude argon gas containing carbon dioxide.
[0048] Preferably, the catalytic reactor group 12 is implemented to include at least three catalytic furnaces connected in series or in parallel, each of which is provided with a catalyst and a copper-based catalyst as a getter. The catalytic reaction of the catalyst is: 2CO+O 2 =2CO2 ; The role of the getter makes the following reactions interactive: (1): 2X+O 2 =2XO; (2): XO+CO=X+CO 2 .
[0049] The first phase connection pipe 1121 includes an inlet pipe 11211 and a first outlet pipe 11212. The heating group 1111 includes a regenerator 11111 and an electric heater 11112. The regenerator 11111 is connected to one end of the inlet pipe 11211 so as to introduce crude argon gas from the inlet pipe 11211 to the regenerator 11111. The regenerator 11111 is used to preliminarily heat the introduced crude argon gas. The electric heater 11112 is connected to the regenerator 11111 through a pipeline so as to introduce the preliminarily heated crude argon gas from the regenerator 11111 to the electric heater 11112. The electric heater 11112 is used to perform secondary heating on the preliminarily heated crude argon gas. The two ends of the first exhaust pipe 11212 are respectively connected to the electric heater 11112 and the catalytic reactor group 12. The electric heater 11112 is connected to the catalytic reactor group 12 through the first exhaust pipe 11212 so that the heated crude argon gas is introduced into the catalytic reactor group 12 by the electric heater 11112.
[0050] Preferably, the inlet pipe 11211 includes a feed pipe 112111 and an oxygen supply pipe 112112, one end of the feed pipe 112111 is connected to the regenerator 11111, and the crude argon gas is introduced into the regenerator 11111 through the feed pipe 112111. The feed pipe 112111 is connected to the oxygen supply pipe 112112 in the radial direction, and the oxygen supply pipe 112112 is used to introduce air or oxygen into the feed pipe 112111, so that when the oxygen content in the crude argon gas is lower than 1000ppm, the ratio of carbon monoxide to oxygen is maintained at 2:1 by supplementing air or oxygen, so as to ensure that the carbon monoxide in the crude argon gas after heating is fully removed after being processed by the catalytic reactor group 12. Compared with the prior art, hydrogen does not need to be introduced during deoxygenation, which simplifies the argon extraction process, improves the safety of the equipment, and reduces the processing cost.
[0051] The argon recovery equipment capable of stable distillation further includes an argon precooling and purification system 13, and the phase pipe group 112 further includes a second phase pipe 1122, the two ends of the second phase pipe 1122 are respectively connected to the catalytic reactor group 12 and the argon precooling and purification system 13, and the catalytic reactor group 12 is connected to the argon precooling and purification system 13 through the second phase pipe 1122. The heat transfer component 111 further includes a water cooler 1112, and the water cooler 1112 is installed on the second phase pipe 1122. The crude argon gas containing carbon dioxide obtained by the treatment of the catalytic reactor group 12 flows through the water cooler 1112 and is cooled in the water cooler 1112 before being guided to the argon precooling and purification system 13. The argon precooling and purification system 13 is used to remove water and carbon dioxide from the crude argon gas containing carbon dioxide to obtain dry crude argon gas.
[0052] Preferably, the argon precooling and purification system 13 is filled with alumina and molecular sieves.
[0053] It is worth mentioning that the second phase connection pipe 1122 includes a heat recovery pipe 11221 and a second discharge pipe 11222. The two ends of the heat recovery pipe 11221 are respectively connected to the catalytic reactor group 12 and the regenerator 11111. The catalytic reactor group 12 is connected to the regenerator 11111 through the heat recovery pipe 11221 to introduce crude argon containing carbon dioxide into the regenerator 11111 as a heat source for heating the crude argon introduced into the regenerator 11111. The two ends of the second discharge pipe 11222 are respectively connected to the regenerator 11111 and the argon precooling and purification system 13. The regenerator 11111 is connected to the argon precooling and purification system 13 through the second discharge pipe 11222. The water cooler 1112 is installed on the second exhaust pipe 11222. The crude argon gas containing carbon dioxide discharged from the regenerator 11111 flows into the water cooler 1112 through the second exhaust pipe 11222 and is introduced into the argon precooling purification system 13 after being cooled by the water cooler 1112.
[0054] The raw material pre-impurity removal system 10 also includes a first compressor 14, which is installed on the feed pipe 112111. The first compressor 14 is connected to the regenerator 11111 through the feed pipe 112111. The crude argon gas after oil and dust removal is compressed by the first compressor 14 and introduced into the regenerator 11111 through the feed pipe 112111.
[0055] Preferably, the temperature of the crude argon gas guided to the first compressor 14 by the feed pipe 112111 is 25-30°C, and the temperature of the crude argon gas after compression by the first compressor 14 is 35-40°C. The temperature of the heated crude argon gas obtained by heating in the regenerator 11111 is 170-180°C, and the temperature of the heated crude argon gas after secondary heating by the electric heater 11112 is 200-220°C. The contents of carbon monoxide and oxygen in the crude argon gas containing carbon dioxide obtained by treatment in the catalytic reactor group 12 are both not greater than 1 ppm, and the temperature of the crude argon gas containing carbon dioxide is 200-250°C. The temperature of the crude argon gas containing carbon dioxide after heat recovery in the regenerator 11111 is 75-80°C, and the temperature of the crude argon gas containing carbon dioxide after cooling obtained by treatment in the water cooler 1112 is 35-40°C. The temperature of the dry crude argon gas obtained by the argon precooling and purification system 13 is 15-25° C., wherein the nitrogen content in the dry crude argon gas is 0.4%.
[0056] refer to Figure 1 , Figure 3 and Figure 4 The argon recovery equipment capable of stable distillation also includes a distillation system 20, the distillation system 20 includes a temperature control mechanism 21, the temperature control mechanism 21 includes a temperature control component 211 and a conducting pipe group 212, the temperature control component 211 includes a main heat exchanger 2111, the conducting pipe group 212 includes a feed pipe 2121, the main heat exchanger 2111 is installed on the feed pipe 2121, the argon precooling and purification system 13 is connected to one end of the feed pipe 2121, the dry crude argon gas obtained by the argon precooling and purification system 13 is introduced into the main heat exchanger 2111 through the feed pipe 2121 and discharged after being cooled in the main heat exchanger 2111.
[0057] The distillation system 20 includes an argon extraction unit 22, which includes an argon refinement column 221 and an argon column reboiler 222. The argon column reboiler 222 is installed in the argon refinement column 221 and is located at the bottom of the column. The argon column reboiler 222 is connected to the other end of the feed pipe 2121. The cooled and dried crude argon gas obtained by heat exchange in the main heat exchanger 2111 is introduced into the argon column reboiler 222 through the portion of the feed pipe 2121 located between the main heat exchanger 2111 and the argon column reboiler 222. The cooled and dried crude argon gas is liquefied in the argon column reboiler 222 to obtain crude liquid argon.
[0058] The argon extraction unit 22 includes a refined argon pipe group 223 and a first valve group 224. The refined argon pipe group 223 includes a first draft pipe 2231. The first valve group 224 includes a crude liquid argon throttle valve 2241. The two ends of the first draft pipe 2231 are respectively connected to the lower end of the argon column reboiler 222 and the upper end of the refined argon column 221. The crude liquid argon throttle valve 2241 is installed on the first draft pipe 2231. Crude liquid argon enters the first draft pipe 2231 from the argon column reboiler 222 and flows through the crude liquid argon throttle valve 2241 to be introduced into the refined argon column 221 after being depressurized by the crude liquid argon throttle valve 2241.
[0059] Due to the pressure difference, the boiling point temperature will change according to the pressure, which makes the pressure-reduced crude liquid argon obtained by reducing the pressure through the crude liquid argon throttle valve 2241 and the temperature-reduced dry crude argon gas in the argon tower reboiler 222 have a temperature difference, so that the heat exchange operation can be carried out normally. The depressurized crude liquid argon is introduced into the refined argon tower 221 and then distilled to obtain pure liquid argon placed at the bottom of the tower and argon-nitrogen mixed gas rising to the top of the tower, wherein the pure liquid argon is used as a cold source to liquefy the temperature-reduced dry crude argon gas in the argon tower reboiler 222, and the pure liquid argon exchanges heat with the temperature-reduced dry crude argon gas to partially gasify it as a part of the argon-nitrogen mixed gas, and the argon-nitrogen mixed gas rising in the refined argon tower 221 is in gas-liquid contact with the depressurized crude liquid argon flowing downward in the refined argon tower 221 to transfer mass and heat.
[0060] The argon extraction unit 22 further includes an argon tower condenser evaporator 225, which is installed on the top of the argon refinement tower 221. The argon refinement pipe group 223 includes a second draft pipe 2232, and the two ends of the second draft pipe 2232 are respectively connected to the lower end of the argon refinement tower 221 and the upper end of the argon tower condenser evaporator 225. The first valve group 224 includes a pure liquid argon throttle valve 2242, which is installed on the second draft pipe 2232. Part of the pure liquid argon in the argon refinement tower 221 passes through the second draft pipe 2232 and the pure liquid argon throttle valve 2242, and is introduced into the argon tower condenser evaporator 225 after being reduced in pressure by the pure liquid argon throttle valve 2242.
[0061] The refined argon pipe group 223 includes a third drainage pipe 2233, and the two ends of the third drainage pipe 2233 are respectively connected to the high end of the refined argon tower 221 and the high end of the argon tower condenser evaporator 225. The refined argon tower 221 is connected to the argon tower condenser evaporator 225 through the third drainage pipe 2233, so that the refined argon tower 221 supplies argon-nitrogen mixed gas to the argon tower condenser evaporator 225.
[0062] The refined argon pipe group 223 further includes a supplementary pipe 2234 and a reflux pipe 2235. One end of the supplementary pipe 2234 is connected to the argon tower condenser evaporator 225 to provide external liquid argon to the argon tower condenser evaporator 225. Pure liquid argon and external liquid argon are heat exchanged with the argon nitrogen mixed gas introduced by the third draft pipe 2233 to obtain pure argon, argon nitrogen mixed liquid and dirty argon. The two ends of the reflux pipe 2235 are respectively connected to the lower end of the argon tower condenser evaporator 225 and the upper end of the refined argon tower 221. The argon tower condenser evaporator 225 is connected to the refined argon tower 221 through the reflux pipe 2235, so that the argon nitrogen mixed liquid is supplied to the refined argon tower 221 from the argon tower condenser evaporator 225. The argon nitrogen mixed liquid flows downward in the refined argon tower 221 and performs heat and mass transfer with the argon nitrogen mixed gas rising in the refined argon tower 221, so as to recover argon as much as possible.
[0063] It is worth mentioning that the external liquid argon introduced by the supplementary pipe 2234 is introduced into the argon tower condenser evaporator 225 after cold treatment, so as to provide sufficient cooling capacity for the heat exchange operation in the argon tower condenser evaporator 225. Compared with the uncooled liquid argon, the supplementary amount can be as low as possible while the argon extraction rate is guaranteed, thereby reducing the use of liquid argon.
[0064] Preferably, the temperature of the external liquid argon introduced into the argon tower condenser evaporator 225 is -182-184° C., which reduces the liquid argon consumption by 20% based on the same argon extraction rate compared with the uncooled liquid argon.
[0065] Preferably, the first valve group 224 also includes an external liquid argon control valve 2243, which is installed on the supplementary pipe 2234. The external liquid argon control valve 2243 is used to adjust the flow of external liquid argon directed to the argon tower condenser evaporator 225, so that the external liquid argon supplemented to the argon tower condenser evaporator 225 can meet the required cooling demand without being wasted.
[0066] The conducting pipe group 212 includes a pure argon gas pipeline 2122 and a dirty argon gas pipeline 2123, and the dirty argon gas pipeline 2123 includes a dirty argon gas main pipe 21231. One end of the pure argon gas pipeline 2122 and one end of the dirty argon gas main pipe 21231 are both connected to the argon tower condenser evaporator 225. The pure argon gas obtained by heat exchange in the argon tower condenser evaporator 225 is discharged through the pure argon gas pipeline 2122 for use by users. The dirty argon gas obtained by heat exchange in the argon tower condenser evaporator 225 is discharged through the dirty argon gas main pipe 21231 for venting.
[0067] Preferably, the main heat exchanger 2111 is installed on the pure argon gas pipeline 2122 and the dirty argon gas main pipe 21231, and the pure argon gas flowing through the pure argon gas pipeline 2122 to be introduced into the main heat exchanger 2111 and the dirty argon gas flowing through the dirty argon gas main pipe 21231 to be introduced into the main heat exchanger 2111 serve as cold sources to exchange heat with the dry crude argon gas flowing through the feed pipe 2121 to be introduced into the main heat exchanger 2111.
[0068] It is worth mentioning that the argon extraction unit 22 also includes a stabilizing component 226, the stabilizing component 226 includes a stabilizing assembly 2261, the stabilizing assembly 2261 includes a nitrogen compressor 22611, the conducting pipe group 212 includes a nitrogen pipe group 2124, the nitrogen pipe group 2124 includes a first nitrogen conducting pipe 21241, one end of the first nitrogen conducting pipe 21241 is connected to the nitrogen compressor 22611, the main heat exchanger 2111 is installed on the first nitrogen conducting pipe 21241, the nitrogen compressor 22611 introduces dry nitrogen into the first nitrogen conducting pipe 21241, and the dry nitrogen is introduced into the main heat exchanger 2111 through the first nitrogen conducting pipe 21241 to exchange heat with the pure argon and dirty argon introduced into the main heat exchanger 2111 in the main heat exchanger 2111 to cool down.
[0069] The stabilization component 2261 further includes a nitrogen reboiler 22612, which is installed at the other end of the first nitrogen conduit 21241. The cooled and dried nitrogen obtained by heat exchange in the main heat exchanger 2111 is introduced into the nitrogen reboiler 22612 through the first nitrogen conduit 21241 located between the nitrogen reboiler 22612 and the main heat exchanger 2111. The refined argon pipe group 223 further includes a pure liquid argon connecting pipe 2236, the two ends of which are respectively connected to the nitrogen reboiler 22612 and the lower end of the refined argon tower 221, and part of the pure liquid argon in the refined argon tower 221 is introduced into the nitrogen reboiler 22612 through the pure liquid argon connecting pipe 2236. Pure liquid argon and cooled and dried nitrogen exchange heat in the nitrogen reboiler 22612 to obtain pure argon and liquid nitrogen.
[0070] The refined argon pipe group 223 further includes a pure argon gas connecting pipe 2237, the two ends of which are respectively connected to the lower end of the refined argon tower 221 and the upper end of the nitrogen reboiler 22612, and the refined argon tower 221 is connected to the nitrogen reboiler 22612 through the pure argon gas connecting pipe 2237. The pure argon gas obtained by heat exchange in the nitrogen reboiler 22612 is introduced into the refined argon tower 221 through the pure argon gas connecting pipe 2237, and cooperates with the pure argon gas obtained by heat exchange and gasification of the dried crude argon gas after cooling in the argon tower reboiler 222, so as to rectify the crude liquid argon after pressure reduction.
[0071] The stabilizing member 226 includes a temperature detecting member 2262, which is installed at the portion of the feed pipe 2121 between the main heat exchanger 2111 and the argon column reboiler 222, and is used to detect the temperature of the reduced-temperature dry crude argon gas flowing through the portion of the feed pipe 2121 between the main heat exchanger 2111 and the argon column reboiler 222 and directed to the argon column reboiler 222. The nitrogen compressor 22611 can be operated at a variable speed to adjust the flow rate of the dry nitrogen gas directed to the main heat exchanger 2111.
[0072] Specifically, when the temperature detecting element 2262 detects that the temperature of the dried crude argon gas after cooling is maintained outside the predetermined temperature range, the flow rate of the dry nitrogen gas directed to the main heat exchanger 2111 is adjusted by the nitrogen compressor 22611, that is, when the temperature of the dried crude argon gas after cooling is too low, the cooling capacity required for liquefying the dried crude argon gas after cooling in the argon tower reboiler 222 is reduced, which reduces the evaporation amount during the distillation of the crude liquid argon after pressure reduction. At this time, the operating speed of the nitrogen compressor 22611 is increased to increase the flow rate of the dry nitrogen gas directed to the main heat exchanger 2111, so that the flow rate of the dried nitrogen gas after cooling introduced into the nitrogen reboiler 22612 is increased. The amount of pure argon obtained by heat exchange in the nitrogen reboiler 22612 increases, so as to provide more pure argon to the refined argon tower 221, thereby ensuring that the gas-liquid two-phase in the refined argon tower 221 reaches equilibrium; when the temperature of the dry crude argon after cooling is too high, the cooling capacity required for liquefaction of the dry crude argon after cooling in the argon tower reboiler 222 increases, which increases the evaporation amount during distillation of the crude liquid argon after pressure reduction. At this time, the operating speed of the nitrogen compressor 22611 is reduced to reduce the flow rate of the dry nitrogen directed to the main heat exchanger 2111, so as to reduce the pure argon supplied to the refined argon tower 221, so as to achieve better distillation effect and save energy.
[0073] In this way, by utilizing the coordinated effect of the refined argon tower 221, the argon tower reboiler 222 and the stabilizing component 226, according to the amount of pure argon gasified by heat exchange between the pure liquid argon obtained by rectification in the refined argon tower 221 and the dried crude argon gas after cooling in the argon tower reboiler 222, the supply amount of dry nitrogen is adaptively adjusted through the stabilizing component 226 to adjust the amount of pure argon gas supplied from the nitrogen reboiler 22612 to the refined argon tower 221, so as to match the actual working condition of the argon tower reboiler 222, improve the anti-interference ability of the argon extraction unit 22, make the evaporation amount during the distillation of the crude liquid argon after pressure reduction constant, ensure the stability of the distillation process, and further ensure the purity of the obtained pure argon gas. Compared with the prior art, it effectively prevents the fluctuation of the component of the dried crude argon gas after cooling or the deviation of the heat exchange temperature of the main heat exchanger 2111, so as to prevent the heat load of the argon tower reboiler 222 from fluctuating and affecting the distillation effect.
[0074] Preferably, the temperature detecting element 2262 is implemented as a thermometer.
[0075] The refined argon pipe group 223 further includes a liquid nitrogen connecting pipe 2238, and the stabilization assembly 2261 further includes a nitrogen condenser evaporator 22613. The two ends of the liquid nitrogen connecting pipe 2238 are respectively connected to the high end of the nitrogen condenser evaporator 22613 and the low end of the nitrogen reboiler 22612, and the nitrogen reboiler 22612 is connected to the nitrogen condenser evaporator 22613 through the liquid nitrogen connecting pipe 2238. The first valve group 224 further includes a liquid nitrogen throttle valve 2244, and the liquid nitrogen throttle valve 2244 is installed on the liquid nitrogen connecting pipe 2238. The liquid nitrogen obtained by heat exchange in the nitrogen reboiler 22612 enters the liquid nitrogen connecting pipe 2238 and flows through the liquid nitrogen throttle valve 2244 to be introduced into the nitrogen condenser evaporator 22613 after being reduced in pressure by the liquid nitrogen throttle valve 2244.
[0076] The dirty argon gas pipeline 2123 further includes a dirty argon gas branch pipe 21232, one end of which is connected to the dirty argon gas main pipe 21231 located between the main heat exchanger 2111 and the argon tower condenser evaporator 225. The dirty argon gas introduced from the argon tower condenser evaporator 225 into the dirty argon gas main pipe 21231 is introduced into the nitrogen condenser evaporator 22613 through the dirty argon gas branch pipe 21232. The dirty argon gas and liquid nitrogen exchange heat in the nitrogen condenser evaporator 22613 to obtain nitrogen and dirty liquid argon. The nitrogen pipe group 2124 further includes a second nitrogen gas conducting pipe 21242, the two ends of which are respectively connected to the high end of the nitrogen condenser evaporator 22613 and the nitrogen compressor 22611, and the main heat exchanger 2111 is installed on the second nitrogen gas conducting pipe 21242. The nitrogen obtained by heat exchange in the nitrogen condensation evaporator 22613 is introduced into the main heat exchanger 2111 through the second nitrogen conduit 21242 to heat and heat up with the dry crude argon gas introduced into the main heat exchanger 2111 by the argon precooling purification system 13 and the dry nitrogen gas introduced into the main heat exchanger 2111 by the nitrogen compressor 22611. The heated nitrogen obtained by heat exchange in the main heat exchanger 2111 is introduced into the nitrogen compressor 22611 through the second nitrogen conduit 21242 located between the main heat exchanger 2111 and the nitrogen compressor 22611, so as to realize the recycling of nitrogen and save nitrogen source.
[0077] The refined argon pipe group 223 further includes a dirty liquid argon connecting pipe 2239, the two ends of which are respectively connected to the lower end of the nitrogen condenser evaporator 22613 and the upper end of the refined argon tower 221. The nitrogen condenser evaporator 22613 is connected to the refined argon tower 221 through the dirty liquid argon connecting pipe 2239, and the dirty liquid argon obtained by heat exchange in the nitrogen condenser evaporator 22613 is introduced into the refined argon tower 221 through the dirty liquid argon connecting pipe 2239. While the dirty liquid argon flows downward in the refined argon tower 221, it performs heat and mass transfer with the argon-nitrogen mixed gas rising in the refined argon tower 221, so as to recover argon as much as possible.
[0078] Preferably, the temperature of the cooled and dried crude argon gas directed to the argon column reboiler 222 after cooling by the main heat exchanger 2111 is -155~-160°C. The temperature of the crude liquid argon discharged from the argon column reboiler 222 is -158~-160°C, and the temperature of the crude liquid argon after the pressure reduction by the crude liquid argon throttle valve 2241 is -161~-163°C. The nitrogen content in the pure liquid argon discharged from the refined argon column 221 is not more than 4ppm, the temperature of the pure liquid argon is -161~-163°C, and the temperature of the pure liquid argon after the pressure reduction by the pure liquid argon throttle valve 2242 is -163~-165°C. The temperature of the argon-nitrogen mixed gas directed to the argon tower condenser evaporator 225 is -162~-164°C, the temperature of the dirty argon gas discharged from the argon tower condenser evaporator 225 is -162~-164°C, the temperature of the argon-nitrogen mixed liquid discharged from the argon tower condenser evaporator 225 is -162~-164°C, and the temperature of the pure argon gas discharged from the argon tower condenser evaporator 225 is -163~-165°C. The temperature of the pure argon gas and the dirty argon gas after heat exchange in the main heat exchanger 2111 is 10~20°C. The temperature of the external liquid argon introduced into the argon tower condenser evaporator 225 is -182~-184°C. The temperature of the dry nitrogen discharged from the nitrogen compressor 22611 and directed to the main heat exchanger 2111 through the first nitrogen conduit 21241 and the heated nitrogen that is heated in the main heat exchanger 2111 and directed to the nitrogen compressor 22611 through the second nitrogen conduit 21242 are both 10-20°C. The temperature of the cooled dry nitrogen gas which is cooled by heat exchange in the main heat exchanger 2111 and then directed to the nitrogen reboiler 22612 is -153~-158°C, the temperature of the pure argon gas discharged from the nitrogen reboiler 22612 is -160°C, the temperature of the liquid nitrogen discharged from the nitrogen reboiler 22612 is -158~-160°C, the temperature of the liquid nitrogen after pressure reduction by the liquid nitrogen throttle valve 2244 is -174~-178°C, the temperature of the nitrogen gas discharged from the nitrogen condensation evaporator 22613 is -162~-164°C, and the temperature of the dirty liquid argon discharged from the nitrogen condensation evaporator 22613 is -161~-163°C.
[0079] refer to Figure 1 and Figure 5 The argon recovery equipment capable of stable distillation also includes an air pretreatment system 30, and the air pretreatment system 30 includes an air purification device 31. The compressed air is passed into the air purification device 31 to adsorb carbon dioxide and water by the air purification device 31 to obtain dry air.
[0080] The air pretreatment system 30 further includes a second compressor 32 . The second compressor 32 is connected to the air purification device 31 through a pipeline. The air is compressed by the second compressor 32 and then introduced into the air purification device 31 .
[0081] Preferably, the temperature of the air introduced into the second compressor 32 is 20-25°C, the temperature of the air after being compressed by the second compressor 32 is 35-40°C, and the temperature of the dry air obtained by the air purification device 31 is 15-25°C.
[0082] The conducting pipe group 212 also includes a dry air duct 2125. The air purification device 31 is installed at one end of the dry air duct 2125. The main heat exchanger 2111 is installed on the dry air duct 2125. The dry air discharged from the air purification device 31 is introduced into the main heat exchanger 2111 through the dry air duct 2125 to exchange heat with the pure argon gas introduced into the main heat exchanger 2111 through the pure argon gas pipe 2122, the dirty argon gas introduced into the main heat exchanger 2111 through the dirty argon gas main pipe 21231, and the nitrogen introduced into the main heat exchanger 2111 through the second nitrogen conducting pipe 21242 to reduce the temperature.
[0083] refer to Figure 1 and Figure 5 The distillation system 20 further includes an auxiliary unit 23, which includes a nitrogen refiner 231. The nitrogen refiner 231 is connected to the other end of the dry air duct 2125. The temperature control component 211 includes a temperature control assembly 2112, which is installed in the dry air duct 2125 between the main heat exchanger 2111 and the nitrogen refiner 231. The cooled dry air discharged from the main heat exchanger 2111 flows through the dry air duct 2125 to the temperature control assembly 2112, and is cooled again by the temperature control assembly 2112 and then guided to the nitrogen refiner 231. The cooled dry air is distilled in the nitrogen refiner 231 to obtain oxygen-rich liquid and nitrogen.
[0084] The auxiliary unit 23 includes an auxiliary pipeline 232 and a nitrogen tower condenser evaporator 233. The auxiliary pipeline 232 includes a first flow guide pipeline 2321. The two ends of the first flow guide pipeline 2321 are respectively connected to the high end of the refined nitrogen tower 231 and the high end of the nitrogen tower condenser evaporator 233. The refined nitrogen tower 231 is connected to the nitrogen tower condenser evaporator 233 through the first flow guide pipeline 2321. The nitrogen rising in the refined nitrogen tower 231 is introduced into the nitrogen tower condenser evaporator 233 through the first flow guide pipeline 2321.
[0085] The temperature regulating member 211 includes a subcooler group 2113. The subcooler group 2113 includes a first subcooler 21131. The auxiliary pipeline 232 includes a second diversion pipeline 2322. The two end portions of the second diversion pipeline 2322 are respectively connected to the lower end portion of the refined nitrogen tower 231 and the upper end portion of the nitrogen tower condenser-evaporator 233. The refined nitrogen tower 231 is communicated with the nitrogen tower condenser-evaporator 233 through the second diversion pipeline 2322. The first subcooler 21131 is installed on the second diversion pipeline 2322. The auxiliary unit 23 further includes a second valve group 234. The second valve group 234 includes an oxygen-rich liquid throttle valve 2341. The oxygen-rich liquid throttle valve 2341 is installed on the portion of the second diversion pipeline 2322 between the first subcooler 21131 and the nitrogen tower condenser-evaporator 233. The oxygen-rich liquid discharged from the lower end portion of the refined nitrogen tower 231 is introduced into the first subcooler 21131 through the second diversion pipeline 2322, cooled in the first subcooler 21131, and then flows through the oxygen-rich liquid throttle valve 2341 and is introduced into the nitrogen tower condenser-evaporator 233. The oxygen-rich liquid throttle valve 2341 is used to reduce the pressure of the cooled oxygen-rich liquid that exchanges heat in the first subcooler 21131 and is guided to the nitrogen tower condenser-evaporator 233. After the pressure reduction, the oxygen-rich liquid and nitrogen exchange heat in the nitrogen tower condenser-evaporator 233 to obtain oxygen-rich gas and liquid nitrogen.
[0086] The auxiliary pipeline 232 further includes a third diversion pipeline 2323. The two end portions of the third diversion pipeline 2323 are respectively connected to the lower end portion of the nitrogen tower condenser-evaporator 233 and the upper end portion of the refined nitrogen tower 231. The nitrogen tower condenser-evaporator 233 is communicated with the refined nitrogen tower 231 through the third diversion pipeline 2323. The liquid nitrogen obtained by the nitrogen in the nitrogen tower condenser-evaporator 233 through heat exchange flows to the refined nitrogen tower 231 through the third diversion pipeline 2323 to serve as the reflux liquid of the refined nitrogen tower 231 and make gas-liquid contact with the dried air that rises again and is cooled in the refined nitrogen tower 231 for heat and mass transfer, so that the rectification operation can be continuously carried out.
[0087] The conduction pipe group 212 further includes an oxygen-rich air pipeline 2126. The oxygen-rich air pipeline 2126 includes an oxygen-rich air main pipe 21261. One end portion of the oxygen-rich air main pipe 21261 is connected to the upper end portion of the nitrogen tower condenser-evaporator 233. The first subcooler 21131 is installed on the oxygen-rich air main pipe 21261. The oxygen-rich gas obtained by heat exchange in the nitrogen tower condenser-evaporator 233 is introduced into the first subcooler 21131 through the oxygen-rich air main pipe 21261 to serve as a cold source for heat exchange with the oxygen-rich liquid flowing through the first subcooler 21131.
[0088] The oxygen-enriched air pipeline 2126 also includes a liquid nitrogen pipe body 21262, and the subcooler group 2113 includes a second subcooler 21132. The second subcooler 21132 is installed on the supplementary pipeline 2234 and the liquid nitrogen pipe body 21262. One end of the liquid nitrogen pipe body 21262 is connected to the third guide pipe 2323. The liquid nitrogen portion discharged from the nitrogen tower condenser evaporator 233 to the third guide pipe 2323 flows through the liquid nitrogen pipe body 21262 and is introduced into the second subcooler 21132 to serve as a cold source and exchange heat with the external liquid argon flowing through the second subcooler 21132. At this time, there is no need to supplement an additional cold source, which is energy-saving and environmentally friendly.
[0089] Preferably, one end of the liquid nitrogen pipe body 21262 away from the third flow guide pipe 2323 is connected to the part of the oxygen-enriched air main pipe 21261 located between the first subcooler 21131 and the nitrogen tower condenser evaporator 233, so that the liquid nitrogen heated by heat exchange in the second subcooler 21132 flows into the oxygen-enriched air main pipe 21261 to mix with the oxygen-enriched gas discharged from the nitrogen tower condenser evaporator 233 to be guided to the first subcooler 21131 together, and the liquid nitrogen and the oxygen-enriched gas as a whole exchange heat with the oxygen-enriched liquid introduced into the first subcooler 21131 to obtain oxygen-enriched air.
[0090] It is worth mentioning that the air purification device 31 is connected to the other end of the oxygen-enriched air main pipe 21261. The oxygen-enriched air obtained by heat exchange in the first subcooler 21131 is introduced into the air purification device 31 through the part of the oxygen-enriched air main pipe 21261 located between the first subcooler 21131 and the air purification device 31, and is used as the regeneration gas of the air purification device 31, so as to realize the recycling of resources without the need to introduce additional regeneration gas, which is energy-saving and environmentally friendly.
[0091] The conducting pipe group 212 also includes a nitrogen pipeline 2127, and the first subcooler 21131 is installed on the nitrogen pipeline 2127. One end of the nitrogen pipeline 2127 is connected to the first guide pipeline 2321. The nitrogen part discharged from the refined nitrogen tower 231 to the first guide pipeline 2321 flows through the nitrogen pipeline 2127 and is introduced into the first subcooler 21131 to serve as a cold source and exchange heat with the oxygen-rich liquid introduced into the first subcooler 21131.
[0092] It is worth mentioning that the argon precooling purification system 13 is connected to the other end of the nitrogen pipeline 2127. The nitrogen that is heated by heat exchange in the first subcooler 21131 is introduced into the argon precooling purification system 13 through the part of the nitrogen pipeline 2127 located between the first subcooler 21131 and the argon precooling purification system 13 to serve as the regeneration gas of the argon precooling purification system 13, so as to realize the recycling of resources without the need to introduce additional regeneration gas, which is energy-saving and environmentally friendly.
[0093] Preferably, the main heat exchanger 2111 is installed at the portion of the oxygen-enriched air main pipe 21261 between the air purification device 31 and the first subcooler 21131, and the main heat exchanger 2111 is installed at the portion of the nitrogen pipeline 2127 between the argon precooling purification system 13 and the first subcooler 21131. The oxygen-enriched air and nitrogen heated by heat exchange in the first subcooler 21131 are guided to the main heat exchanger 2111 through the portions of the oxygen-enriched air main pipe 21261 and the nitrogen pipeline 2127 respectively located between the first subcooler 21131 and the main heat exchanger 2111. The oxygen-enriched air and nitrogen flowing into the main heat exchanger 2111 serve as cold sources for heat exchange with the dry air introduced into the main heat exchanger 2111 through the dry air pipe 2125, the dry crude argon introduced into the main heat exchanger 2111 through the feed pipe 2121, and the dry nitrogen introduced into the main heat exchanger 2111 through the first nitrogen conduit 21241.
[0094] The dry air duct 2125 includes a dry air inlet pipe 21251 and a dry air outlet pipe 21252. The two ends of the dry air inlet pipe 21251 are respectively connected to the air purification device 31 and the main heat exchanger 2111. The air purification device 31 is connected to the main heat exchanger 2111 through the dry air inlet pipe 21251. The dry air outlet pipe 21252 includes two branch pipes 212521 and a main pipe 212522. One end of the main pipe 212522 is connected to the main heat exchanger 2111, and the end of the main pipe 212522 away from the main heat exchanger 2111 is simultaneously connected to one end of the two branch pipes 212521. The cooled dry air obtained by heat exchange in the main heat exchanger 2111 flows to the two branch pipes 212521 through the main pipe 212522. The ends of the two branch pipes 212521 away from the main pipe 212522 are both connected to the nitrogen tower 231. The temperature control component 2112 includes an auxiliary heat exchanger 21121 and an expander 21122. The auxiliary heat exchanger 21121 and the expander 21122 are respectively installed on the two branch pipes 212521. The cooled and dried air flowing through the two branch pipes 212521 is respectively introduced into the auxiliary heat exchanger 21121 and the expander 21122 for further cooling. The auxiliary heat exchanger 21121 is installed on the oxygen-enriched air main pipe 21261 and the nitrogen pipe 2127 between the first subcooler 21131 and the main heat exchanger 2111. The oxygen-enriched air and nitrogen flowing through the oxygen-enriched air main pipe 21261 and the nitrogen pipe 2127, each located between the auxiliary heat exchanger 21121 and the first subcooler 21131, and introduced into the auxiliary heat exchanger 21121 serve as cold sources for heat exchange with the cooled dry air introduced into the auxiliary heat exchanger 21121 through the corresponding branch pipe 212521.
[0095] The second valve group 234 includes a dry air throttle valve 2342, which is installed in the branch pipe 212521 where the auxiliary heat exchanger 21121 is provided, and is located between the auxiliary heat exchanger 21121 and the nitrogen refining tower 231. The dry air throttle valve 2342 is used to reduce the pressure of the dry air that has been cooled again and is discharged from the auxiliary heat exchanger 21121 and directed to the nitrogen refining tower 231.
[0096] The second valve group 234 also includes a liquid nitrogen control valve 2343, which is installed on the liquid nitrogen pipe body 21262 and located on the side of the second subcooler 21132 away from the third drainage pipe 2233. The liquid nitrogen control valve 2343 is used to adjust the flow rate of the heated liquid nitrogen discharged from the second subcooler 21132 to match the flow rate of external liquid argon introduced into the second subcooler 21132, thereby ensuring that the external liquid argon can be cooled to a predetermined temperature range.
[0097] Preferably, the temperature of the cooled dry air discharged from the main heat exchanger 2111 is -163~-165°C, the temperature of the dried air cooled again after cooling by the auxiliary heat exchanger 21121 is -170~-174°C, the temperature of the dried air cooled again after depressurization by the dry air throttle valve 2342 is -176~-181°C, and the temperature of the cooled dry air discharged from the expander 21122 is -176~-181°C. The temperature of the nitrogen discharged from the refined nitrogen tower 231 is -184~-186°C, the temperature of the oxygen-rich liquid discharged from the refined nitrogen tower 231 is -180~-182°C, the temperature of the oxygen-rich liquid discharged from the first subcooler 21131 is -181~-183°C, and the temperature of the oxygen-rich liquid after depressurization by the oxygen-rich liquid throttle valve 2341 is -186~-189°C. The temperature of the liquid nitrogen discharged from the nitrogen tower condenser evaporator 233 is -184~-186°C, and the temperature of the oxygen-enriched air discharged from the nitrogen tower condenser evaporator 233 and the liquid nitrogen discharged from the second subcooler 21132 are both -184~-186°C. The temperature of the external liquid argon introduced into the second subcooler 21132 is -155~-160°C, and the temperature of the external liquid argon after heat exchange in the second subcooler 21132 is -182~-184°C. The temperature of the oxygen-enriched air and nitrogen discharged from the first subcooler 21131 is both -175~-178°C, the temperature of the oxygen-enriched air and nitrogen discharged from the auxiliary heat exchanger 21121 is both -165~-168°C, and the temperature of the oxygen-enriched air and nitrogen discharged from the main heat exchanger 2111 is both 10~20°C.
[0098] A working method of an argon recovery device capable of stable distillation is now proposed, comprising the following steps:
[0099] The dry crude argon gas is introduced into the main heat exchanger 2111 through the feed pipe 2121 to exchange heat in the main heat exchanger 2111 to obtain the dried crude argon gas after cooling. The dried crude argon gas after cooling is introduced into the refined argon tower 221 to be liquefied in the argon tower reboiler 222 in the refined argon tower 221 to obtain the crude liquid argon. The crude liquid argon enters the first draft pipe 2231 from the argon tower reboiler 222 and flows through the crude liquid argon throttle valve 2241 to be introduced into the crude liquid argon tower 221 after the pressure is reduced by the crude liquid argon throttle valve 2241. The refined argon tower 221, after the depressurized crude liquid argon is introduced into the refined argon tower 221, it is rectified to obtain pure liquid argon placed at the bottom of the tower and argon-nitrogen mixed gas rising to the top of the tower, wherein the pure liquid argon is used as a cold source to liquefy the cooled and dried crude argon gas in the argon tower reboiler 222, and the pure liquid argon exchanges heat with the cooled and dried crude argon gas to be partially vaporized to serve as a part of the argon-nitrogen mixed gas, and the argon-nitrogen mixed gas rising in the refined argon tower 221 is in gas-liquid contact with the depressurized crude liquid argon flowing downward in the refined argon tower 221 to transfer mass and heat;
[0100] The temperature detecting element 2262 detects the temperature of the cooled and dried crude argon gas which flows through the portion of the feed pipe 2121 between the main heat exchanger 2111 and the argon column reboiler 222 and is directed to the argon column reboiler 222. The operating speed of the nitrogen compressor 22611 is adjusted according to the detected temperature of the cooled and dried crude argon gas to regulate the flow rate of the dry nitrogen gas directed to the main heat exchanger 2111. The nitrogen compressor 22611 introduces dry nitrogen into the main heat exchanger 2111 through the first nitrogen conducting pipe 21241 to exchange heat in the main heat exchanger 2111 to obtain cooled and dried nitrogen. Dry nitrogen is introduced into the nitrogen reboiler 22612 through the portion of the first nitrogen conducting pipe 21241 located between the nitrogen reboiler 22612 and the main heat exchanger 2111, and part of the pure liquid argon in the refined argon tower 221 is introduced into the nitrogen reboiler 22612 through the pure liquid argon connecting pipe 2236. Pure liquid argon and the cooled and dried nitrogen are heat exchanged in the nitrogen reboiler 22612 to obtain pure argon and liquid nitrogen. Pure argon is introduced into the refined argon tower 221 through the pure argon connecting pipe 2237, and cooperates with the pure argon obtained by gasification through heat exchange with the cooled and dried crude argon in the argon tower reboiler 222, so that the distillation process can be carried out stably.
[0101] The working method of the argon recovery equipment capable of stable distillation further comprises the following steps:
[0102] Part of the pure liquid argon in the refined argon tower 221 passes through the second drainage pipe 2232 and flows through the pure liquid argon throttle valve 2242 to be introduced into the argon tower condenser evaporator 225 after being reduced in pressure by the pure liquid argon throttle valve 2242, and the argon-nitrogen mixed gas in the refined argon tower 221 is introduced into the argon tower condenser evaporator 225 through the third drainage pipe 2233, and external liquid argon is provided to the argon tower condenser evaporator 225 through the supplementary pipe 2234. At this time, the pure liquid argon and the external liquid argon are heat-exchanged with the argon-nitrogen mixed gas as a whole to obtain pure argon gas, argon-nitrogen mixed liquid and dirty argon gas. The pure argon gas passes through the pure argon gas pipeline 2122 and flows through the main heat exchanger 2111 to be discharged, and the dirty argon gas passes through the dirty argon gas main pipe 21231 and flows through the main heat exchanger 2111 to be discharged. The pure argon gas and the dirty argon gas serve as cold sources for heat exchange in the main heat exchanger 2111.
[0103] The working method of the argon recovery equipment capable of stable distillation further comprises the following steps:
[0104] After being compressed and deoiled and dusted, the crude argon gas passes through the first phase connecting pipe 1121 and flows through the heating group 1111 to be heated by the heating group 1111 and then introduced into the catalytic reactor group 12. The catalytic reactor group 12 removes carbon monoxide and oxygen in the heated crude argon gas to obtain a crude argon gas containing carbon dioxide. Subsequently, the crude argon gas containing carbon dioxide flows into the second phase connecting pipe 1122 and is cooled by the water cooler 1112 and then introduced into the argon precooling purification system 13. The argon precooling purification system 13 removes water and carbon dioxide from the crude argon gas containing carbon dioxide to obtain dry crude argon gas.
[0105] The working method of the argon recovery equipment capable of stable distillation further comprises the following steps:
[0106] The liquid nitrogen obtained by heat exchange in the nitrogen reboiler 22612 enters the liquid nitrogen connecting pipe 2238 and flows through the liquid nitrogen throttle valve 2244 to be introduced into the nitrogen condenser evaporator 22613 after being reduced in pressure by the liquid nitrogen throttle valve 2244. The dirty argon gas part in the dirty argon gas main pipe 21231 is introduced into the nitrogen condenser evaporator 22613 through the dirty argon gas branch pipe 21232. The dirty argon gas and liquid nitrogen exchange heat in the nitrogen condenser evaporator 22613 to obtain nitrogen and dirty liquid argon. The nitrogen obtained by heat exchange in the nitrogen condenser evaporator 22613 passes through the second nitrogen conducting pipe 21242 and flows through the main heat exchanger 2111 to serve as a cold source for heat exchange in the main heat exchanger 2111 and is guided to the nitrogen compressor 22611 after being heated.
[0107] The working method of the argon recovery equipment capable of stable distillation further comprises the following steps:
[0108] The argon-nitrogen mixed liquid in the argon tower condenser evaporator 225 is introduced into the argon refinement tower 221 through the reflux pipe 2235. While flowing downward in the argon refinement tower 221, the argon-nitrogen mixed liquid transfers heat and mass with the argon-nitrogen mixed gas rising in the argon refinement tower 221 to recover argon as much as possible.
[0109] The working method of the argon recovery equipment capable of stable distillation further comprises the following steps:
[0110] The dirty liquid argon obtained by heat exchange in the nitrogen condensation evaporator 22613 is introduced into the refined argon tower 221 through the dirty liquid argon connecting pipe 2239. The dirty liquid argon flows downward in the refined argon tower 221 and transfers heat and mass with the argon-nitrogen mixed gas rising in the refined argon tower 221 to recover argon as much as possible.
[0111] The working method of the argon recovery equipment capable of stable distillation also includes the following steps: the oxygen supply pipeline 112112 is used to introduce air or oxygen into the feed pipeline 112111 to keep the ratio of carbon monoxide to oxygen at 2:1.
[0112] The working method of the argon recovery equipment capable of stable distillation further comprises the following steps:
[0113] The catalytic reactor group 12 supplies crude argon containing carbon dioxide to the regenerator 11111 through the heat recovery pipe 11221 as a heat source for heating the crude argon introduced into the regenerator 11111. Subsequently, the crude argon containing carbon dioxide discharged from the regenerator 11111 flows into the water cooler 1112 through the second discharge pipe 11222 and is introduced into the argon pre-cooling purification system 13 after being cooled by the water cooler 1112.
[0114] The working method of the argon recovery equipment capable of stable distillation further comprises the following steps:
[0115] The compressed air is introduced into the air purification device 31 so that the air purification device 31 adsorbs carbon dioxide and water to obtain dry air. The dry air discharged from the air purification device 31 is introduced into the main heat exchanger 2111 through the dry air pipeline 2125 to mix with the pure argon gas introduced into the main heat exchanger 2111 through the pure argon gas pipeline 2122, the dirty argon gas introduced into the main heat exchanger 2111 through the dirty argon gas main pipeline 21231, and the second nitrogen gas pipeline 2124. The nitrogen introduced into the main heat exchanger 2111 through the pipe 21242 is cooled by heat exchange, and the cooled dry air discharged from the main heat exchanger 2111 flows to the temperature regulating component 2112 through the dry air pipeline 2125 located between the main heat exchanger 2111 and the nitrogen refining tower 231, and is cooled again by the temperature regulating component 2112 and then guided to the nitrogen refining tower 231. The cooled dry air is rectified in the nitrogen refining tower 231 to obtain oxygen-rich liquid and nitrogen.
[0116] The nitrogen rising in the nitrogen tower 231 is introduced into the nitrogen tower condenser evaporator 233 through the first guide pipe 2321, and the oxygen-rich liquid discharged from the lower end of the nitrogen tower 231 is introduced into the first subcooler 21131 through the second guide pipe 2322, and after being cooled in the first subcooler 21131, it flows through the oxygen-rich liquid throttle valve 2341, and is introduced into the nitrogen tower condenser evaporator 233 after being reduced in pressure by the oxygen-rich liquid throttle valve 2341. The nitrogen and the oxygen-rich liquid exchange heat in the nitrogen tower condenser evaporator 233 to obtain liquid nitrogen and oxygen-rich oxygen. The liquid nitrogen flows to the nitrogen tower 231 through the third guide pipe 2323, and while the liquid nitrogen flows downward in the nitrogen tower 231, it is heated by the dry air rising in the nitrogen tower 231 and cooled again. Heat and mass transfer are performed to enable the distillation operation to proceed continuously. The oxygen-rich oxygen is introduced into the first subcooler 21131 through the oxygen-rich air main pipe 21261 to serve as a cold source for the oxygen-rich liquid flowing through the first subcooler 21131. The liquid nitrogen portion discharged from the nitrogen tower condenser evaporator 233 to the third flow guide pipe 2323 flows through the liquid nitrogen pipe body 21262 and is introduced into the second subcooler 21132 as a cold source. The external liquid argon flowing through the second subcooler 21132 and guided to the argon tower condenser evaporator 225 through the supplementary pipe 2234 exchanges heat with the liquid nitrogen introduced into the second subcooler 21132 and is cooled. In this way, the argon tower condenser evaporator 225 is provided with external liquid argon that is kept subcooled, so as to provide sufficient cooling capacity while reducing liquid argon waste.
[0117] The working method of the argon recovery equipment capable of stable distillation further comprises the following steps:
[0118] The liquid nitrogen heated by heat exchange in the second subcooler 21132 flows into the oxygen-enriched air main pipe 21261 to be mixed with the oxygen-enriched gas discharged from the nitrogen tower condenser evaporator 233 to be jointly guided to the first subcooler 21131. The liquid nitrogen and oxygen-enriched gas as a whole exchange heat with the oxygen-enriched liquid introduced into the first subcooler 21131 to obtain oxygen-enriched air.
[0119] The working method of the argon recovery equipment capable of stable distillation further comprises the following steps:
[0120] The oxygen-enriched air obtained by heat exchange in the first subcooler 21131 is introduced into the air purification device 31 through the portion of the oxygen-enriched air main pipe 21261 located between the first subcooler 21131 and the air purification device 31 to serve as the regeneration gas of the air purification device 31 .
[0121] The working method of the argon recovery equipment capable of stable distillation further comprises the following steps:
[0122] The nitrogen gas discharged from the nitrogen tower 231 to the first flow conduit 2321 partially flows through the nitrogen conduit 2127 and is introduced into the first subcooler 21131 to serve as a cold source and exchange heat with the oxygen-rich liquid introduced into the first subcooler 21131 .
[0123] The working method of the argon recovery equipment capable of stable distillation further comprises the following steps:
[0124] The nitrogen gas heated by heat exchange in the first subcooler 21131 is introduced into the argon precooling purification system 13 through the nitrogen pipeline 2127 located between the first subcooler 21131 and the argon precooling purification system 13 to serve as the regeneration gas of the argon precooling purification system 13.
[0125] It should be understood by those skilled in the art that the embodiments of the present application described above and shown in the accompanying drawings are only examples and do not limit the present application. The advantages of the present application have been fully and effectively realized. The functions and structural principles of the present application have been demonstrated and explained in the embodiments, and the embodiments of the present application may be deformed or modified in any way without departing from the principles.
Claims
1. Argon recovery equipment capable of stable distillation, characterized in that: The argon recovery equipment capable of stable distillation comprises a distillation system, and the distillation system comprises: A temperature regulating mechanism, the temperature regulating mechanism comprises a temperature regulating component and a conducting pipe group, the temperature regulating component comprises a main heat exchanger, the conducting pipe group comprises a feed pipe and a nitrogen pipe group, the main heat exchanger is installed on the feed pipe, the dry crude argon gas is introduced into the main heat exchanger through the feed pipe and discharged after being cooled in the main heat exchanger, and the nitrogen pipe group comprises a first nitrogen conducting pipe; An argon extraction unit, the argon extraction unit comprising: Argon tower; An argon column reboiler, the argon column reboiler is installed in the refined argon column and is located at the bottom of the column. The argon column reboiler is connected to one end of the feed pipe. The cooled and dried crude argon gas obtained by heat exchange in the main heat exchanger is introduced into the argon column reboiler through the portion of the feed pipe located between the main heat exchanger and the argon column reboiler. The cooled and dried crude argon gas is liquefied in the argon column reboiler to obtain crude liquid argon. A refined argon pipe group, the refined argon pipe group comprising a first draft pipe, a pure liquid argon connecting pipe and a pure argon gas connecting pipe, wherein two ends of the first draft pipe are respectively connected to the lower end of the argon tower reboiler and the upper end of the refined argon tower; a first valve group, wherein the first valve group comprises a crude liquid argon throttle valve, wherein the crude liquid argon throttle valve is installed on the first draft pipe, wherein the crude liquid argon enters the first draft pipe from the argon column reboiler and flows through the crude liquid argon throttle valve to be introduced into the refined argon column after being depressurized by the crude liquid argon throttle valve, wherein the depressurized crude liquid argon is introduced into the refined argon column and then rectified to obtain pure liquid argon at the bottom of the column and argon-nitrogen mixed gas rising to the top of the column, wherein the pure liquid argon is used as a cold source to liquefy the cooled and dried crude argon gas in the argon column reboiler, and is heat-exchanged with the cooled and dried crude argon gas to be partially vaporized to be a part of the argon-nitrogen mixed gas; A stabilization component, the stabilization component comprising: A nitrogen compressor, wherein one end of the first nitrogen conduit is connected to the nitrogen compressor, the main heat exchanger is installed on the first nitrogen conduit, the nitrogen compressor introduces dry nitrogen into the first nitrogen conduit, the dry nitrogen is introduced into the main heat exchanger through the first nitrogen conduit to exchange heat in the main heat exchanger and cool down, and the nitrogen compressor can operate at a variable speed to adjust the flow rate of the dry nitrogen introduced into the main heat exchanger; A nitrogen reboiler is installed at the other end of the first nitrogen conduit. The cooled and dried nitrogen obtained by heat exchange in the main heat exchanger is introduced into the nitrogen reboiler through the portion of the first nitrogen conduit located between the nitrogen reboiler and the main heat exchanger. Both ends of the pure liquid argon connecting pipe are respectively connected to the nitrogen reboiler and the lower end of the argon refinement tower. Part of the pure liquid argon in the argon refinement tower is introduced into the nitrogen reboiler through the pure liquid argon connecting pipe. The pure liquid argon and the cooled and dried nitrogen are introduced into the nitrogen reboiler. The dry nitrogen is heat exchanged in the nitrogen reboiler to obtain pure argon and liquid nitrogen. The two ends of the pure argon connecting pipe are respectively connected to the lower end of the refined argon tower and the higher end of the nitrogen reboiler. The refined argon tower is connected to the nitrogen reboiler through the pure argon connecting pipe. The pure argon obtained by heat exchange in the nitrogen reboiler is introduced into the refined argon tower through the pure argon connecting pipe, and cooperates with the pure argon gas obtained by heat exchange and gasification of the dried crude argon gas after cooling in the argon tower reboiler, so as to rectify the crude liquid argon after pressure reduction. a temperature detecting member, the temperature detecting member being installed at a portion of the feed pipe between the main heat exchanger and the argon column reboiler, the temperature detecting member being used to detect the temperature of the cooled dry crude argon gas flowing through the portion of the feed pipe between the main heat exchanger and the argon column reboiler and directed to the argon column reboiler, and when the temperature detecting member detects that the temperature of the cooled dry crude argon gas remains outside a predetermined temperature range, the nitrogen compressor adjusts the flow rate of the dry nitrogen gas directed to the main heat exchanger; The argon extraction unit also includes an argon tower condenser evaporator, which is installed on the top of the refined argon tower. The refined argon pipe group includes a second drainage pipe. The first valve group includes a pure liquid argon throttle valve. The two ends of the second drainage pipe are respectively connected to the lower end of the refined argon tower and the high end of the argon tower condenser evaporator. The pure liquid argon throttle valve is installed on the second drainage pipe. Part of the pure liquid argon in the refined argon tower passes through the second drainage pipe and the pure liquid argon throttle valve to be introduced into the argon tower condenser evaporator after being reduced in pressure by the pure liquid argon throttle valve. The refined argon pipe group includes a third A drainage pipe, wherein both ends of the third drainage pipe are respectively connected to the high end of the refined argon tower and the high end of the argon tower condenser evaporator, the refined argon tower is in communication with the argon tower condenser evaporator through the third drainage pipe, so that the refined argon tower supplies argon-nitrogen mixed gas to the argon tower condenser evaporator from the refined argon tower, the refined argon pipe group further comprises a supplementary pipe, one end of the supplementary pipe is connected to the argon tower condenser evaporator to provide external liquid argon to the argon tower condenser evaporator, and the pure liquid argon and the external liquid argon are integrally heat-exchanged with the argon-nitrogen mixed gas introduced through the third drainage pipe to obtain pure argon, argon-nitrogen mixed liquid and dirty argon; The argon recovery equipment capable of stable distillation includes an air pretreatment system, the air pretreatment system includes an air purification device, air is compressed and then introduced into the air purification device so that the air purification device adsorbs carbon dioxide and water to obtain dry air, the conductive pipe group also includes a dry air pipeline, the air purification device is installed at one end of the dry air pipeline, the main heat exchanger is installed on the dry air pipeline, the dry air discharged from the air purification device is introduced into the main heat exchanger through the dry air pipeline for heat exchange and cooling, the distillation system also includes an auxiliary unit, the auxiliary unit includes a nitrogen tower, the nitrogen tower is connected to the other end of the dry air pipeline, the temperature control component includes a temperature control component, the temperature control The component is installed in the part of the dry air pipeline located between the main heat exchanger and the nitrogen tower. The cooled dry air discharged from the main heat exchanger flows to the temperature regulating component through the dry air pipeline to be cooled again by the temperature regulating component and then guided to the nitrogen tower. The cooled dry air is distilled in the nitrogen tower to obtain oxygen-rich liquid and nitrogen. The auxiliary unit includes an auxiliary pipeline and a nitrogen tower condenser evaporator. The auxiliary pipeline includes a first guide pipeline. The two ends of the first guide pipeline are respectively connected to the high end of the nitrogen tower and the high end of the nitrogen tower condenser evaporator. The nitrogen tower is connected to the nitrogen tower condenser evaporator through the first guide pipeline. The nitrogen rising in the nitrogen tower is introduced into the nitrogen tower through the first guide pipeline. The temperature regulating component comprises a subcooler group, the subcooler group comprises a first subcooler, the auxiliary pipeline comprises a second guide pipeline, the two ends of the second guide pipeline are respectively connected to the lower end of the refined nitrogen tower and the high end of the nitrogen tower condenser evaporator, the refined nitrogen tower is connected to the nitrogen tower condenser evaporator through the second guide pipeline, the first subcooler is installed on the second guide pipeline, the auxiliary unit also comprises a second valve group, the second valve group comprises an oxygen-rich liquid throttle valve, the oxygen-rich liquid throttle valve is installed in the second guide pipeline between the first subcooler and the nitrogen tower condenser evaporator, the oxygen-rich liquid discharged from the lower end of the refined nitrogen tower is introduced into the first subcooler through the second guide pipeline and After cooling in the first subcooler, the liquid flows through the oxygen-rich liquid throttle valve and is introduced into the nitrogen tower condenser evaporator. The oxygen-rich liquid throttle valve is used to reduce the pressure of the cooled oxygen-rich liquid that is heat-exchanged in the first subcooler and directed to the nitrogen tower condenser evaporator. After the pressure reduction, the oxygen-rich liquid and nitrogen exchange heat in the nitrogen tower condenser evaporator to obtain oxygen-rich gas and liquid nitrogen. The auxiliary pipeline also includes a third guide pipeline, one end of which is connected to the lower end of the nitrogen tower condenser evaporator. The conducting pipe group also includes an oxygen-rich air pipeline, which includes a liquid nitrogen pipe body. The subcooler group includes a second subcooler, which is installed on the supplementary pipeline and the liquid nitrogen pipe body, and one end of the liquid nitrogen pipe body is connected to the third guide pipeline.The liquid nitrogen discharged from the nitrogen tower condenser evaporator to the third flow guide pipe flows through the liquid nitrogen pipe body and is introduced into the second subcooler to serve as a cold source and exchange heat with the external liquid argon flowing through the second subcooler.
2. The argon recovery equipment capable of stable distillation according to claim 1, characterized in that: The conducting pipe group includes a pure argon gas pipeline and a dirty argon gas pipeline, and the dirty argon gas pipeline includes a dirty argon gas main pipe. One end of the pure argon gas pipeline and one end of the dirty argon gas main pipe are both connected to the argon tower condenser evaporator. The pure argon gas obtained by heat exchange in the argon tower condenser evaporator is discharged through the pure argon gas pipeline, and the dirty argon gas obtained by heat exchange in the argon tower condenser evaporator is discharged through the dirty argon gas main pipe. The main heat exchanger is installed on the pure argon gas pipeline and the dirty argon gas main pipe. The pure argon gas flowing through the pure argon gas pipeline to be introduced into the main heat exchanger and the dirty argon gas flowing through the dirty argon gas main pipe to be introduced into the main heat exchanger are used as cold sources to exchange heat with the dry crude argon gas flowing through the feed pipe to be introduced into the main heat exchanger.
3. The argon recovery equipment capable of stable distillation according to claim 2, characterized in that: The refined argon pipe group also includes a reflux pipe, the two ends of which are respectively connected to the lower end of the argon tower condenser evaporator and the upper end of the refined argon tower. The argon tower condenser evaporator is connected to the refined argon tower through the reflux pipe, so that the argon tower condenser evaporator supplies argon-nitrogen mixed liquid to the refined argon tower.
4. The argon recovery equipment capable of stable distillation according to claim 3, characterized in that: The argon recovery equipment capable of stable distillation includes a raw material pre-impurity removal system, the raw material pre-impurity removal system includes a heat transfer component, the heat transfer component includes a heat transfer assembly and a phase connection group, the heat transfer assembly includes a heating group, the phase connection group includes a first phase connection, the heating group is installed on the first phase connection, the crude argon gas is introduced into the heating group through the first phase connection after being compressed and deoiled and dusted, the heating group is used to heat the crude argon gas, the raw material pre-impurity removal system includes a catalytic reactor group, the catalytic reactor group is connected to one end of the first phase connection, the heated crude argon gas obtained by heating the heating group is introduced into the catalytic reactor group through the first phase connection, the catalytic reactor group is used to remove carbon monoxide and oxygen in the heated crude argon gas to obtain crude argon gas containing carbon dioxide, the raw material pre-impurity removal system includes an argon precooling The phase pipe group also includes a second phase pipe, and the two ends of the second phase pipe are respectively connected to the catalytic reactor group and the argon precooling purification system, and the catalytic reactor group is connected to the argon precooling purification system through the second phase pipe. The heat transfer component also includes a water cooler, which is installed on the second phase pipe. The crude argon gas containing carbon dioxide obtained by the catalytic reactor group flows through the water cooler and is cooled in the water cooler before being guided to the argon precooling purification system. The argon precooling purification system is used to remove water and carbon dioxide from the crude argon gas containing carbon dioxide to obtain dry crude argon gas. The argon precooling purification system is connected to the other end of the feed pipe, and the dry crude argon gas obtained by the argon precooling purification system is introduced into the main heat exchanger through the feed pipe.
5. The argon recovery equipment capable of stable distillation according to claim 4, characterized in that: The first phase pipe includes an inlet pipe and a first discharge pipe, the heating group includes a regenerator and an electric heater, the regenerator is connected to one end of the inlet pipe so as to introduce crude argon gas from the inlet pipe to the regenerator, the regenerator is used to preliminarily heat the introduced crude argon gas, the electric heater is connected to the regenerator through a pipeline so as to introduce the preliminarily heated crude argon gas from the regenerator to the electric heater, the electric heater is used to perform secondary heating on the preliminarily heated crude argon gas, the two ends of the first discharge pipe are respectively connected to the electric heater and the catalytic reactor group, the electric heater is connected to the catalytic reactor group through the first discharge pipe so as to introduce the heated crude argon gas from the electric heater to the catalytic reactor group, the inlet pipe includes a feed pipe and an oxygen supply pipe, one end of the feed pipe is connected to the regenerator, the crude argon gas is introduced into the regenerator through the feed pipe, the feed pipe is radially connected with the oxygen supply pipe, the oxygen supply pipe is used to introduce air or oxygen into the feed pipe.
6. The argon recovery equipment capable of stable distillation according to claim 5, characterized in that: The second phase connecting pipe includes a heat recovery pipe and a second discharge pipe, the two ends of the heat recovery pipe are respectively connected to the catalytic reactor group and the regenerator, the catalytic reactor group is connected with the regenerator through the heat recovery pipe to introduce crude argon containing carbon dioxide into the regenerator, so as to serve as a heat source for heating the crude argon introduced into the regenerator, the two ends of the second discharge pipe are respectively connected to the regenerator and the argon precooling purification system, the regenerator is connected with the argon precooling purification system through the second discharge pipe, the water cooler is installed on the second discharge pipe, the crude argon containing carbon dioxide discharged from the regenerator flows into the water cooler through the second discharge pipe and is introduced into the argon precooling purification system after being cooled by the water cooler.
7. The argon recovery equipment capable of stable distillation according to claim 4, characterized in that: The refined argon pipe group also includes a liquid nitrogen connecting pipe, the stabilization assembly also includes a nitrogen condenser evaporator, the two ends of the liquid nitrogen connecting pipe are respectively connected to the high end of the nitrogen condenser evaporator and the low end of the nitrogen reboiler, the nitrogen reboiler is connected to the nitrogen condenser evaporator through the liquid nitrogen connecting pipe, the first valve group also includes a liquid nitrogen throttle valve, the liquid nitrogen throttle valve is installed on the liquid nitrogen connecting pipe, the liquid nitrogen obtained by heat exchange in the nitrogen reboiler enters the liquid nitrogen connecting pipe and flows through the liquid nitrogen throttle valve to be introduced into the nitrogen condenser evaporator after being reduced in pressure by the liquid nitrogen throttle valve, the dirty argon gas pipeline also includes a dirty argon gas branch pipe, one end of the dirty argon gas branch pipe is connected to the part of the dirty argon gas main pipe located between the main heat exchanger and the argon tower condenser evaporator, and the dirty argon gas part introduced from the argon tower condenser evaporator into the dirty argon gas main pipe passes through The dirty argon gas branch pipe is introduced into the nitrogen condensing evaporator, and the dirty argon gas and liquid nitrogen exchange heat in the nitrogen condensing evaporator to obtain nitrogen and dirty liquid argon. The nitrogen pipe group also includes a second nitrogen conducting pipe, and the two ends of the second nitrogen conducting pipe are respectively connected to the high end of the nitrogen condensing evaporator and the nitrogen compressor, and the main heat exchanger is installed on the second nitrogen conducting pipe. The nitrogen obtained by heat exchange in the nitrogen condensing evaporator is introduced into the main heat exchanger through the second nitrogen conducting pipe to heat exchange with the dry crude argon gas introduced into the main heat exchanger by the argon precooling purification system and the dry nitrogen introduced into the main heat exchanger by the nitrogen compressor to increase the temperature. The heated nitrogen obtained by heat exchange in the main heat exchanger is introduced into the nitrogen compressor through the part of the second nitrogen conducting pipe located between the main heat exchanger and the nitrogen compressor.
8. The argon recovery equipment capable of stable distillation according to claim 7, characterized in that: The refined argon pipe group also includes a dirty liquid argon connecting pipe, the two ends of which are respectively connected to the lower end of the nitrogen condensing evaporator and the upper end of the refined argon tower. The nitrogen condensing evaporator is connected to the refined argon tower through the dirty liquid argon connecting pipe, and the dirty liquid argon obtained by heat exchange in the nitrogen condensing evaporator is introduced into the refined argon tower through the dirty liquid argon connecting pipe.
9. The working method of the argon recovery equipment capable of stable distillation according to any one of claims 1 to 8, characterized in that: The working method of the argon recovery device capable of stable distillation comprises the following steps: The dry crude argon gas is introduced into the main heat exchanger through the feed pipe to exchange heat in the main heat exchanger to obtain the dried crude argon gas after cooling. The dried crude argon gas after cooling is introduced into the argon refinement column to be liquefied in the argon column reboiler in the argon refinement column to obtain crude liquid argon. The crude liquid argon enters the first draft pipe from the argon column reboiler and flows through the crude liquid argon throttle valve to be introduced into the argon refinement column after the pressure is reduced by the crude liquid argon throttle valve. The crude liquid argon after the pressure reduction is introduced into the argon refinement column and then rectified to obtain pure liquid argon placed at the bottom of the column and argon-nitrogen mixed gas rising to the top of the column, wherein the pure liquid argon serves as a cold source to liquefy the dried crude argon gas after cooling in the argon column reboiler. The pure liquid argon exchanges heat with the dried crude argon gas after cooling to be partially vaporized to serve as a part of the argon-nitrogen mixed gas. The argon-nitrogen mixed gas rising in the argon refinement column is in gas-liquid contact with the crude liquid argon gas after pressure reduction flowing downward in the argon refinement column to transfer mass and heat; The temperature detecting element detects the temperature of the cooled and dried crude argon gas flowing through the portion of the feed pipe between the main heat exchanger and the argon column reboiler and directed to the argon column reboiler. The running speed of the nitrogen compressor is adjusted according to the detected temperature of the cooled and dried crude argon gas to regulate the flow rate of the dry nitrogen gas directed to the main heat exchanger. The nitrogen compressor introduces dry nitrogen into the main heat exchanger through the first nitrogen conduit to exchange heat in the main heat exchanger to obtain cooled and dried nitrogen. The cooled and dried nitrogen gas is introduced into the nitrogen reboiler through the portion of the first nitrogen conduit between the nitrogen reboiler and the main heat exchanger. Part of the pure liquid argon in the refined argon column is introduced into the nitrogen reboiler through the pure liquid argon connecting pipe. The pure liquid argon and the cooled and dried nitrogen gas exchange heat in the nitrogen reboiler to obtain pure argon and liquid nitrogen. The pure argon gas is introduced into the refined argon column through the pure argon connecting pipe to cooperate with the pure argon gas obtained by gasification through heat exchange with the cooled and dried crude argon gas in the argon column reboiler. Part of the pure liquid argon in the refined argon tower passes through the second drainage pipe and flows through the pure liquid argon throttle valve to be introduced into the argon tower condenser evaporator after being depressurized by the pure liquid argon throttle valve, and the argon-nitrogen mixed gas in the refined argon tower is introduced into the argon tower condenser evaporator through the third drainage pipe, and external liquid argon is provided to the argon tower condenser evaporator through the supplementary pipeline. At this time, the pure liquid argon and the external liquid argon are heat-exchanged with the argon-nitrogen mixed gas as a whole to obtain pure argon gas, argon-nitrogen mixed liquid and dirty argon gas; The compressed air is passed into the air purification device so that the air purification device adsorbs carbon dioxide and water to obtain dry air. The dry air discharged from the air purification device is introduced into the main heat exchanger through the dry air pipeline for heat exchange and cooling. The cooled dry air discharged from the main heat exchanger flows to the temperature adjustment component through the part of the dry air pipeline located between the main heat exchanger and the nitrogen refiner to be cooled again by the temperature adjustment component and then guided to the nitrogen refiner. After cooling again, the dry air is distilled in the nitrogen refiner to obtain oxygen-rich liquid and nitrogen. The nitrogen rising in the nitrogen refiner is introduced into the nitrogen tower condenser evaporator through the first guide pipeline, and the nitrogen tower is discharged from the lower end of the nitrogen refiner. The oxygen-rich liquid discharged from the nitrogen tower condenser evaporator is introduced into the first supercooler through the second guide pipe, and after being cooled in the first supercooler, it flows through the oxygen-rich liquid throttle valve to be reduced in pressure by the oxygen-rich liquid throttle valve and then introduced into the nitrogen tower condenser evaporator. Nitrogen and oxygen-rich liquid exchange heat in the nitrogen tower condenser evaporator to obtain liquid nitrogen and oxygen-rich oxygen. The liquid nitrogen part discharged from the nitrogen tower condenser evaporator to the third guide pipe flows through the liquid nitrogen pipe body and is introduced into the second supercooler as a cold source. The external liquid argon that flows through the second supercooler and is guided to the argon tower condenser evaporator through the supplementary pipe exchanges heat with the liquid nitrogen introduced into the second supercooler to be cooled, thereby providing the argon tower condenser evaporator with external liquid argon that is kept subcooled.
Citation Information
Patent Citations
Single-tower low-temperature rectification argon recycling system with cycle and single-tower low-temperature rectification argon recycling method
CN111637684A