CN211198612U - Argon recovery device for removing carbon monoxide and integrating high-purity nitrogen by rectification method - Google Patents

Argon recovery device for removing carbon monoxide and integrating high-purity nitrogen by rectification method Download PDF

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CN211198612U
CN211198612U CN201922201252.1U CN201922201252U CN211198612U CN 211198612 U CN211198612 U CN 211198612U CN 201922201252 U CN201922201252 U CN 201922201252U CN 211198612 U CN211198612 U CN 211198612U
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argon
tower
nitrogen
rectification
pipeline
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郝文炳
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Shanghai Lianfeng Energy Technology Co ltd
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Shanghai Lianfeng Energy Technology Co ltd
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/044—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a single pressure main column system only
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04563—Integration with a nitrogen consuming unit, e.g. for purging, inerting, cooling or heating
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04612—Heat exchange integration with process streams, e.g. from the air gas consuming unit
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/02—Processes or apparatus using separation by rectification in a single pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/40—Processes or apparatus using other separation and/or other processing means using hybrid system, i.e. combining cryogenic and non-cryogenic separation techniques
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • F25J2205/66—Regenerating the adsorption vessel, e.g. kind of reactivation gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/82—Processes or apparatus using other separation and/or other processing means using a reactor with combustion or catalytic reaction
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/58—Argon
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/58—Argon
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/02—Internal refrigeration with liquid vaporising loop
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/58—Quasi-closed internal or closed external argon refrigeration cycle
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • F25J2270/904—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

The utility model relates to a carbon monoxide is got rid of to rectification method and argon gas recovery unit of integrated high-purity nitrogen, including argon compressor, carbon monoxide reacting furnace, argon gas precooling purification system, air compressor, air precooling purification system, heat exchanger, smart argon tower, the first reboiler in argon tower, argon tower second reboiler, argon tower condensation evaporimeter, nitrogen tower and nitrogen tower condensation evaporimeter. The utility model utilizes the integrated air nitrogen flow path, and can reduce the limit of regenerated gas by self-producing nitrogen in the cold box and improve the extraction rate of recovered argon gas by utilizing the rich cold quantity of liquid argon; and partial liquid nitrogen is produced by utilizing the cold energy of the abundant liquid argon, so that the economic benefit is improved.

Description

Argon recovery device for removing carbon monoxide and integrating high-purity nitrogen by rectification method
Technical Field
The utility model relates to an argon gas recovery unit especially relates to an argon gas recovery unit that carbon monoxide and integrated high-purity nitrogen were got rid of to rectification method.
Background
Czochralski method (Czochralski method) is the main method for producing single crystal silicon, and 70% to 80% of silicon single crystal worldwide is produced by the Czochralski method. The most common Czochralski process for producing single crystal silicon employs a reduced pressure crystal pulling process that is both a vacuum process and a flowing atmosphere process; the decompression process is characterized in that high-purity argon is continuously introduced into a hearth of a single crystal furnace at a constant speed in the silicon single crystal drawing process, and meanwhile, a vacuum pump continuously pumps the argon outwards from the hearth to keep the vacuum degree in the hearth to be stabilized at about 20 torr. The vacuum pump for the reduced pressure crystal pulling process generally adopts a slide valve pump, and the slide valve pump is a mechanical vacuum pump which uses oil to maintain sealing. The argon gas carries silicon oxide and impurity volatiles generated due to high temperature during the single crystal pulling process, and is discharged to the atmosphere by pumping of a vacuum pump.
Through the analysis of the discharged argon, the main impurity components are alkane such as oxygen, nitrogen, carbon monoxide, carbon dioxide, methane and the like, and liquid lubricating oil mist; the recycling of the argon has great practical significance.
Known techniques for argon recovery purification: carrying out coarse oil removal on argon recovered from a single crystal furnace, and then carrying out high-precision oil removal and dust removal after compression and cooling; then, hydrocarbons such as methane and the like and carbon monoxide react with oxygen to produce water and carbon dioxide through high-temperature catalysis, and the excess oxygen (the oxygen is added when the impurity oxygen is insufficient) is ensured in the catalytic reaction; after cooling, enabling excessive oxygen to react with added hydrogen under the action of a catalyst to generate water, and ensuring excessive reaction hydrogen, wherein impurity components in the argon after treatment are water, carbon dioxide, hydrogen and nitrogen; and finally, adsorbing water and carbon dioxide by an argon normal-temperature adsorption unit to obtain crude argon only containing nitrogen and hydrogen as impurities. The argon normal-temperature adsorption unit consists of two adsorbers, adsorbents for adsorbing water and carbon dioxide are filled in the adsorbers, one adsorber performs adsorption work, and the other adsorber performs regeneration work including pressure relief, heating and cold blowing. The gas for regeneration work uses nitrogen, the regenerated nitrogen comes from the production or outsourcing of the low-temperature rectifying tower in the cold box, and the argon normal-temperature adsorption unit automatically controls the operation switching through the time program controller.
In patent 201210078306.x, the low-temperature rectification part uses air for circulating refrigeration, so that the energy consumption is high, the flow is complex, the excessive hydrogen added is discharged, and the utilization rate is low; in patent 201410618341.5, air compression and double-tower flow are adopted, so that the energy consumption is not advantageous, the structure is complex, and the equipment investment is increased; in patent 201621146690.2, the amount of external liquid argon provided for keeping the cold box is large, and the extraction rate is low because of the limitation of regenerated gas, and the patent only designs a hydrogenation mode to remove oxygen, so that the danger is large; in patent CN 108645118A, the stability is poor due to the low-temperature moving part; in patent CN 109631495A, use positive current expansion flow, take low temperature moving part, stability is relatively poor, is applicable to the argon atmosphere and takes the pressure to go out the tower the condition, is not suitable for the argon.
Therefore, the technical personnel in the field are dedicated to develop an argon recovery device which has simpler flow, no hydrogen deoxygenation process, no low-temperature moving part, more convenient operation and higher extraction rate and is used for removing carbon monoxide by using a rectification method.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing an argon gas recovery device that carbon monoxide and integrated high-purity nitrogen were got rid of to the not enough among the prior art to the rectification method.
In order to achieve the purpose, the utility model adopts the technical proposal that:
the argon recovery device comprises an argon compressor, a carbon monoxide reaction furnace, an argon precooling and purifying system, an air compressor, an air precooling and purifying system, a heat exchanger, a fine argon tower, an argon tower first reboiler, an argon tower second reboiler, an argon tower condensation evaporator, a nitrogen tower and a nitrogen tower condensation evaporator; wherein:
the argon compressor is connected with the argon precooling and purifying system through the carbon monoxide reaction furnace by a pipeline, the argon compressor is used for pressurizing the recovered argon, the pressurized recovered argon is subjected to oxygen removal by the carbon monoxide reaction furnace and then is sent into the argon precooling and purifying system to be cooled to remove water and carbon dioxide in the argon;
the argon precooling and purifying system is connected with a first reboiler of the argon tower arranged at the bottom of the argon rectifying tower through a pipeline and a heat exchanger so as to cool dry argon to a liquefaction temperature through the heat exchanger and send the dry argon into the first reboiler of the argon tower to form a gas-liquid mixed fluid, and the bottom of the first reboiler of the argon tower is communicated with the middle upper part of the argon rectifying tower through a pipeline so as to send the gas-liquid mixed fluid in the first reboiler of the argon tower into the middle upper part of the argon rectifying tower to participate in rectification after pressure regulation;
the bottom of the fine argon tower is communicated with the argon tower condensation evaporator through a pipeline so as to pump pure liquid argon at the bottom of the fine argon tower to the evaporation side of the argon tower condensation evaporator and evaporate the pure liquid argon into argon at the evaporation side; the evaporation side of the argon tower condensation evaporator is communicated with the outside of the rectification cold box through a pipeline and the heat exchanger, so that argon on the evaporation side is reheated by the heat exchanger and then is sent out of the rectification cold box;
the top of the argon refining tower is communicated with the argon precooling and purifying system through a heat exchanger rectification cold box and is communicated with the gas side of the argon tower condensation evaporator through a pipeline;
the air compressor is connected with the air pre-cooling purification system through a pipeline, and air is pressurized by the air compressor and then sent into the air pre-cooling purification system so as to remove water and carbon dioxide in the air after being cooled;
the air pre-cooling purification system is communicated with the bottom of the nitrogen tower through a heat exchanger through a pipeline, so that dried air is cooled to a liquefaction temperature through the heat exchanger and then is sent to the bottom of the nitrogen tower, and rectification gas is provided for the nitrogen tower;
the top of the nitrogen tower is communicated with the argon pre-cooling and purifying system through a heat exchanger outlet rectification cold box and communicated with the high-temperature side of the nitrogen tower condensation evaporator through a pipeline; and
the bottom of the nitrogen tower is communicated with the top of the nitrogen tower condensation evaporator through a pipeline.
Further, still include:
the cooler is arranged on a pipeline between the carbon monoxide reaction furnace and the argon precooling and purifying system; used for cooling the high-temperature argon after the oxygen removal of the carbon monoxide reaction furnace.
Further, the evaporation side of the argon tower condensation evaporator is communicated with the outside of the rectification cold box through a pipeline so as to supplement liquid argon for the argon tower condensation evaporator through the pipeline.
Furthermore, the pipeline out of the rectification cold box is divided into two branches, wherein one branch can be directly connected with an argon product end or connected with an argon product end after being pressurized, and the other branch is connected with a second reboiler of the argon tower through a heat exchanger; so as to divide the argon sent out of the rectification cold box into two parts: a first portion of argon is used as an argon product; and the second part of argon is taken as circulating gas and sent back to the rectification cold box, and after being cooled by the heat exchanger, the second part of argon enters the argon tower second reboiler at the bottom of the fine argon tower, is liquefied therein, and is sent to the argon tower condensation evaporator after being depressurized to provide a cold source for the argon tower condensation evaporator.
Further preferably, the method further comprises the following steps:
the argon circulating compressor is arranged on a pipeline which sequentially passes through the argon tower condensation evaporator and the heat exchanger and sequentially passes through the heat exchanger and a second reboiler of the argon tower; and the circulating argon is used for pressurizing the circulating argon sent out of the rectifying cold box and then is sent back to the rectifying cold box.
Further, the gas withdrawn from the top of the fine argon column was divided into two parts: the first part is sent out of the tower for emptying after being reheated by a heat exchanger to recover cold energy; and the second part of gas enters the gas side of the argon tower condensation evaporator to be condensed into liquid, flows into the argon refining tower and provides liquid for rectification.
Further, gas extracted from the top of the nitrogen tower is divided into two parts, the first part is sent to the high-temperature side of the condensation evaporator of the nitrogen tower and cooled into liquid nitrogen, one part of the liquid nitrogen is sent to the top of the nitrogen tower through a pipeline to participate in rectification, and the other part of the liquid nitrogen is sent out of a rectification cold box through a pipeline; and the second part is reheated by the heat exchanger and then is discharged from the rectification cold box and sent to the argon precooling and purifying system to be used as regeneration gas.
And further, the oxygen-enriched liquid air extracted from the bottom of the nitrogen tower enters the nitrogen tower condensation evaporator to provide a cold source for the nitrogen tower condensation evaporator after being subjected to pressure regulation, is vaporized into oxygen-enriched air, then enters the nitrogen tower condensation evaporator, is reheated in the heat exchanger, and is conveyed to the air precooling and purifying system after being discharged from the rectifying cold box to serve as dry gas.
The utility model adopts the above technical scheme, compare with prior art, have following technological effect:
the utility model has the advantages that the utilization and recovery site can provide the convenience of liquid argon, and the liquid argon is used for providing cold energy; the carbon monoxide gas generated in the crystal pulling process is used for removing the mixed oxygen, and the nitrogen and the excessive carbon monoxide are removed by using a low-temperature rectification method, so that the recovery rate of argon is improved, the flow and operation of low-temperature rectification are simplified, and the operation energy consumption is reduced; by utilizing an integrated air nitrogen flow path and utilizing the rich cold energy of liquid argon, the nitrogen produced in the cold box can reduce the limitation of regenerated gas and improve the extraction rate of recovered argon; and partial liquid nitrogen is produced by utilizing the cold energy of the abundant liquid argon, so that the economic benefit is improved.
Drawings
FIG. 1 is a schematic flow diagram of an argon recovery unit for removing carbon monoxide and integrating high purity nitrogen by rectification according to the present invention;
wherein the reference numerals are:
an argon compressor 1; a carbon monoxide reaction furnace 2; a cooler 3; an argon pre-cooling purification system 4; a rectification cold box 5; a heat exchanger 6; a fine argon column 7; an argon column first reboiler 8; argon column second reboiler 9; an argon column condenser-evaporator 10; a nitrogen column 11; a nitrogen column condenser evaporator 12; an air compressor 13; an air pre-cooling purification system 14; an argon gas circulation compressor 15; v1 pure liquid argon throttle valve; v2 crude liquid argon throttle valve; v5 recycle liquid argon throttle.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by a person of ordinary skill in the art without creative efforts belong to the protection scope of the present invention.
It should be noted that, in the present invention, the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention will be further described with reference to the accompanying drawings and specific embodiments, but the present invention is not limited thereto.
Example 1
As shown in fig. 1, an embodiment of the present invention provides an argon recovery device for removing carbon monoxide and integrating high purity nitrogen by rectification, including an argon compressor 1, a carbon monoxide reaction furnace 2, a cooler 3, an argon precooling and purifying system 4, an air compressor 13, an air precooling and purifying system 14, a heat exchanger 6, a refined argon tower 7, an argon tower first reboiler 8, an argon tower second reboiler 9, an argon tower condensation evaporator 10, a nitrogen tower 11, a nitrogen tower condensation evaporator 12, and an argon gas circulation compressor 15; wherein:
the argon compressor 1 is connected with an argon precooling and purifying system 4 through the carbon monoxide reaction furnace 2 by a pipeline, the argon compressor 1 is used for pressurizing the recovered argon, the pressurized recovered argon is subjected to oxygen removal by the carbon monoxide reaction furnace 2, and then the pressurized recovered argon is sent into the argon precooling and purifying system 4 to be cooled to remove water and carbon dioxide;
the cooler 3 is arranged on a pipeline between the carbon monoxide reaction furnace 2 and the argon precooling and purifying system 4; used for cooling the high-temperature argon after the oxygen removal in the carbon monoxide reaction furnace 2.
The argon precooling and purifying system 4 is connected with a first argon column reboiler 8 arranged at the bottom of the fine argon column 7 through a heat exchanger 6 through a pipeline so as to cool dry argon to a liquefaction temperature through the heat exchanger 6 and send the dry argon into the first argon column reboiler 8 to form a gas-liquid mixed fluid, the bottom of the first argon column reboiler 8 is communicated with the middle upper part of the fine argon column 7 through a pipeline so as to send the gas-liquid mixed fluid in the first argon column reboiler 8 into the middle upper part of the fine argon column 7 to participate in rectification after pressure regulation;
the bottom of the fine argon tower 7 is communicated with the argon tower condensation evaporator 10 through a pipeline, so that pure liquid argon at the bottom of the fine argon tower 7 is pumped to the evaporation side of the argon tower condensation evaporator 10 and is evaporated into argon at the evaporation side; the evaporation side of the argon tower condensation evaporator 10 is communicated with the outside of the rectification cold box 5 through the heat exchanger 6 by a pipeline, so that the argon on the evaporation side is reheated by the heat exchanger 6 and then is sent out of the rectification cold box 5;
the pipeline out of the rectifying cold box is divided into two branches, wherein one branch can be directly connected with an argon product end or connected with an argon product end after being pressurized, and the other branch is connected with a second reboiler of the argon tower through a heat exchanger; so as to divide the argon sent out of the rectification cold box 5 into two parts: a first portion of argon is used as an argon product; a second part of argon is taken as circulating gas and sent back to the rectifying cold box 5, is cooled by the heat exchanger 6, enters a second reboiler 9 of the argon tower at the bottom of the argon refining tower 7, is liquefied therein, is sent into a condensation evaporator 10 of the argon tower after being depressurized and provides a cold source for the condensation evaporator;
the argon circulating compressor 15 is arranged on a pipeline which sequentially passes through the argon tower condensation evaporator 10 and the heat exchanger 6 and sequentially passes through a position between the heat exchanger 6 and the argon tower second reboiler 9; and the circulating argon is used for pressurizing the circulating argon sent out of the rectifying cold box 5 and then is sent back to the rectifying cold box 5.
The top of the fine argon tower 7 is respectively communicated with the argon precooling and purifying system 4 through a heat exchanger 6 and a rectification cold box 5 through pipelines and is communicated with the gas side of the argon tower condensation evaporator 10 through a pipeline;
the gas withdrawn from the top of the fine argon column 7 was divided into two portions: the first part is sent out of the tower for emptying after being reheated and recycled by a heat exchanger 6; the second part of gas enters the gas side of the argon tower condensation evaporator 10 to be condensed into liquid, flows into the argon refining tower 7 and provides liquid for rectification;
further, the evaporation side of the argon column condensation evaporator 10 is communicated with the outside of the rectification cold box 5 through a pipeline so as to supplement liquid argon for the argon column condensation evaporator 10 through the pipeline.
The air compressor 13 is connected with the air pre-cooling purification system 14 through a pipeline, and air is pressurized by the air compressor 13 and then sent into the air pre-cooling purification system 14 so as to remove water and carbon dioxide in the air after being cooled;
the air pre-cooling purification system 14 is communicated with the bottom of the nitrogen tower 11 through the heat exchanger 6 through a pipeline, so that dried air is cooled to a liquefaction temperature through the heat exchanger 6 and then is sent to the bottom of the nitrogen tower 11, and rectification gas is provided for the nitrogen tower 11;
the top of the nitrogen tower 11 is respectively communicated with the argon pre-cooling and purifying system 4 through a heat exchanger 6 and a rectification cold box 5 through pipelines, and is communicated with the high-temperature side of the nitrogen tower condensation evaporator 12 through a pipeline; the gas extracted from the top of the nitrogen tower 11 is divided into two parts, the first part is sent to the high-temperature side of the nitrogen tower condensation evaporator 12 and cooled into liquid nitrogen, one part of the liquid nitrogen is sent to the top of the nitrogen tower 11 through a pipeline to participate in rectification, and the other part of the liquid nitrogen is sent out of the rectification cold box 5 through a pipeline; the second part is reheated by the heat exchanger 6 and then is sent to the argon precooling and purifying system 4 from the rectification cold box 5 to be used as regeneration gas; and
the bottom of the nitrogen tower 11 is communicated with the top of the nitrogen tower condensation evaporator 12 through a pipeline; the oxygen-enriched liquid air extracted from the bottom of the nitrogen tower 11 enters the nitrogen tower condensation evaporator 12 after being subjected to pressure regulation to provide a cold source for the nitrogen tower condensation evaporator, is vaporized into oxygen-enriched air, then enters the nitrogen tower condensation evaporator 12, enters the heat exchanger 6 for reheating, and is conveyed to the air precooling and purifying system 14 after being discharged from the rectification cold box 5 to serve as dry gas.
Example 2
This example provides an application example of the device according to the above example 1, comprising an argon recovery flow path and an air-nitrogen flow path,
the argon gas recovery flow path comprises the following steps:
s11, recovering argon components: o2 is less than or equal to 400ppm, N2 is less than or equal to 2000ppm, CO: 1000ppm and the balance Ar. Where the CO content requires > 2 times the O2 content. Since the amount of O2 is mainly due to the amount of air incorporation, N2 is present in proportion to O2;
pressurizing the recovered argon to 1.0-1.1 MPaA by an argon compressor 1, removing oil and dust, and then feeding the argon into a carbon monoxide reaction furnace 2 to remove oxygen in the argon; cooling the deoxidized argon to about 40 ℃ by a cooler 3, then entering an argon precooling and purifying system 4, cooling by an argon precooling machine, and then entering an argon purifier to remove water and carbon dioxide in the argon to obtain dry crude argon; the remaining crude argon mainly becomes: ar, N2, CO, etc.;
s12, feeding the dry crude argon into a rectification cold box 5, cooling to about-155 to-158 ℃ through a heat exchanger 6, then feeding the dry crude argon into a first reboiler 8 of an argon column arranged at the bottom of an argon rectification column 7, liquefying the gas in the first reboiler 8 of the argon column, gasifying the liquid out of the first reboiler 8 of the argon column through a throttling and pressure reducing part, and feeding the liquid into the middle upper part of the argon rectification column 7 to participate in rectification; the operating pressure of the first reboiler 8 of the argon column is 0.95MPaA to 1.05MPaA, and the pressure of the fine argon column 7 is 0.75MPaA to 0.85 MPaA; due to the pressure difference, the boiling point temperature of the medium can be changed according to the pressure, so that the temperature difference of about 1-1.5 ℃ is formed between the inner side and the outer side of the first reboiler 8 of the argon tower, and the heat exchange of the first reboiler 8 of the argon tower is ensured;
s13, feeding the gas-liquid mixed fluid into the fine argon tower 7, wherein the liquid part descends along with the liquid in the tower, and pure liquid argon is obtained at the bottom of the tower; pure liquid argon is extracted from the bottom of the argon rectifying tower 7, throttled and depressurized and then sent to the evaporation side of the argon tower condensation evaporator 10, make-up liquid argon from the outside of the rectifying cold box 5 enters the evaporation side of the argon rectifying tower condensation evaporator 12 through a pipeline, the pure liquid argon is evaporated into argon at the evaporation side of the argon tower condensation evaporator 10, and the argon is sent out of the rectifying cold box 5 after being reheated and cold energy is recovered by a heat exchanger 6;
the argon gas sent out of the rectification cold box 5 is divided into two parts: the first part of argon is used as an argon product, and the pressure of the argon product is 0.6 MPaA-0.65 MPaA; a second part of argon is taken as circulating gas, enters an argon circulating compressor 15, is pressurized to 0.9 MPaA-1.0 MPaA, is sent back to a rectifying cold box 5, is cooled to-155 to-158 ℃ through a heat exchanger 6, enters an argon tower second reboiler 8 at the bottom of an argon tower 7, is liquefied, is depressurized and is sent to an argon tower condensation evaporator 12 to provide a cold source for the argon tower condensation evaporator; the operating pressure of the argon column condenser-evaporator 10 is about 0.63 to 0.68 MPaA; if the pressure requirement of the cold box is reduced, the pressure of the whole system can be reduced;
s14, feeding the gas-liquid mixed fluid into the fine argon column 7, wherein the gas part rises along with the gas in the column, the gas at the top of the column mainly comprises carbon monoxide and nitrogen, and one part of the gas extracted from the top of the fine argon column 7 enters the argon column condensation evaporator 10 and is condensed into liquid and then fed into the fine argon column 7;
the gas withdrawn from the top of the fine argon column 7 was divided into two portions: the first part is reheated to normal temperature by a heat exchanger 6, and is generally sent out of the tower for emptying after being recovered with cold energy at the temperature 1.5-3 ℃ lower than the inlet air temperature; the second part of gas enters the gas side of the argon tower condensation evaporator 10 to be condensed into liquid, flows into the argon refining tower 7 and provides liquid for rectification;
the air nitrogen flow path comprises the following steps:
s21, after being compressed to 0.7-1.2 MPaG by the air compressor 13, the air enters the air precooling and purifying system 14, and water and carbon dioxide in the air are removed; the dried air is cooled to-160 to-175 ℃ through a heat exchanger 6 in a rectification cold box 5, and then is sent to the bottom of a nitrogen tower 11 to provide rectification gas for the nitrogen tower 11;
s22, feeding the air with liquid into the bottom of the nitrogen tower 11, wherein the heavy components are accumulated in the liquid, and obtaining liquid oxygen-enriched air at the bottom of the tower, wherein the oxygen content is about 30-40%; wherein light components are accumulated in the gas, high-purity nitrogen is obtained at the top of the tower, and the oxygen content is less than 1 ppm;
s23, the pressure of the nitrogen tower 11 is 0.4-0.8 MPaG, and the temperature is the boiling point of the liquid under the pressure; the high-purity nitrogen gas extracted from the top of the nitrogen column 11 is divided into two parts: the first part of nitrogen is sent to the high-temperature side of a nitrogen tower condensation evaporator 12, after being cooled to liquid nitrogen, one part of nitrogen is sent back to the nitrogen tower 11 to participate in the rectification of the nitrogen tower 11, and the other part of liquid nitrogen can be taken as a byproduct and is pumped out of a rectification cold box 5; the second part of nitrogen is sent out of a rectification cold box 5 after being reheated by a heat exchanger 6 to recover cold energy, and then is sent into an argon precooling and purifying system 4 to be used as regenerated gas;
s24, after adjusting the pressure of the oxygen-enriched liquid air extracted from the bottom of the nitrogen tower 11 to 0.3-0.5 MPaA, the oxygen-enriched liquid air enters the nitrogen tower condensation evaporator 12 to provide a cold source for the nitrogen tower, is vaporized into oxygen-enriched gas and then exits the nitrogen tower condensation evaporator 12, and the temperature at the moment is the boiling point temperature or higher of the oxygen-enriched gas (0.3-0.5 MPaA) under the pressure and has the temperature difference of 5-15 ℃ with the boiling point temperature of crude argon at the top of the fine argon tower 7; then enters a heat exchanger 6 for reheating, and is delivered to an air pre-cooling purification system 14 as a drying gas after being discharged from a rectification cold box 5.
The utility model utilizes the convenience provided by liquid argon in the recycling site, and uses the liquid argon to provide cold energy; the carbon monoxide gas generated in the crystal pulling process is used for removing the mixed oxygen, and the nitrogen and the excessive carbon monoxide are removed by using a low-temperature rectification method, so that the recovery rate of argon is improved, the flow and operation of low-temperature rectification are simplified, and the operation energy consumption is reduced; by utilizing an integrated air nitrogen flow path and utilizing the rich cold energy of liquid argon, the nitrogen produced in the cold box can reduce the limitation of regenerated gas and improve the extraction rate of recovered argon; and partial liquid nitrogen is produced by utilizing the cold energy of the abundant liquid argon, so that the economic benefit is improved.
The above description is only an example of the preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and those skilled in the art should be able to realize the equivalent alternatives and obvious variations of the present invention.

Claims (8)

1. An argon recovery device for removing carbon monoxide and integrating high-purity nitrogen by a rectification method is characterized by comprising an argon compressor (1), a carbon monoxide reaction furnace (2), an argon precooling and purifying system (4), an air compressor (13), an air precooling and purifying system (14), a heat exchanger (6), a refined argon tower (7), an argon tower first reboiler (8), an argon tower second reboiler (9), an argon tower condensation evaporator (10), a nitrogen tower (11) and a nitrogen tower condensation evaporator (12); wherein:
the argon compressor (1) is connected with an argon precooling and purifying system (4) through the carbon monoxide reaction furnace (2) through a pipeline, the argon compressor (1) is used for pressurizing recovered argon, the pressurized recovered argon is subjected to oxygen removal through the carbon monoxide reaction furnace (2), and then the pressurized recovered argon is sent into the argon precooling and purifying system (4) to be cooled to remove water and carbon dioxide in the argon;
the argon precooling and purifying system (4) is connected with a first argon column reboiler (8) arranged at the bottom of the argon rectifying column (7) through the heat exchanger (6) through a pipeline so as to cool the dried argon to the liquefaction temperature through the heat exchanger (6) and send the cooled argon into the first argon column reboiler (8) to form a gas-liquid mixed fluid, and the bottom of the first argon column reboiler (8) is communicated with the upper middle part of the argon rectifying column (7) through a pipeline so as to send the gas-liquid mixed fluid in the first argon column reboiler (8) into the upper middle part of the argon rectifying column (7) to be rectified after pressure regulation;
the bottom of the fine argon tower (7) is communicated with the argon tower condensation evaporator (10) through a pipeline so as to pump pure liquid argon at the bottom of the fine argon tower (7) to the evaporation side of the argon tower condensation evaporator (10) and evaporate the pure liquid argon into argon at the evaporation side; the evaporation side of the argon tower condensation evaporator (10) is communicated with the outside of the rectification cold box (5) through a pipeline by the heat exchanger (6) so as to reheat argon on the evaporation side through the heat exchanger (6) and then send the reheated argon out of the rectification cold box (5);
the top of the fine argon tower (7) is respectively communicated with the argon precooling and purifying system (4) through a rectification cold box (5) of the heat exchanger (6) through a pipeline and is communicated with the gas side of the argon tower condensation evaporator (10) through a pipeline;
the air compressor (13) is connected with the air pre-cooling purification system (14) through a pipeline, and air is pressurized by the air compressor (13) and then sent into the air pre-cooling purification system (14) so as to remove water and carbon dioxide in the air after being cooled;
the air pre-cooling purification system (14) is communicated with the bottom of the nitrogen tower (11) through the heat exchanger (6) through a pipeline, so that dried air is cooled to a liquefaction temperature through the heat exchanger (6) and then is sent to the bottom of the nitrogen tower (11), and rectification gas is provided for the nitrogen tower (11);
the top of the nitrogen tower (11) is communicated with the argon pre-cooling and purifying system (4) through a pipeline and a rectification cold box (5) of the heat exchanger (6) respectively, and is communicated with the high-temperature side of the nitrogen tower condensation evaporator (12) through a pipeline; and
the bottom of the nitrogen tower (11) is communicated with the top of the nitrogen tower condensation evaporator (12) through a pipeline.
2. The argon recovery device for removing carbon monoxide and integrating high-purity nitrogen by rectification according to claim 1, further comprising:
a cooler (3) arranged on a pipeline between the carbon monoxide reaction furnace (2) and the argon precooling and purifying system (4); used for cooling the high-temperature argon after the oxygen removal of the carbon monoxide reaction furnace (2).
3. The argon recovery device for removing carbon monoxide and integrating high-purity nitrogen by rectification according to claim 1, characterized in that the evaporation side of the argon column condensation evaporator (10) is communicated with the outside of the rectification cold box (5) through a pipeline so as to supplement liquid argon for the argon column condensation evaporator (10) through the pipeline.
4. The argon recovery device for removing carbon monoxide and integrating high-purity nitrogen by the rectification method according to claim 1, wherein a pipeline out of the rectification cold box is divided into two branches, wherein one branch can be directly or after pressurization connected with an argon product end, and the other branch is connected with a second reboiler of an argon tower through a heat exchanger; so as to divide the argon sent out of the rectification cold box (5) into two parts: a first portion of argon is used as an argon product; and the second part of argon is used as circulating gas, sent back to the rectification cold box (5), cooled by the heat exchanger (6), enters the argon tower second reboiler (9) at the bottom of the fine argon tower (7), is liquefied therein, and is sent to the argon tower condensation evaporator (10) after being depressurized to provide a cold source for the argon tower condensation evaporator.
5. The argon recovery device for removing carbon monoxide and integrating high-purity nitrogen by rectification according to claim 4, further comprising:
the argon circulating compressor (15) is arranged on a pipeline which sequentially passes through the argon tower condensation evaporator (10) and the heat exchanger (6) and sequentially passes through the heat exchanger (6) and the argon tower second reboiler (9); used for pressurizing the circulating argon sent out of the rectifying cold box (5) and then sending the pressurized circulating argon back to the rectifying cold box (5).
6. Argon recovery plant with rectification to remove carbon monoxide and to integrate high purity nitrogen according to claim 1, characterized in that the gas extracted from the top of the rectification argon column (7) is divided into two parts: the first part is sent out of the tower for emptying after being reheated and recycled by a heat exchanger (6); the second part of gas enters the gas side of the argon column condensation evaporator (10) to be condensed into liquid, flows into the argon refining column (7) and provides liquid for rectification.
7. The argon recovery device for removing carbon monoxide and integrating high-purity nitrogen through the rectification method according to claim 1, wherein the gas extracted from the top of the nitrogen tower (11) is divided into two parts, the first part is sent to the high-temperature side of the nitrogen tower condensation evaporator (12) and cooled to liquid nitrogen, one part of the liquid nitrogen is sent to the top of the nitrogen tower (11) through a pipeline to participate in rectification, and the other part of the liquid nitrogen is sent out of a rectification cold box (5) through a pipeline; the second part is reheated by the heat exchanger (6), then is discharged from the rectification cold box (5) and is sent to the argon precooling and purifying system (4) to be used as regeneration gas.
8. The argon recovery device for removing carbon monoxide and integrating high-purity nitrogen through rectification according to claim 1, wherein oxygen-enriched liquid air extracted from the bottom of the nitrogen tower (11) enters the nitrogen tower condensation evaporator (12) to provide a cold source for the nitrogen tower condensation evaporator after being subjected to pressure regulation, is vaporized into oxygen-enriched gas, then enters the heat exchanger (6) for reheating, and is conveyed to an air precooling and purifying system (14) as dry gas after being discharged from a rectification cold box (5).
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116332139A (en) * 2023-03-08 2023-06-27 上海联风气体有限公司 Argon recovery device integrating high-purity nitrogen and enhancing efficiency and application method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116332139A (en) * 2023-03-08 2023-06-27 上海联风气体有限公司 Argon recovery device integrating high-purity nitrogen and enhancing efficiency and application method thereof

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