CN211198611U - Argon recovery device for removing carbon monoxide by rectification method - Google Patents

Argon recovery device for removing carbon monoxide by rectification method Download PDF

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Publication number
CN211198611U
CN211198611U CN201922199670.1U CN201922199670U CN211198611U CN 211198611 U CN211198611 U CN 211198611U CN 201922199670 U CN201922199670 U CN 201922199670U CN 211198611 U CN211198611 U CN 211198611U
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argon
tower
carbon monoxide
rectification
pipeline
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Chinese (zh)
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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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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/02Processes or apparatus using separation by rectification in a single pressure main column system
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/40Features relating to the provision of boil-up in the bottom of a column
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/50Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/72Refluxing the column with at least a part of the totally condensed overhead gas
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00Processes or apparatus using other separation and/or other processing means
    • F25J2205/40Processes or apparatus using other separation and/or other processing means using hybrid system, i.e. combining cryogenic and non-cryogenic separation techniques
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00Processes or apparatus using other separation and/or other processing means
    • F25J2205/82Processes or apparatus using other separation and/or other processing means using a reactor with combustion or catalytic reaction
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00Processes characterised by the type or other details of the feed stream
    • F25J2210/58Argon
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00Processes characterised by the type or other details of the product stream
    • F25J2215/58Argon
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00Details related to the use of reboiler-condensers
    • F25J2250/20Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00Refrigeration techniques used
    • F25J2270/02Internal refrigeration with liquid vaporising loop
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00Refrigeration techniques used
    • F25J2270/58Quasi-closed internal or closed external argon refrigeration cycle
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00Refrigeration techniques used
    • F25J2270/90External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • F25J2270/904External 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

Abstract

The utility model relates to an argon gas recovery unit of carbon monoxide is got rid of to rectification method, including argon gas compressor, carbon monoxide reacting furnace, argon gas precooling purification system, heat exchanger, smart argon tower, the first reboiler in argon tower, argon tower second reboiler, argon tower condensation evaporimeter. 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.

Description

Argon recovery device for removing carbon monoxide by rectification method
Technical Field
The utility model relates to an argon gas recovery unit especially relates to an argon gas recovery unit of carbon monoxide is 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 for removing carbon monoxide by a rectification method aiming at the defects in the prior art.
In order to achieve the purpose, the utility model adopts the technical proposal that:
the argon recovery device for removing carbon monoxide by a rectification method comprises an argon compressor, a carbon monoxide reaction furnace, an argon precooling and purifying system, a heat exchanger, a fine argon tower, a first reboiler of the argon tower, a second reboiler of the argon tower and a condensation evaporator of the argon tower; 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;
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; a second part of argon is taken as circulating gas and sent back to the rectification cold box, the circulating gas is cooled by a heat exchanger and then enters a second reboiler of the argon tower at the bottom of the fine argon tower, the argon is liquefied in the reboiler, and the argon is sent into a condensation evaporator of the argon tower after pressure reduction to provide a cold source for the argon tower;
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.
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.
Drawings
FIG. 1 is a schematic flow diagram of an argon recovery device for removing carbon monoxide 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; an argon gas circulation compressor 11; 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 by rectification, including an argon compressor 1, a carbon monoxide reaction furnace 2, a cooler 3, an argon precooling and purifying system 4, 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, and an argon gas circulation compressor 11; 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 11 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.
Example 2
This embodiment provides an application example of the device according to embodiment 1, including the following steps:
s11, recovering argon components: o is2≤400ppm,N2Less than or equal to 2000ppm, CO: 1000ppm and the balance Ar. In which the CO content requires > 2 times O2And (4) content. Due to O2The quantity being mainly the quantity of air mixed in, N2Will react with O2Are present in proportion;
pressurizing the recovered argon to 1.1MPaA 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-115 to-118 ℃ 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;
s11, 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 11, is pressurized to 0.9 MPaA-1.0 MPaA, is sent back to a rectifying cold box 5, is cooled to-115 to-118 ℃ 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 column condensation evaporator 10 to be condensed into liquid, flows into the argon refining column 7 and provides liquid for rectification.
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.
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 (6)

1. An argon recovery device for removing carbon monoxide 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), a heat exchanger (6), an argon refining tower (7), an argon tower first reboiler (8), an argon tower second reboiler (9) and an argon tower condensation evaporator (10); 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 communicated with the argon precooling and purifying system (4) through a pipeline and the gas side of the argon tower condensation evaporator (10) through a pipeline by the heat exchanger (6) and the rectification cold box (5).
2. The argon recovery device for removing carbon monoxide 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 by rectification according to claim 1, wherein 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 the argon column condensation evaporator (10) with liquid argon through the pipeline.
4. The argon recovery device for removing carbon monoxide by a 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 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 unit for the removal of carbon monoxide by rectification according to claim 1, characterised in that the gas withdrawn 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.
CN201922199670.1U 2019-12-10 2019-12-10 Argon recovery device for removing carbon monoxide by rectification method Active CN211198611U (en)

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