CN111637684A - Single-tower cryogenic rectification argon recovery system with circulation and method - Google Patents

Single-tower cryogenic rectification argon recovery system with circulation and method Download PDF

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Publication number
CN111637684A
CN111637684A CN202010631829.7A CN202010631829A CN111637684A CN 111637684 A CN111637684 A CN 111637684A CN 202010631829 A CN202010631829 A CN 202010631829A CN 111637684 A CN111637684 A CN 111637684A
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argon
column
tower
rectification
liquid
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郝文炳
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Shanghai Yingfei Energy Technology Co ltd
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Shanghai Yingfei 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
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/0228Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/028Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases
    • F25J3/0285Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases of argon
    • 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
    • F25J5/00Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
    • F25J5/002Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger
    • F25J5/007Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger combined with mass exchange, i.e. in a so-called dephlegmator
    • 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
    • F25J2205/02Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F25J2205/04Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum in the feed line, i.e. upstream of the fractionation step
    • 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
    • F25J2205/60Processes 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
    • F25J2205/66Regenerating the adsorption vessel, e.g. kind of reactivation gas
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J2245/00Processes or apparatus involving steps for recycling of process streams
    • F25J2245/02Recycle of a stream in general, e.g. a by-pass stream
    • 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 invention discloses a single-tower cryogenic rectification argon recovery system with circulation and a method thereof, wherein the system comprises an argon compressor, a carbon monoxide remover, a first cooler, a deaerator, a second cooler, an argon pre-cooler, a purification system, a rectification cold box and an argon circulation compressor; the rectification cold box comprises a heat exchanger, an argon tower reboiler, a crude liquid argon throttling valve, a fine argon tower, a pure liquid argon throttling valve, an argon tower condensation evaporator and an auxiliary reboiler. The invention utilizes the convenience provided by liquid argon in the recovery field, uses the liquid argon to provide cold energy, does not need to be provided with an expander separately, purifies the crude argon, removes nitrogen and hydrogen by using a cryogenic rectification method, enhances the efficiency of the rectification tower by using circulating argon, improves the recovery rate of the argon, simplifies the flow and operation of the cryogenic rectification and reduces the energy consumption for operation.

Description

Single-tower cryogenic rectification argon recovery system with circulation and method
Technical Field
The invention relates to the technical field of argon recovery, in particular to a single-tower cryogenic rectification argon recovery system with circulation and a method thereof.
Background
The Czochralski method is a main method for producing single crystal silicon, and 70-80% of the 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 carries silicon oxide and impurity volatile matters generated due to high temperature in the single crystal pulling process, and is exhausted to the atmosphere through the pumping of the vacuum pump, and the recycling of the argon has great practical significance.
However, in the existing technology for recovering and purifying argon, for example, patent 201210078306.X discloses a method and a device for recovering and purifying argon in monocrystalline silicon production, wherein a low-temperature rectification part uses air for circulating refrigeration, so that the energy consumption is high, the flow is complex, excessive hydrogen added is discharged, and the utilization rate is low; patent 201410618341.5 discloses a double-tower coupled argon recovery and purification device and an argon recovery and purification method, which use air compression, double-tower process, no advantage of energy consumption, complex structure and increased equipment investment.
Therefore, the technical personnel in the field are dedicated to develop an argon recovery method with simpler process, more convenient operation, higher argon recovery rate and lower energy consumption.
Disclosure of Invention
The invention provides a single-tower low-temperature rectification argon recovery system with circulation and a method thereof, aiming at solving the problems of more moving parts, high energy consumption and large investment in the existing argon recovery technology.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a single-tower low-temperature rectification argon recovery system with circulation, which comprises an argon compressor, a carbon monoxide remover, a first cooler, a deaerator, a second cooler, an argon pre-cooler, a purification system, a rectification cold box and an argon circulation compressor, wherein the first cooler is connected with the argon compressor; the rectification cold box comprises a heat exchanger, an argon tower reboiler, a crude liquid argon throttling valve, a fine argon tower, a pure liquid argon throttling valve, an argon tower condensation evaporator and an auxiliary reboiler;
the pipeline connection sequence is as follows:
the argon compressor, the carbon monoxide remover, the first cooler, the deaerator, the second cooler, the argon pre-cooler and the purification system are sequentially connected;
a gas outlet pipeline of the purification system is connected with the argon column reboiler through the heat exchanger, a condensation side pipeline of the argon column reboiler is connected with the middle upper part of the fine argon column through the crude liquid argon throttling valve, a liquid argon pipeline at the bottom of the fine argon column is connected with the evaporation side of the argon column condensation evaporator through the pure liquid argon throttling valve, an evaporation side argon outlet pipeline of the argon column condensation evaporator is divided into two paths after passing through the heat exchanger, one path is sent out of the rectification cold box, and the other path is connected with the argon gas circulating compressor; an outlet pipeline of the argon circulating compressor is connected with the evaporation side of the argon tower condensation evaporator through the heat exchanger and an auxiliary reboiler; and the outlet pipeline at the top of the fine argon tower is divided into two paths, one path of the outlet pipeline is sent out of the rectification cold box after passing through the heat exchanger and is connected with the purification system, and the other path of the outlet pipeline is connected with the condensation side of the condensation evaporator of the argon tower.
Furthermore, a cold source of the auxiliary reboiler is pure liquid argon at the bottom of the rectifying tower, and an outlet pipeline of the auxiliary reboiler is connected with the lower part of the fine argon tower.
Furthermore, a liquid argon throttling valve is arranged on a connecting pipeline between the auxiliary reboiler and the argon tower condensation evaporator.
Further, the evaporation side of the argon tower condensation evaporator is also connected with a liquid argon supplement pipeline.
Furthermore, a hydrogenation pipeline is arranged on a connecting pipeline of the first cooler and the deaerator.
And further, a nitrogen supplementing pipeline is arranged on a pipeline of the tower top nitrogen outlet pipeline of the argon refining tower which is sent out of the rectifying cold box part.
The invention provides a method for recovering argon by single-tower cryogenic rectification, which comprises the following steps:
s1: compressing waste argon to be recovered by the argon compressor, sending the compressed waste argon into the carbon monoxide remover, cooling the waste argon subjected to carbon monoxide removal to 35-40 ℃ by the first cooler, mixing the waste argon with hydrogen, sending the mixture into the deaerator, cooling the mixture to 5-8 ℃ by the second cooler and the argon pre-cooler, sending the mixture into the purifier, removing water and carbon dioxide, and sending the mixture into the rectification cold box;
s2: dry crude argon fed from S1 enters the heat exchanger to be cooled to-154 ℃ firstly, and then enters an argon column reboiler at the bottom of the fine argon column, gas-liquid mixed fluid of the argon column reboiler is throttled and depressurized by the crude argon throttling valve and then is fed into the middle upper part of the rectification column to be rectified, wherein gas part rises along with gas in the column, liquid falls along with liquid in the column, and pure liquid argon is obtained at the bottom of the fine argon column;
s3: pure liquid argon is extracted from the bottom of the fine argon tower, throttled and depressurized by a pure liquid argon throttling valve and then sent to the evaporation side of the condensation evaporator of the argon tower; meanwhile, externally supplemented liquid argon enters the evaporation side of the condensation evaporator of the argon tower; pure liquid argon is evaporated into argon gas at the evaporation side of the argon tower condensation evaporator, and after entering the heat exchanger for reheating and cold quantity recovery, one path of pure liquid argon is sent out of the rectification cold box and supplied to customers; the other route is pressurized by the argon gas circulating compressor, then is sent to the heat exchanger to be cooled to the liquefaction temperature, is liquefied by the auxiliary reboiler, and is throttled by the liquid argon throttling valve and then is sent to the evaporation side of the condensation evaporator of the liquid argon column;
s4: the mixed gas of hydrogen and nitrogen is mainly taken from the top of the fine argon column and then is divided into two paths, one path of mixed gas is sent out after the heat exchanger recovers heat and recovers cold, the other path of mixed gas is sent out from the rectification cold box and enters the purification system for regeneration, the other path of mixed gas enters the condensation side of the condensation evaporator of the argon column to be condensed into liquid, and the liquid flows into the fine argon column
Further, at the CO outlet of the carbon monoxide remover, the CO content is <1 ppm.
Further, a temperature difference of 1.2-1.4 ℃ is formed between the inner side and the outer side of the argon column reboiler.
Furthermore, the cold source of the auxiliary reboiler is pure liquid argon from the bottom of the argon refining column, and the gasified gas is returned to the argon refining column to participate in rectification as ascending gas.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the invention utilizes the convenience provided by liquid argon in the recovery field, uses the liquid argon to provide cold energy, does not need to be provided with an expander separately, purifies the crude argon, removes nitrogen and hydrogen by using a cryogenic rectification method, enhances the efficiency of the rectification tower by using circulating argon, improves the recovery rate of the argon, simplifies the flow and operation of the cryogenic rectification and reduces the energy consumption for operation.
Drawings
FIG. 1 is a schematic diagram of a single column cryogenic rectification argon recovery system of the present invention;
the reference signs are:
the system comprises an argon compressor 1, a carbon monoxide remover 2, a first cooler 3, a deaerator 4, a second cooler 5, an argon pre-cooler 6, a purification system 7, a rectification cold box 8, a heat exchanger 9, an argon tower reboiler 10, a crude liquid argon throttling valve 11, a fine argon tower 12, a pure liquid argon throttling valve 13, a liquid argon supplement pipeline throttling valve 14, an argon tower condensation evaporator 15, an auxiliary reboiler 16, a liquid argon throttling valve 17 and an argon circulating compressor 18.
Detailed Description
The present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
Example 1
As shown in fig. 1, the embodiment provides a single-tower cryogenic rectification argon recovery system with circulation, which includes an argon compressor 1, a carbon monoxide remover 2, a first cooler 3, a deaerator 4, a second cooler 5, an argon pre-cooler 6, a purification system 7, a rectification cold box 8 and an argon circulation compressor 18; the rectification cold box 8 comprises a heat exchanger 9, an argon tower reboiler 10, a crude liquid argon throttling valve 11, a fine argon tower 12, a pure liquid argon throttling valve 13, an argon tower condensation evaporator 15 and an auxiliary reboiler 16;
the pipeline connection sequence is as follows:
the argon compressor 1, the carbon monoxide remover 2, the first cooler 3, the deaerator 4, the second cooler 5, the argon pre-cooler 7 and the purification system 7 are sequentially connected;
a gas outlet pipeline of the purification system 7 is connected with an argon column reboiler 10 through a heat exchanger 9, a condensation side pipeline of the argon column reboiler 10 is connected with the middle upper part of an argon refining column 12 through a crude liquid argon throttling valve 11, a liquid argon pipeline at the bottom of the argon refining column 12 is connected with an evaporation side of an argon column condensation evaporator 15 through a pure liquid argon throttling valve 13, an evaporation side argon outlet pipeline of the argon column condensation evaporator 15 is divided into two paths after passing through the heat exchanger 9, one path is sent out of a rectification cold box 8, and the other path is connected with an argon gas circulating compressor 18; an outlet pipeline of the argon circulating compressor 18 is connected with the evaporation side of the argon tower condensation evaporator 15 through a heat exchanger 9 and an auxiliary reboiler 16; the outlet pipeline at the top of the fine argon column 12 is divided into two paths, one path is sent out of the rectification cold box 8 after passing through the heat exchanger 9 and is connected with the purification system 7, and the other path is connected with the condensation side of the condensation evaporator 15 of the argon column.
As a preferred embodiment, the cold source of the auxiliary reboiler 16 is pure liquid argon at the bottom of the rectification column 12, and the outlet pipeline of the auxiliary reboiler 16 is connected with the lower part of the argon refining column 12.
In a preferred embodiment, a liquid argon throttle valve 17 is provided in a connection between the auxiliary reboiler 16 and the argon column condenser-evaporator 15.
In a preferred embodiment, a liquid argon make-up line is also connected to the vapor side of the argon column condenser-evaporator 15.
As a preferred embodiment, a hydrogenation line is arranged on a connection line between the first cooler 3 and the deaerator 4.
As a preferred embodiment, a nitrogen supplementing pipeline is arranged on a pipeline of a top nitrogen outlet pipeline of the argon refining tower 12 which is sent out of the cold rectifying box 8.
Example 2
With the system provided in example 1, this example provides a method for recovering argon:
1890Nm required for recovery3The pressure of the waste argon gas is very low, about 5 percent of air is mixed, firstly the waste argon gas is pressurized to 1.45MPa (A) by an argon compressor 1 and enters a carbon monoxide remover 2 by a pipeline GAr-101, the carbon monoxide remover 2 is filled with a catalyst, the carbon monoxide is catalyzed into carbon dioxide by catalytic reaction, and the content of CO at an outlet is reduced<1 ppm; after the waste argon gas without CO comes out, the waste argon gas enters a first cooler 3 through a pipeline GAr-102 to be cooled to 35-40 ℃, the waste argon gas is mixed with added hydrogen in a pipeline GAr-103 and then enters a deaerator 4, and oxygen and the hydrogen are generated in the deaerator 4The raw reaction generates water and releases heat (the temperature can be different according to the rise of oxygen amount, in O)2When the content is not more than 0.4%, the temperature is in<100 ℃); then the high-temperature argon enters a second cooler 5 through a pipeline GAr-104 to be cooled to 40 ℃, enters an argon pre-cooler 6 through a pipeline GAr-105 to be cooled to 5-8 ℃ (the temperature is favorable for adsorption of a molecular sieve), enters a purification system 7 through a pipeline GAr-106 to remove water and carbon dioxide, and the obtained crude argon mainly becomes Ar and N2、H2
The dry crude argon enters a rectification cold box 8, firstly enters a heat exchanger 9 through a pipeline GAr-107 to be cooled to-154 ℃, then enters an argon tower reboiler 10 positioned at the bottom of a refined argon tower 12, in the argon tower reboiler 10, the temperature of liquid is-156.7 ℃, through simulation, 94% of gas in GAr-109 is liquefied, and gas-liquid mixed fluid out of the argon tower reboiler 10 is throttled and reduced to 0.62MPaA through a crude liquid argon throttle valve 11 and then is sent to the middle upper part of the refined argon tower 12 to participate in rectification. Wherein the condensing side of argon column reboiler 10 is 1.23mpa (a), -155.5 ℃ due to the pressure differential; the evaporation side is 1MPa (A) and-156.7 ℃, the boiling temperature can be changed according to the pressure, so that the temperature difference between the inner side and the outer side of the reboiler is 1.2 ℃, thereby ensuring the work of the argon column reboiler 10.
The gas part of the fluid entering the fine argon column 12 through the pipeline GAr-109 rises along with the gas in the column, the liquid descends along with the liquid in the column, the gas and the liquid generate heat and mass transfer in the rising and descending processes, the Ar content of the liquid part is higher and higher, and pure liquid argon is obtained at the bottom of the column, namely 99.9997 percent; pure liquid argon with a flow path of LAr-201 is extracted from the bottom of the fine argon tower 12 and is throttled and depressurized by a pure liquid argon throttling valve 13 and sent to the evaporation side of an argon tower condensation evaporator 15; meanwhile, the externally supplemented liquid argon 60kg/h enters the evaporation side of the argon tower condensation evaporator 15 together to supplement the refrigeration loss for the whole system.
Pure liquid argon is evaporated into argon at the evaporation side of an argon tower condensation evaporator 15, enters a heat exchanger 9 for reheating and cold recovery, one path of the argon is sent out of a rectification cold box 8 and is supplied to customers, GAr-204 is a conveying pipeline, the pressure is 0.6MPa (G), the temperature is 17 ℃, and the flow is 1978Nm3/h;
The other path is 240Nm in the pipeline GAr-2053After the argon is pressurized by the circulating compressor 18 to 1.22MPa (A), the argon is cooled to 40 ℃ by a cooler of the argon circulating compressor 18, sent to the heat exchanger 9 in the rectification cold box 8 through a pipeline GAr-206 and cooled to the liquefaction temperature (-153.6 ℃), then sent to the auxiliary reboiler 16 for liquefaction, and completely liquefied when coming out from the pipeline LAr-202, the liquid in LAr-202 is throttled by the liquid argon throttling valve 17 and then sent to the evaporation side of the condensation evaporator 15 of the argon tower to provide a cold source for the liquid. Wherein, the cold source of the auxiliary reboiler 16 comes from pure liquid argon at the bottom of the argon refining column 12, and the gasified gas returns to the argon refining column 12 to participate in rectification as ascending gas.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.

Claims (10)

1. A single-tower low-temperature rectification argon recovery system with circulation is characterized by comprising an argon compressor, a carbon monoxide remover, a first cooler, a deaerator, a second cooler, an argon pre-cooler, a purification system, a rectification cold box and an argon circulation compressor; the rectification cold box comprises a heat exchanger, an argon tower reboiler, a crude liquid argon throttling valve, a fine argon tower, a pure liquid argon throttling valve, an argon tower condensation evaporator and an auxiliary reboiler;
the pipeline connection sequence is as follows:
the argon compressor, the carbon monoxide remover, the first cooler, the deaerator, the second cooler, the argon pre-cooler and the purification system are sequentially connected;
a gas outlet pipeline of the purification system is connected with the argon column reboiler through the heat exchanger, a condensation side pipeline of the argon column reboiler is connected with the middle upper part of the fine argon column through the crude liquid argon throttling valve, a liquid argon pipeline at the bottom of the fine argon column is connected with the evaporation side of the argon column condensation evaporator through the pure liquid argon throttling valve, an evaporation side argon outlet pipeline of the argon column condensation evaporator is divided into two paths after passing through the heat exchanger, one path is sent out of the rectification cold box, and the other path is connected with the argon gas circulating compressor; an outlet pipeline of the argon circulating compressor is connected with the evaporation side of the argon tower condensation evaporator through the heat exchanger and an auxiliary reboiler; and the outlet pipeline at the top of the fine argon tower is divided into two paths, one path of the outlet pipeline is sent out of the rectification cold box after passing through the heat exchanger and is connected with the purification system, and the other path of the outlet pipeline is connected with the condensation side of the condensation evaporator of the argon tower.
2. The single column cryogenic rectification argon gas recovery system of claim 1 wherein the cold source of the auxiliary reboiler is pure liquid argon at the bottom of the rectification column and the outlet line of the auxiliary reboiler is connected to the lower portion of the fine argon column.
3. The single column cryogenic rectification argon gas recovery system of claim 1 wherein a liquid argon throttle valve is provided in a connection line between the auxiliary reboiler and the argon column condenser vaporizer.
4. The single column cryogenic rectification argon gas recovery system of claim 1 wherein the vapor side of the argon column condenser vaporizer is further connected to a liquid argon make-up line.
5. The single-tower cryogenic rectification argon gas recovery system according to claim 1, wherein a hydrogenation pipeline is arranged on a connecting pipeline between the first cooler and the deaerator.
6. The single column cryogenic rectification argon gas recovery system of claim 1 wherein a nitrogen make-up line is provided on a line from the overhead nitrogen outlet line of the argon rectification column out of the cold box section of the rectification.
7. A method for recovering argon by using single-tower cryogenic rectification of a system according to any one of claims 1 to 6, comprising the steps of:
s1: compressing waste argon to be recovered by the argon compressor, sending the compressed waste argon into the carbon monoxide remover, cooling the waste argon subjected to carbon monoxide removal to 35-40 ℃ by the first cooler, mixing the waste argon with hydrogen, sending the mixture into the deaerator, cooling the mixture to 5-8 ℃ by the second cooler and the argon pre-cooler, sending the mixture into the purifier, removing water and carbon dioxide, and sending the mixture into the rectification cold box;
s2: dry crude argon fed from S1 enters the heat exchanger to be cooled to-154 ℃ firstly, and then enters an argon column reboiler at the bottom of the fine argon column, gas-liquid mixed fluid of the argon column reboiler is throttled and depressurized by the crude argon throttling valve and then is fed into the middle upper part of the rectification column to be rectified, wherein gas part rises along with gas in the column, liquid falls along with liquid in the column, and pure liquid argon is obtained at the bottom of the fine argon column;
s3: pure liquid argon is extracted from the bottom of the fine argon tower, throttled and depressurized by a pure liquid argon throttling valve and then sent to the evaporation side of the condensation evaporator of the argon tower; meanwhile, externally supplemented liquid argon enters the evaporation side of the condensation evaporator of the argon tower; pure liquid argon is evaporated into argon gas at the evaporation side of the argon tower condensation evaporator, and after entering the heat exchanger for reheating and cold quantity recovery, one path of pure liquid argon is sent out of the rectification cold box and supplied to customers; the other route is pressurized by the argon gas circulating compressor, then is sent to the heat exchanger to be cooled to the liquefaction temperature, is liquefied by the auxiliary reboiler, and is throttled by the liquid argon throttling valve and then is sent to the evaporation side of the condensation evaporator of the liquid argon column;
s4: the mixed gas of hydrogen and nitrogen is mainly taken out of the top of the fine argon tower and then divided into two paths, one path of mixed gas is sent out of the rectification cold box after being reheated by the heat exchanger to recover cold energy and then enters the purification system for regeneration, the other path of mixed gas enters the condensation side of the condensation evaporator of the argon tower to be condensed into liquid, and the liquid flows into the fine argon tower.
8. The single column cryogenic rectification argon gas recovery process of claim 7 wherein the CO content at the CO outlet of the carbon monoxide remover is <1 ppm.
9. The single column cryogenic rectification argon gas recovery method of claim 7 wherein a temperature difference of 1.2 to 1.4 ℃ is formed between the inside and outside of the argon column reboiler.
10. The method for recovering argon through single-column cryogenic rectification as claimed in claim 7, wherein a cold source of the auxiliary reboiler is derived from pure liquid argon at the bottom of the argon refining column, and gasified gas is returned to the argon refining column to participate in rectification as ascending gas.
CN202010631829.7A 2020-07-03 2020-07-03 Single-tower cryogenic rectification argon recovery system with circulation and method Pending CN111637684A (en)

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CN110803689A (en) * 2019-12-10 2020-02-18 上海联风能源科技有限公司 Argon recovery method and device for removing carbon monoxide and integrating high-purity nitrogen by rectification method
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JPH11228116A (en) * 1998-02-12 1999-08-24 Nippon Sanso Kk Recovering and purifying method of argon and device therefor
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