CN111637685A - Single-tower cryogenic rectification argon recovery system and method with argon circulation and hydrogen circulation - Google Patents

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

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CN111637685A
CN111637685A CN202010631831.4A CN202010631831A CN111637685A CN 111637685 A CN111637685 A CN 111637685A CN 202010631831 A CN202010631831 A CN 202010631831A CN 111637685 A CN111637685 A CN 111637685A
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argon
tower
rectification
gas
column
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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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    • 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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/028—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases
    • F25J3/0285—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases of argon
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J5/00—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
    • F25J5/002—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger
    • F25J5/007—Arrangements 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
    • 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
    • F25J2200/40—Features relating to the provision of boil-up in the bottom of a 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
    • F25J2200/50—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
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F25J2205/04—Processes 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
    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/02—Recycle of a stream in general, e.g. a by-pass stream
    • 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

Abstract

The invention discloses a single-tower low-temperature rectification argon recovery system with argon circulation and hydrogen circulation and a method thereof, wherein the system comprises a pretreatment system, a rectification cold box, a hydrogen circulation compressor 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 and method with argon circulation and hydrogen circulation
Technical Field
The invention relates to the technical field of argon recovery, in particular to a system and a method for recovering argon by single-tower cryogenic rectification with argon circulation and hydrogen circulation.
Background
In the process for producing the monocrystalline silicon by the Czochralski method, the waste argon generated by recycling has great practical significance. The existing argon recovery and purification process comprises the following steps: 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.
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 argon circulation and hydrogen 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 argon circulation and hydrogen circulation, which comprises a pretreatment system, a rectification cold box, a hydrogen circulation compressor and an argon circulation compressor, wherein the pretreatment system comprises a pre-treatment system, a rectification cold box, a hydrogen circulation compressor and a hydrogen 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 specific pipeline connection sequence is as follows:
a gas outlet pipeline of a purification system of the pretreatment system is connected with the argon column reboiler through the heat exchanger, and 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; the liquid argon pipeline at the bottom of the fine argon tower is connected with the evaporation side of the argon tower condensation evaporator through the pure liquid argon throttling valve, the argon outlet pipeline at the evaporation side of the argon tower 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 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; a noncondensable gas outlet pipeline at the top of the argon tower reboiler passes through the heat exchanger and then is connected with the hydrogen circulating compressor, and an outlet pipeline of the hydrogen circulating compressor is introduced into the pretreatment system; 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.
Further, the pretreatment system comprises an argon compressor, a carbon monoxide remover, a first cooler, a deaerator, a second cooler, an argon pre-cooler and a purification system which are sequentially connected through pipelines.
Furthermore, an outlet pipeline of the hydrogen circulation compressor is combined with a system hydrogenation pipeline and then communicated with a pipeline between the first cooler and the deaerator.
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; and the evaporation side of the argon tower condensation evaporator is also connected with a liquid argon supplement pipeline.
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: after the waste argon gas to be recycled is treated by the pretreatment system, dry crude argon gas mainly containing argon gas, nitrogen gas and hydrogen gas is obtained;
s2: the dry crude argon obtained from S1 enters the rectification cold box, firstly enters the heat exchanger to be cooled to-154 ℃, and then enters an argon column reboiler at the bottom of the rectification argon column, the gas-liquid mixed fluid of the argon column reboiler is throttled and depressurized by the crude argon throttling valve and then is sent to the middle upper part of the rectification column to participate in rectification, the gas part rises along with the gas in the column, the liquid falls along with the liquid in the column, and pure liquid argon is obtained at the bottom of the rectification 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 non-condensable gas at the top of the argon tower reboiler is mainly hydrogen, and after being pumped out and subjected to heat recovery and cold recovery by the heat exchanger, the non-condensable gas is compressed by a hydrogen circulating compressor, mixed with the hydrogen added into the system and sent into the deaerator; 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.
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, an argon circulating compressor 18 and a hydrogen circulating compressor 19.
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 argon circulation and hydrogen 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, an argon circulation compressor 18 and a hydrogen circulation compressor 19; 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 specific 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; a noncondensable gas outlet pipeline at the top of the argon tower reboiler 10 is connected with a hydrogen circulating compressor 19 after passing through a heat exchanger 9, and an outlet pipeline of the hydrogen circulating compressor 19 is combined with a system hydrogenation pipeline and then communicated with a pipeline between the first cooler 3 and the deaerator 4; 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.
As a preferred embodiment, a liquid argon throttle valve 17 is arranged on a connecting pipeline between the auxiliary reboiler 16 and the argon column condensation evaporator 15; the evaporation side of the argon column condensation evaporator 15 is also connected with a liquid argon supplement pipeline.
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, the waste argon gas passes through an argon gas compressor 1, a carbon monoxide remover 2, a first cooler 3, a deaerator 4, a second cooler 5, an argon gas pre-cooler 6 and a purification system 7 in sequence to obtain the argon gas mainly comprising Ar and N2、H2Dry crude argon.
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 non-condensable gas at the top of the argon tower reboiler 10 is mainly hydrogen (the hydrogen content can reach 7 percent), is extracted through a pipeline GH-302, is sent out of a rectification cold box 8 after being reheated and cold energy recovered by a heat exchanger 9 after being extracted, is pressurized to 1.2MPa (A) through a hydrogen recovery compressor 19, is mixed with the hydrogen introduced into a system hydrogenation pipeline, and then enters a deaerator 4 to participate in reaction; the recovery of hydrogen can greatly reduce the amount of hydrogen added into the system by at least 50%.
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 argon circulation and hydrogen circulation is characterized by comprising a pretreatment system, a rectification cold box, a hydrogen circulation compressor 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 specific pipeline connection sequence is as follows:
a gas outlet pipeline of a purification system of the pretreatment system is connected with the argon column reboiler through the heat exchanger, and 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; the liquid argon pipeline at the bottom of the fine argon tower is connected with the evaporation side of the argon tower condensation evaporator through the pure liquid argon throttling valve, the argon outlet pipeline at the evaporation side of the argon tower 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 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; a noncondensable gas outlet pipeline at the top of the argon tower reboiler passes through the heat exchanger and then is connected with the hydrogen circulating compressor, and an outlet pipeline of the hydrogen circulating compressor is introduced into the pretreatment system; 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-tower cryogenic rectification argon gas recovery system according to claim 1, wherein the pretreatment system comprises an argon gas compressor, a carbon monoxide remover, a first cooler, a deaerator, a second cooler, an argon gas pre-cooler and a purification system which are sequentially connected through pipelines.
3. The single-tower cryogenic rectification argon gas recovery system according to claim 2, wherein an outlet pipeline of the hydrogen recycle compressor is combined with a system hydrogenation pipeline and then communicated with a pipeline between the first cooler and the deaerator.
4. 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.
5. The single column cryogenic rectification argon gas recovery system of claim 1 wherein a liquid argon throttle valve is provided on a connection line between the auxiliary reboiler and the argon column condenser vaporizer; and the evaporation side of the argon tower condensation evaporator is also connected with a liquid argon supplement pipeline.
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: after the waste argon gas to be recycled is treated by the pretreatment system, dry crude argon gas mainly containing argon gas, nitrogen gas and hydrogen gas is obtained;
s2: the dry crude argon obtained from S1 enters the rectification cold box, firstly enters the heat exchanger to be cooled to-154 ℃, and then enters an argon column reboiler at the bottom of the rectification argon column, the gas-liquid mixed fluid of the argon column reboiler is throttled and depressurized by the crude argon throttling valve and then is sent to the middle upper part of the rectification column to participate in rectification, the gas part rises along with the gas in the column, the liquid falls along with the liquid in the column, and pure liquid argon is obtained at the bottom of the rectification 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 non-condensable gas at the top of the argon tower reboiler is mainly hydrogen, and after being pumped out and subjected to heat recovery and cold recovery by the heat exchanger, the non-condensable gas is compressed by a hydrogen circulating compressor, mixed with the hydrogen added into the system and sent into the deaerator; 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.
CN202010631831.4A 2020-07-03 2020-07-03 Single-tower cryogenic rectification argon recovery system and method with argon circulation and hydrogen circulation Pending CN111637685A (en)

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