CN104406364B - The argon of a kind of double tower coupling reclaims purifier apparatus and argon reclaims purification process - Google Patents

The argon of a kind of double tower coupling reclaims purifier apparatus and argon reclaims purification process Download PDF

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Publication number
CN104406364B
CN104406364B CN201410618341.5A CN201410618341A CN104406364B CN 104406364 B CN104406364 B CN 104406364B CN 201410618341 A CN201410618341 A CN 201410618341A CN 104406364 B CN104406364 B CN 104406364B
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argon
liquid
tower
nitrogen
oxygen
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CN104406364A (en
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顾燕新
郑达海
彭旭东
朱云峰
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Hangzhou oxygen generator group Co.,Ltd.
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Hangzhou Hangyang Co Ltd
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/044—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a single pressure main column system only
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/04096—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of argon or argon enriched 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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
    • F25J3/0426—The cryogenic component does not participate in the fractionation
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
    • F25J3/04727—Producing pure argon, e.g. recovered from a crude argon column using an auxiliary pure argon column for nitrogen rejection
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04951—Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network
    • F25J3/04963—Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network and inter-connecting equipment within or downstream of the fractionation unit(s)
    • 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
    • F25J2260/00—Coupling of processes or apparatus to other units; Integrated schemes
    • F25J2260/58—Integration in an installation using argon

Abstract

The argon of a kind of double tower coupling reclaims purifier apparatus and argon reclaims purification process, described equipment mainly includes an ice chest, one main heat exchanger, low-temperature fractionating tower and liquid argon pump, described ice chest is at least provided with main heat exchanger and low-temperature fractionating tower, described low-temperature fractionating tower is the double tower coupled structure being made up of Shang Ta and lower tower, wherein go up tower be argon column, lower tower be nitrogen tower, the top of described argon column arranges condenser；Described method is: crude argon enters main heat exchanger cooling liquid in ice chest, argon column during throttling enters the low-temperature fractionating tower of argon column nitrogen tower double tower coupling again, make argon produce rectification with nitrogen hydrogen in argon column to separate, obtaining pure liquid argon bottom argon column, pure liquid argon obtains pure argon product after liquid argon pump supercharging main heat exchanger re-heat；It is high that it has the argon response rate, reclaims purity of argon high, and impurity oxygen Gas content is low, reclaims the purification energy consumption feature such as nitrogen side-product and oxygen-enriched air side-product low, available.

Description

The argon of a kind of double tower coupling reclaims purifier apparatus and argon reclaims purification process
Technical field
The present invention relates to a kind of argon being mainly used in the double tower coupling that argon in monocrystalline silicon production reclaims purification and reclaim purifier apparatus and argon recovery purification process.
Background technology
Vertical pulling method (Czochralski Method) being the main method producing monocrystal silicon, the monocrystal silicon in the whole world 70% ~ 80% is produced by vertical pulling method.It is to use i.e. picture vacuum technology again as the decompression crystal pulling technique of the atmosphere technique that flows that the most frequently used vertical pulling method produces monocrystal silicon technique；Decompression technique is in silicon single crystal pulling process, constant speed in single crystal growing furnace burner hearth, it is passed through high purity argon continuously, vacuum pump is constantly from the outside pump Argon of burner hearth simultaneously, in keeping burner hearth, vacustat is about 20 torr, the feature of the existing vacuum technology of this technique, has again the feature of flowing atmosphere technique.The vacuum pump of decompression crystal pulling technique typically uses slide valve pump, and slide valve pump is the oil-sealed rotary pump keeping sealing with oil.Si oxide that argon produces due to high temperature during carrying crystal-pulling and impurity volatile matter, and it is discharged into air by pumping of vacuum pump.
By the analysis to discharge argon, major impurity composition is, the alkane such as oxygen, nitrogen, carbon monoxide, carbon dioxide, methane, liquid lubricant mist；Recycle this part argon and have the biggest realistic meaning.
Argon reclaims the known technology of purification: the argon reclaimed from single crystal growing furnace carries out high accuracy oil removing dedusting after thick oil removing, more compressed cooling；Then passing through high-temperature catalytic makes the hydro carbons such as methane and carbon monoxide produce water and carbon dioxide with oxygen reaction, ensures oxygen excess (impurity oxygen the most then adds oxygen) in catalytic reaction；By making the same hydrogen water generation reaction added of excessive oxygen after cooling under catalyst action, and ensureing to react hydrogen excess, after process, in argon, impurity component is water, carbon dioxide, hydrogen and nitrogen；Eventually pass argon room temperature absorbing unit absorption water and carbon dioxide, obtain comprising only nitrogen and hydrogen is the crude argon of impurity.Argon room temperature absorbing unit is made up of two adsorbers, and equipped with absorption water and the adsorbent of carbon dioxide in adsorber, an adsorber carries out adsorbing work, and another adsorber carries out including pressure release, heats, blows cold reproduction operation.The gas of described reproduction operation uses nitrogen, and this regeneration nitrogen produces or outsourcing from low-temperature fractionating tower in ice chest, and argon room temperature absorbing unit is switched by program timer auto-controll operation.
Summary of the invention
It is an object of the invention to provide a kind of argon response rate high, recovery purity of argon is high, oxygen content is low, recovery purification energy consumption is low, and the argon being particularly suitable for the double tower coupling that large-scale monocrystalline silicon production enterprise carries out a large amount of argon recovery purification recycling reclaims purifier apparatus and argon recovery purification process.
The purpose of the present invention completes by following technical solution, the argon of a kind of double tower coupling reclaims purifier apparatus, this equipment mainly includes an ice chest, one main heat exchanger, low-temperature fractionating tower and liquid argon pump, described ice chest is at least provided with main heat exchanger and low-temperature fractionating tower, described low-temperature fractionating tower is the double tower coupled structure being made up of Shang Ta and lower tower, wherein go up tower be argon column, lower tower be nitrogen tower, middle be coupled by condenser/evaporator；The top of described argon column arranges condenser, and described argon column is a upper rectifying column that the crude argon rectification entering this tower can be separated into liquid argon and rectification waste gas；And described nitrogen tower is one air to be isolated nitrogen and make a part of nitrogen as side-product, another part is for the lower rectifying column of argon room temperature absorbing unit regeneration.
Condenser/evaporator between argon column of the present invention and nitrogen tower is to be coupled to form by the condenser as the vaporizer bottom argon column with as nitrogen top of tower, thermal source therein is the source nitrogen from nitrogen tower, low-temperature receiver is the liquid argon source from argon column, and source nitrogen is in intermediate condensation, and liquid argon evaporates in outside；The thermal source of the condenser that described argon column top is arranged is the upflowing vapor from argon column, and low-temperature receiver is the throttling oxygen-enriched liquid air from nitrogen tower bottom, and wherein upflowing vapor evaporates in the outside of condenser at the intermediate condensation of condenser, throttling oxygen-enriched liquid air；Described liquid argon pump is also mounted in ice chest, and the liquid argon products export bottom described argon column connects described liquid argon pump and carries out supercharging, and accesses user's argon pipe network by the main heat exchanger re-heat in ice chest to room temperature.
In main heat exchanger of the present invention at least provided with:
One crude argon cooling liquid passage, the import of this passage connects the crude argon inlet pipe entering ice chest, and outlet connects a choke valve and accesses argon column again；
One pressure-air cooling passage, the import of this passage connects the compressed air inlet pipe entering ice chest, and outlet accesses nitrogen tower；
One nitrogen re-heat passage, the import connection of this passage and the nitrogen outlet of nitrogen top of tower, the outlet of passage picks out ice chest by nitrogen tube；
One oxygen-enriched re-heat passage, the import of this passage is respectively communicated with oxygen-enriched liquid air outlet and the oxygen-rich steam outlet at argon column top, and the outlet of passage picks out ice chest by oxygen-enriched connecting tube；Or having two oxygen-enriched re-heat passages, the import of these two passages is respectively communicated with oxygen-enriched liquid air outlet and the oxygen-rich steam outlet at argon column top, and the outlet of two passages picks out ice chest by oxygen-enriched connecting tube respectively.
A kind of argon utilizing above-mentioned double tower to couple reclaims purifier apparatus and carries out the method that argon reclaims purification, and described argon reclaims the method for purification and includes:
A) cooling of crude argon, first uses known technology to produce the crude argon containing only nitrogen hydrogen, and crude argon enters ice chest, and entering back into main heat exchanger cooling liquid is liquid argon；Liquid argon enters argon column after choke valve throttles and carries out rectification separation；
B) crude argon rectification, crude argon carries out rectification separation according to the characteristic that component boiling point is different in argon column, obtains liquid argon product bottom argon column, discharges rectification waste gas at argon column top；The condenser condensation upflowing vapor at argon column top, the liquid of condensation is as the backflow of argon column, and not solidifying gas is rectification waste gas, and this rectification waste gas is extracted out from condenser condensation side；The liquid of condensation and under the choke valve throttling liquid that obtains of liquid argon is as rectification descending liquid, the upflowing vapor counter current contacting that lower descending liquid is evaporated with condenser/evaporator bottom argon column carries out heat and mass, flowing to obtain bottom argon column liquid argon under thus, upflowing vapor is from rising at the bottom of tower and converging and eventually become upflowing vapor from the gas obtained through choke valve throttling liquid argon；Bottom argon column, a part for liquid argon is discharged as product liquid argon, and another part is condensed evaporator evaporation as upflowing vapor；
C) the producing of argon product, product liquid argon is pressurized to the liquid argon of user's argon ductwork pressure through liquid argon pump, and liquid argon enters main heat exchanger re-heat becomes the real argon entrance user's argon pipe network reclaiming purification to room temperature；In product liquid argon, oxygen content general control is at below 2PPm, and the mole of product liquid argon can reach in crude argon more than the 92% of argon mole.
Method of the present invention also includes:
D) through removing the compressed air of the impurity such as moisture content and carbon dioxide, enter ice chest, enter back into main heat exchanger and be cooled into Cryogenic air, Cryogenic air can be all gas also can contain a small amount of liquid, Cryogenic air enters low-temperature fractionating tower nitrogen tower, wherein gas part is as the upflowing vapor of nitrogen tower, and liquid portion flows to the tower reactor at the bottom of tower；Upflowing vapor carries out heat and mass with the backflow counter current contacting flowed down from tower top, obtain nitrogen at nitrogen top of tower and enter condenser/evaporator nitrogen, nitrogen is condensed into liquid portion as nitrogen tower liquid nitrogen reflux liquid in condenser/evaporator, not coagulating portion gas is that fixed gas extracts condenser/evaporator discharge out, and the discharge capacity of fixed gas is generally less than compressed-air actuated 1%；Liquid nitrogen reflux liquid to dirty, flow to the liquid joint of tower reactor and becomes oxygen-enriched liquid air with Cryogenic air and extract out in the tower reactor at the bottom of nitrogen tower tower through flowing to the heat and mass of upflowing vapor in nitrogen tower.
Nitrogen of the present invention obtains side-product nitrogen through main heat exchanger re-heat to room temperature, and this nitrogen partial is as the regeneration nitrogen of argon room temperature absorbing unit, and remaining can use as plant protection gas；
Described oxygen-enriched liquid air enters argon column condenser after choke valve, condenses the upflowing vapor from argon column as low-temperature receiver within the condenser, and self overwhelming majority is vaporizated into oxygen-rich steam, does not has evaporation section to discharge bottom condenser as oxygen-enriched liquid air；The discharge effect of oxygen-enriched liquid air is a small amount of CH preventing from containing in oxygen-enriched liquid air4In condenser accumulation thus causing dangerous hidden danger with the heavy component such as nitrous oxide, the discharge capacity of oxygen-enriched liquid air is generally the 1%～about 3% of oxygen-enriched liquid air total amount；Described oxygen-enriched liquid air and oxygen-rich steam converge entrance main heat exchanger re-heat after going out condenser become room temperature oxygen-enriched air to room temperature；Or oxygen-enriched liquid air and oxygen-rich steam enter main heat exchanger respectively, go out main heat exchanger respectively；Oxygen-enriched air as the regeneration gas of air room temperature absorbing unit it can also be used to need the place of oxygen-enriched combusting.
The fresh liquid argon of supplementary rectification institute chilling requirement can be passed directly into bottom argon column of the present invention, then discharge argon column with the liquid argon product reclaimed and become liquid argon product, fresh liquid argon also can add in liquid argon after liquid argon pump, or described fresh liquid argon the most directly enters after main heat exchanger carries out re-heat to individually enter argon pipe network.
The present invention first uses known technology to produce the crude argon comprising only hydrogen nitrogen, then the present invention is used to carry out argon and the separation of nitrogen hydrogen, the crude argon using known technology to produce enters main heat exchanger cooling liquid in ice chest, enter low-temperature fractionating tower, make argon produce rectification with nitrogen hydrogen to separate, obtaining pure liquid argon, liquid argon obtains straight argon product after liquid argon pump supercharging main heat exchanger re-heat；The argon response rate of argon retracting device of the present invention is the highest up to 92%, and fresh liquid argon can supplement cryogenic rectification cold while supplementing argon waste, is thus not required to additionally arrange refrigeration plant such as decompressor etc., thus simple flow and minimizing investment.
It is high that the present invention has the argon response rate, reclaims purity of argon high, and oxygen content is low, reclaims purification energy consumption low, is particularly suitable for large-scale monocrystalline silicon production enterprise and carries out the features such as a large amount of argon recovery purification recycling.
Accompanying drawing explanation
Fig. 1 is the structure explanation schematic flow sheet that argon of the present invention reclaims purification devices.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention will be described in detail: shown in Fig. 1, and the argon of a kind of double tower of the present invention coupling reclaims purifier apparatus, and this equipment mainly includes an ice chest B1, a main heat exchanger E1, low-temperature fractionating tower and liquid argon pump 107.
Ice chest purposes is to provide a cold insulated cabinet for cryogenic equipment pipeline, and equipment pipe loads full pearlife after being arranged in centre, thus reduces medium apparatus pipeline and transmit cold in environment.The placement of liquid argon pump also can be placed on outside ice chest in can being placed on ice chest, is placed on outside ice chest and then needs to use vacuum tube heat insulation.
Described ice chest B1 is at least provided with main heat exchanger E1 and low-temperature fractionating tower, described low-temperature fractionating tower is the double tower coupled structure being made up of Shang Ta and lower tower, wherein go up tower be argon column T1, lower tower be nitrogen tower T2, centre is coupled by condenser/evaporator E2, it can save energy consumption, saves space；It is a upper rectifying column that the crude argon rectification entering this tower can be separated into liquid argon and rectification waste gas that the top of described argon column T1 arranges condenser E3, described argon column T1；And described nitrogen tower T2 is one air to be isolated nitrogen and make a part of nitrogen as side-product, another part is for the lower rectifying column of argon room temperature absorbing unit regeneration.
Condenser/evaporator E2 between described argon column T1 and nitrogen tower T2 is to be coupled to form by the condenser as the vaporizer bottom argon column T1 with as nitrogen tower T2 top, thermal source therein is the source nitrogen from nitrogen tower T2, low-temperature receiver is the liquid argon source from argon column T1, source nitrogen is in intermediate condensation, and liquid argon evaporates in outside；The thermal source of the condenser that described argon column top is arranged is the upflowing vapor from argon column, and low-temperature receiver is the throttling oxygen-enriched liquid air from nitrogen tower bottom, and wherein upflowing vapor evaporates in the outside of condenser at the intermediate condensation of condenser, throttling oxygen-enriched liquid air；Described liquid argon pump 107 is also mounted in ice chest B1, and the liquid argon products export bottom described argon column T1 connects described liquid argon pump 107 and carries out supercharging, and accesses user's argon pipe network by the main heat exchanger re-heat in ice chest B1 to room temperature.
In main heat exchanger E1 of the present invention at least provided with:
One crude argon cooling liquid passage 1, the import of this passage connects crude argon 101 inlet pipe entering ice chest B1, and outlet connects a choke valve 103 and accesses argon column T1 again；
One pressure-air cooling passage 2, the import of this passage connects compressed air 121 inlet pipe entering ice chest B1, and outlet accesses nitrogen tower T2；
The nitrogen outlet at one nitrogen re-heat passage 3, the import connection of this passage and nitrogen tower T2 top, the outlet of passage picks out ice chest B1 by nitrogen tube；
One oxygen-enriched re-heat passage 4, the import of this passage is respectively communicated with oxygen-enriched liquid air outlet and the oxygen-rich steam outlet at argon column T1 top, and the outlet of passage picks out ice chest B1 by oxygen-enriched connecting tube；Or having two oxygen-enriched re-heat passages, the import of these two passages is respectively communicated with oxygen-enriched liquid air outlet and the oxygen-rich steam outlet at argon column top, and the outlet of two passages picks out ice chest by oxygen-enriched connecting tube respectively.
A kind of argon utilizing described double tower to couple reclaims purifier apparatus and carries out the method that argon reclaims purification, and described argon reclaims the method for purification and includes:
A) cooling of crude argon, first uses known technology to produce the crude argon containing only nitrogen hydrogen, and crude argon 101 enters ice chest B1, and entering back into main heat exchanger E1 cooling liquid is liquid argon 102；Liquid argon 102 enters argon column T1 after choke valve 103 throttles and carries out rectification separation；
B) crude argon rectification, crude argon carries out rectification separation according to the characteristic that component boiling point is different in argon column T1, obtains liquid argon product 106 bottom argon column T1, discharges rectification waste gas 112 at argon column T1 top；The condenser E3 at argon column T1 top condenses upflowing vapor 104, and the liquid 111 of condensation is as the backflow of argon column T1, and not solidifying gas is rectification waste gas 112, and this rectification waste gas 112 is extracted out from condenser E3 condensation side；The liquid 111 of condensation and through choke valve 103 throttle liquid that liquid argon 102 obtains as rectification under descending liquid, the upflowing vapor counter current contacting that lower descending liquid is evaporated with condenser/evaporator E2 bottom argon column T1 carries out heat and mass, flowing to obtain bottom argon column T1 liquid argon under thus, upflowing vapor is from rising at the bottom of tower and converging and eventually become upflowing vapor 104 from through choke valve 103 gas that liquid argon 102 obtains that throttles；Bottom argon column T1, a part for liquid argon is discharged as product liquid argon 106, and another part is condensed vaporizer E2 evaporation as upflowing vapor；
C) the producing of argon product, product liquid argon 106 is pressurized to the liquid argon 108 of user's argon ductwork pressure through liquid argon pump 107, and liquid argon 108 enters main heat exchanger E1 re-heat to be become the real argon 109 reclaiming purification to room temperature and enter user's argon pipe network；In product liquid argon 106, oxygen content general control is at below 2PPm, and the mole of product liquid argon 106 can reach in crude argon 101 more than the 92% of argon mole.
Shown in Fig. 1, rectification waste gas 112 be mainly composed of nitrogen, hydrogen and argon, the response rate of argon in how many direct reflection crude argons 101 of this portion gas amount.
Method of the present invention also includes:
Through removing the compressed air 121 of the impurity such as moisture content and carbon dioxide, enter ice chest B1, enter back into main heat exchanger E1 and be cooled into Cryogenic air 122, Cryogenic air 122 can be all gas also can contain a small amount of liquid, Cryogenic air 122 enters low-temperature fractionating tower nitrogen tower T2, wherein gas part is as the upflowing vapor of nitrogen tower T2, and liquid portion flows to the tower reactor at the bottom of tower；Upflowing vapor carries out heat and mass with the backflow counter current contacting flowed down from tower top, obtain nitrogen 123 at nitrogen tower T2 top and enter condenser/evaporator E2 nitrogen 124, nitrogen 124 is condensed into liquid portion as nitrogen tower liquid nitrogen reflux liquid 126 in condenser/evaporator E2, not coagulating portion gas is that fixed gas 127 extracts condenser/evaporator E2 discharge out, and the discharge capacity of fixed gas 127 is generally less than the 1% of compressed air 121；Liquid nitrogen reflux liquid 126 to dirty, flow to the liquid joint of tower reactor and becomes oxygen-enriched liquid air 128 with Cryogenic air 122 and extract out in the tower reactor at the bottom of nitrogen tower T2 tower through flowing to the heat and mass of upflowing vapor in nitrogen tower T2.
Described nitrogen 123 obtains side-product nitrogen 125 through main heat exchanger E1 re-heat to room temperature, and this nitrogen 125 part is as the regeneration nitrogen of argon room temperature absorbing unit, and remaining can use as plant protection gas；
Described oxygen-enriched liquid air 128 enters argon column condenser E3 after choke valve 129, the upflowing vapor 104 from argon column T1 is condensed as low-temperature receiver in condenser E3, self overwhelming majority is vaporizated into oxygen-rich steam 130, does not has evaporation section to discharge bottom condenser E3 as oxygen-enriched liquid air 131；The discharge effect of oxygen-enriched liquid air 131 is a small amount of CH preventing from containing in oxygen-enriched liquid air 1284In condenser E3 accumulation thus causing dangerous hidden danger with the heavy component such as nitrous oxide, the discharge capacity of oxygen-enriched liquid air 131 is generally the 1%～about 3% of oxygen-enriched liquid air 128 total amount；Described oxygen-enriched liquid air 131 and oxygen-rich steam 130 converge entrance main heat exchanger E1 re-heat after going out condenser E3 become room temperature oxygen-enriched air 133 to room temperature；Or oxygen-enriched liquid air 131 and oxygen-rich steam 130 enter main heat exchanger E1 respectively, go out main heat exchanger E1 respectively；Oxygen-enriched air 133 as the regeneration gas of air room temperature absorbing unit it can also be used to need the place of oxygen-enriched combusting.
The fresh liquid argon 105 of supplementary rectification institute chilling requirement can be passed directly into bottom argon column T1 of the present invention, then discharge argon column T1 with the liquid argon product reclaimed and become liquid argon product 106, fresh liquid argon 105 also can add in liquid argon 108 after liquid argon pump 107, or described fresh liquid argon 105 individually directly enters after main heat exchanger E1 carries out re-heat to individually enter argon pipe network.
Cryogenic rectification of the present invention uses double tower coupled structure, upper tower is argon column, and lower tower is nitrogen tower, and centre couples together by condenser/evaporator, rectification institute chilling requirement is provided by supplementing fresh liquid argon, produces nitrogen side-product and oxygen-enriched air side-product while reclaiming purification argon.
Embodiment:
In the argon designed for certain monocrystalline silicon production enterprise reclaims purification project, the amount of crude argon 101 is 960Nm3/ H, argon molar content～97% in crude argon 101, nitrogen and hydrogen molar content～3%, argon mole is～931.2 Nm3/H.Product liquid argon 106 yield 927 Nm3/ H, oxygen content 1.5PPm, nitrogen content 3PPm.Fresh liquid argon 127 is passed directly into bottom argon column, and fresh liquid argon 127 magnitude of recruitment is 60Nm3/ H, the argon amount reclaimed from crude argon is 867 Nm3/H.The response rate of argon is 93.1%, and the supplementary rate of fresh liquid argon is the 6.25% of crude argon.The amount of compressed air 121 is 1250 Nm3/ H, the yield of nitrogen 123 is 230 Nm3/H。
Utilizing argon organic efficiency of the present invention to can reach more than 92%, purity of argon is 1.5PPm oxygen and 3PPm nitrogen, and it is simple that rectification cold uses fresh liquid argon to supplement without the extra low system of refrigeration plant energy consumption, and can produce nitrogen side-product and secondary oxygen air side-product.

Claims (7)

1. the argon of a double tower coupling reclaims purifier apparatus, this equipment mainly includes an ice chest, one main heat exchanger, low-temperature fractionating tower and liquid argon pump, it is characterized in that described ice chest is at least provided with main heat exchanger and low-temperature fractionating tower, described low-temperature fractionating tower is the double tower coupled structure being made up of Shang Ta and lower tower, wherein go up tower be argon column, lower tower be nitrogen tower, middle be coupled by condenser/evaporator；The top of described argon column arranges condenser, and described argon column is a upper rectifying column that the crude argon rectification entering this tower can be separated into liquid argon and rectification waste gas；And described nitrogen tower is one air to be isolated nitrogen and make a part of nitrogen as side-product, another part is for the lower rectifying column of argon room temperature absorbing unit regeneration.
The argon of double tower the most according to claim 1 coupling reclaims purifier apparatus, it is characterized in that the condenser/evaporator between described argon column and nitrogen tower is to be coupled to form by the condenser as the vaporizer bottom argon column with as nitrogen top of tower, thermal source therein is the source nitrogen from nitrogen tower, low-temperature receiver is the liquid argon source from argon column, source nitrogen is in intermediate condensation, and liquid argon evaporates in outside；The thermal source of the condenser that described argon column top is arranged is the upflowing vapor from argon column, and low-temperature receiver is the throttling oxygen-enriched liquid air from nitrogen tower bottom, and wherein upflowing vapor evaporates in the outside of condenser at the intermediate condensation of condenser, throttling oxygen-enriched liquid air；Described liquid argon pump is also mounted in ice chest, and the liquid argon products export bottom described argon column connects described liquid argon pump and carries out supercharging, and accesses user's argon pipe network by the main heat exchanger re-heat in ice chest to room temperature.
The argon of double tower the most according to claim 1 and 2 coupling reclaims purifier apparatus, it is characterized in that in main heat exchanger at least provided with a crude argon cooling liquid passage, the import of this passage connects the crude argon inlet pipe entering ice chest, and outlet connects a choke valve and accesses argon column again；
One pressure-air cooling passage, the import of this passage connects the compressed air inlet pipe entering ice chest, and outlet accesses nitrogen tower；
One nitrogen re-heat passage, the import connection of this passage and the nitrogen outlet of nitrogen top of tower, the outlet of passage picks out ice chest by nitrogen tube；
One oxygen-enriched re-heat passage, the import of this passage is respectively communicated with oxygen-enriched liquid air outlet and the oxygen-rich steam outlet at argon column top, and the outlet of passage picks out ice chest by oxygen-enriched connecting tube；Or having two oxygen-enriched re-heat passages, the import of these two passages is respectively communicated with oxygen-enriched liquid air outlet and the oxygen-rich steam outlet at argon column top, and the outlet of two passages picks out ice chest by oxygen-enriched connecting tube respectively.
4. the argon recovery purifier apparatus utilizing double tower coupling described in claim 1 or 2 or 3 carries out argon recovery purification process, it is characterised in that described argon reclaims purification process and includes:
A) cooling of crude argon, first uses known technology to produce the crude argon containing only nitrogen hydrogen, and crude argon (101) enters ice chest (B1), and entering back into main heat exchanger (E1) cooling liquid is liquid argon (102)；Liquid argon (102) enters argon column (T1) after choke valve (103) throttles and carries out rectification separation；
B) crude argon rectification, crude argon carries out rectification separation according to the characteristic that component boiling point is different in argon column (T1), obtains liquid argon product (106) in argon column (T1) bottom, discharges rectification waste gas (112) at argon column (T1) top；The condenser (E3) condensation upflowing vapor (104) at argon column (T1) top, the liquid (111) of condensation is as the backflow of argon column (T1), and not solidifying gas is rectification waste gas (112), and this rectification waste gas (112) is extracted out from condenser (E3) condensation side；The liquid (111) of condensation and under choke valve (103) throttling liquid argon (102) liquid that obtains is as rectification descending liquid, lower descending liquid carries out heat and mass with the upflowing vapor counter current contacting evaporated from argon column (T1) bottom condenser/evaporator (E2), flowing to argon column (T1) bottom under thus and obtain liquid argon, upflowing vapor is from rising at the bottom of tower and converging and eventually become upflowing vapor (104) from the gas obtained through choke valve (103) throttling liquid argon (102)；A part for argon column (T1) bottom liquid argon is discharged as product liquid argon (106), and another part is condensed vaporizer (E2) evaporation as upflowing vapor；
C) the producing of argon product, product liquid argon (106) is pressurized to the liquid argon (108) of user's argon ductwork pressure through liquid argon pump (107), and liquid argon (108) enters main heat exchanger (E1) re-heat becomes real argon (109) the entrance user's argon pipe network reclaiming purification to room temperature；In product liquid argon (106), oxygen content general control is at below 2PPm, and the mole of product liquid argon (106) can reach in crude argon (101) more than the 92% of argon mole.
Argon the most according to claim 4 reclaims purification process, it is characterized in that described method also includes: through removing the compressed air (121) of the impurity such as moisture content and carbon dioxide, enter ice chest (B1), enter back into main heat exchanger (E1) and be cooled into Cryogenic air (122), Cryogenic air (122) can be all gas also can contain a small amount of liquid, Cryogenic air (122) enters low-temperature fractionating tower nitrogen tower (T2), wherein gas part is as the upflowing vapor of nitrogen tower (T2), and liquid portion flows to the tower reactor at the bottom of tower；Upflowing vapor carries out heat and mass with the backflow counter current contacting flowed down from tower top, obtain nitrogen (123) at nitrogen tower (T2) top and enter condenser/evaporator (E2) nitrogen (124), nitrogen (124) is condensed into liquid portion as nitrogen tower liquid nitrogen reflux liquid (126) in condenser/evaporator (E2), not coagulating portion gas is that fixed gas (127) extracts condenser/evaporator (E2) discharge out, and the discharge capacity of fixed gas (127) is generally less than the 1% of compressed air (121)；Liquid nitrogen reflux liquid (126) to dirty, flow to the liquid joint of tower reactor and becomes oxygen-enriched liquid air (128) with Cryogenic air (122) and extract out in the tower reactor at the bottom of nitrogen tower (T2) tower through flowing to the heat and mass of upflowing vapor in nitrogen tower (T2).
6. reclaim purification process according to the argon described in claim 5; it is characterized in that described nitrogen (123) obtains side-product nitrogen (125) through main heat exchanger (E1) re-heat to room temperature; this nitrogen (125) part is as the regeneration nitrogen of argon room temperature absorbing unit, and remaining can use as plant protection gas；
Described oxygen-enriched liquid air (128) enters argon column condenser (E3) after choke valve (129), the upflowing vapor (104) from argon column (T1) is condensed as low-temperature receiver in condenser (E3), self overwhelming majority is vaporizated into oxygen-rich steam (130), not having evaporation section to discharge from condenser (E3) bottom is oxygen-enriched liquid air (131), and the discharge capacity of oxygen-enriched liquid air (131) is generally the 1%～3% of oxygen-enriched liquid air (128) total amount；Described oxygen-enriched liquid air (131) and oxygen-rich steam (130) converge entrance main heat exchanger (E1) re-heat after going out condenser (E3) become room temperature oxygen-enriched air (133) to room temperature；Or oxygen-enriched liquid air (131) and oxygen-rich steam (130) enter main heat exchanger (E1) respectively, go out main heat exchanger (E1) respectively；Oxygen-enriched air (133) is as the regeneration gas of air room temperature absorbing unit, or is used for needing the place of oxygen-enriched combusting.
7. reclaim purification process according to the argon described in claim 4 or 6, it is characterized in that described argon column (T1) bottom can be passed directly into the fresh liquid argon (105) of supplementary rectification institute chilling requirement, then discharge argon column (T1) with the liquid argon product reclaimed and become liquid argon product (106), fresh liquid argon (105) also can be in liquid argon pump (107) add liquid argon (108) afterwards, or described fresh liquid argon (105) individually directly enters after main heat exchanger (E1) carries out re-heat to individually enter argon pipe network.
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