CN108645118A - A kind of device and method improving the argon gas rate of recovery - Google Patents

A kind of device and method improving the argon gas rate of recovery Download PDF

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Publication number
CN108645118A
CN108645118A CN201810580354.6A CN201810580354A CN108645118A CN 108645118 A CN108645118 A CN 108645118A CN 201810580354 A CN201810580354 A CN 201810580354A CN 108645118 A CN108645118 A CN 108645118A
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Prior art keywords
argon
gas
liquid
sent
argon gas
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CN201810580354.6A
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Chinese (zh)
Inventor
郝文炳
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Shanghai Union Wind Energy Technology Co Ltd
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Shanghai Union Wind Energy Technology Co Ltd
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Priority to CN201810580354.6A priority Critical patent/CN108645118A/en
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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
    • F25J3/0228—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
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    • 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
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    • F25J3/0295—Start-up or control of the process; Details of the apparatus used, e.g. sieve plates, packings
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    • F25J2270/904—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop

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

Abstract

The invention discloses a kind of device and methods improving the argon gas rate of recovery, the facility of liquid argon offer is provided using recycling scene, cold is provided with liquid argon, recycle cryogenic rectification method removing nitrogen, hydrogen, improve the rate of recovery of argon gas and the utilization rate of hydrogen, flow and the operation for simplifying cryogenic rectification, reduce operation energy consumption；Using integrated air nitrogen flow path, cold is generated by expanding machine, self-produced nitrogen in ice chest can reduce the limitation of regeneration gas, improve the recovery rate of recycling argon gas；In addition, also using the connection function of auxiliary condenser/evaporator, argon gas recycling flow path is subjected to Cooling capacity exchanging with air nitrogen flow path, the extra cold that expanding machine generates, which is transported to argon gas, recycles flow path, the liquid argon amount for reducing extraneous addition, to reduce the operation cost of equipment.

Description

A kind of device and method improving the argon gas rate of recovery
Technical field
The present invention relates to a kind of method of argon gas recycling more particularly to a kind of device and methods improving the argon gas rate of recovery.
Background technology
Vertical pulling method (Czochralski method) is to produce the main method of monocrystalline silicon, the monocrystalline in the whole world 70%~80% Silicon is produced by vertical pulling method.Most common vertical pulling method production monocrystalline silicon technique is using i.e. as vacuum technology is again as flowing atmosphere work The decompression crystal pulling technique of skill；Decompression technique is to be passed through height into single crystal growing furnace burner hearth to continuous constant speed in silicon single crystal pulling process Purity argon, while vacuum pump is constantly from the outside pump Argon of burner hearth keeps in burner hearth vacustat in 20 supports or so, this The characteristics of kind of technique existing vacuum technology, and have the characteristics of flowing atmosphere technique.The vacuum pump of decompression crystal pulling technique generally uses Slide valve pump, slide valve pump are the oil-sealed rotary pumps that sealing is kept with oil.Argon gas is produced during carrying crystal-pulling due to high temperature Raw Si oxide and impurity volatile matter, and air is discharged by pumping for vacuum pump.
By the analysis to discharging argon gas, major impurity ingredient is oxygen, nitrogen, carbon monoxide, carbon dioxide, methane Equal alkane, liquid lubricant mist；Recycling this part argon gas has very big realistic meaning.The known technology of argon gas recovery purifying： Thick oil removing, then high-precision oil removing dedusting after compressed cooling are carried out to the argon gas recycled from single crystal growing furnace；Then it is urged by high temperature Change makes the hydro carbons such as methane and carbon monoxide react production water and carbon dioxide with oxygen, ensures that oxygen is excessive (miscellaneous in catalysis reaction Oxygen is not enough then added in matter oxygen)；It is generated by making excessive oxygen be reacted with the hydrogen being added after cooling under the action of catalyst Water, and ensure to react hydrogen excess, impurity component is water, carbon dioxide, hydrogen and nitrogen in argon gas after processing；Finally pass through argon Gas room temperature absorbing unit adsorbs water and carbon dioxide, obtains the crude argon for containing only nitrogen and hydrogen is impurity.Argon gas room temperature is inhaled Coupon member is made of two absorbers, and the adsorbent equipped with absorption water and carbon dioxide in absorber a, absorber is inhaled Attached work, it includes pressure release that another absorber, which carries out, heats, blows cold reproduction operation.The gas of the reproduction operation uses nitrogen Gas, the regeneration nitrogen come from low-temperature fractionating tower production or outsourcing, argon gas room temperature absorbing unit in ice chest and are controlled by time-program(me) Device auto-controll operation switches.
In addition, publication：As patent CN102583281A discloses argon gas recovery purifying in a kind of monocrystalline silicon production Method and apparatus, cryogenic rectification part uses air cycle refrigeration, and high energy consumption, flow is complicated, and the excess hydrogen being added Emptying, utilization rate are low.As patent CN104406364A discloses a kind of the argon gas recovery purifying equipment and argon gas time of double tower coupling Purification process is received, air is used to compress, double-column process, energy consumption is and complicated without advantage, increases equipment investment.For another example Patent CN206347802U discloses a kind of device of single column cryogenic rectification recycling argon gas, for the extraneous liquid for keeping ice chest to provide Argon amount is larger, and is limited by regeneration gas, and recovery rate is relatively low；And its technical solution is served only for deoxygenation, and it is former to have not been able to removal Excess carbon monoxide in material.
Therefore, for the defect in the presence of currently available technology, those skilled in the art is dedicated to development process more Succinctly, more convenient operation, energy consumption is lower, the higher argon gas recovery method of recovery rate.
Invention content
The purpose of the present invention is be directed in present argon gas recycling the spies such as moving component is more, high energy consumption, investment is big, recovery rate is low Point has the condition of liquid argon supply using monocrystalline silicon producer, provide a kind of cryogenic rectification flow be simple and convenient to operate, energy consumption The higher device and method for improving the argon gas rate of recovery of lower and recovery rate.
To achieve the above object, the present invention uses following technical scheme：
The first aspect of the invention is to provide a kind of method improving the argon gas rate of recovery, including step：
(1) by argon gas to be recycled successively through argon gas compressor, except carbon monoxide remover, oxygen-eliminating device and argon gas precooling purification system After purified treatment, carbon monoxide, oxygen, water and the carbon dioxide in recycling argon gas are removed, dry crude argon is obtained；
(2) dry crude argon is sent into rectifying ice chest, the argon column of pure argon column bottom is sent into again after main heat exchanger cools down Device is boiled, the gas-liquid mixture fluid for going out argon column reboiler is sent into pure argon column middle and upper part participation essence by pipeline through crude argon throttle valve It evaporates, gas part rises with gas in pure argon column, and liquid portion declines with liquid in pure argon column, and obtains pure liquid argon in bottom of tower；
(3) it extracts pure liquid argon out from pure argon column bottom, argon column condenser/evaporator is sent into after pure liquid argon throttle valve reducing pressure by regulating flow Evaporation side；Pure liquid argon is evaporated to argon gas in the evaporation side of argon column condenser/evaporator, goes out after cold is recycled in main heat exchanger re-heat Rectifying ice chest is sent into pure argon user；
(4) argon gas extracted out at the top of pure argon column goes out after tower to be divided into three parts, and first part's argon gas is through main heat exchanger re-heat Argon gas precooling purification system is sent into as a regeneration gas part after recycling cold；Second part argon gas enters argon column condenser/evaporator Gas side be condensed into liquid, and flow back to pure argon column through pipeline, the liquid needed for rectifying be provided for pure argon column；Part III argon gas Enter in auxiliary condenser/evaporator through pipeline and exchange heat with partially liq air, after being condensed into liquid, with second part argon gas The liquid joint of condensation is sent into pure argon column；
(5) simultaneously, by air after air compressor compresses, be sent into air precooling purification system go water removal in air and Carbon dioxide, the air after drying enter nitrogen tower reboiler by partial liquefaction, so after the main heat exchanger cooling in rectifying ice chest It is sent into gas-liquid separator afterwards and carries out gas-liquid separation；
(6) high-purity nitrogen extracted out from nitrogen top of tower, a part are sent into the high temperature side of nitrogen tower condenser/evaporator, are cooled down Nitrogen tower is sent back to after being cooled to liquid nitrogen, and another part goes out rectifying ice chest and be sent into argon gas precooling after cold is recycled in main heat exchanger re-heat Purification system is used as regeneration gas；
(7) oxygen-rich liquid extracted out from nitrogen tower bottom is sent into nitrogen tower condenser/evaporator after pressure regulation, and is vaporizated into oxygen rich air The extraction at the top of nitrogen tower condenser/evaporator goes out rectifying ice chest after main heat exchanger re-heat and is sent into air precooling purification system, as Regeneration gas uses.
Further, in step (1), recycling argon gas carries out catalysis reaction in except carbon monoxide remover, so that in gas The content ＜ 1ppm of carbon monoxide, gas is cooled to 40 DEG C through the first cooler, and is sent into deoxygenation after being mixed with the hydrogen of addition Device reacts, and temperature rise is no more than 200 DEG C；High temperature argon after deoxygenation is sent into after the second cooler is cooled to 40 DEG C again Argon gas precooling purification system is cooled to 5-8 DEG C, and removes water and carbon dioxide.
Further, in step (3), further include：It is sent into the evaporation of argon column condenser/evaporator together from extraneous supplement liquid argon Side, to supplement the loss of refrigeration capacity in removal process.
Further, in step (5), air is compressed to 0.7-1.2MPaG through air compressor, is removed through air precooling system After removing water and carbon dioxide, it is sent into the main heat exchanger entered in rectifying ice chest, is cooled to -160 DEG C to -170 DEG C.
Further, in step (5), after the liquid in gas-liquid separator after gas-liquid separation is flowed out from bottom, a part is sent Enter nitrogen tower, another part is sent into auxiliary condenser/evaporator, cold is provided for it, with the gas at the top of the pure argon column that liquefies out, quilt It is sent into nitrogen tower bottom after the gas of vaporization and the gas mixing at the top of gas-liquid separator out and participates in rectifying, and on pure argon column top Portion obtains high-purity nitrogen, and oxygen-rich liquid is obtained in pure argon column bottom.
Further, in step (7), the oxygen rich air extracted out at the top of nitrogen tower condenser/evaporator, first through main heat exchanger re-heat It is sent into expanding machine afterwards and carries out swell refrigeration, goes out the oxygen rich air after expanding machine and enters again from the low temperature side of main heat exchanger, after re-heat Go out rectifying ice chest and is sent into air precooling purification system.
The second aspect of the invention is to provide a kind of device of the raising argon gas rate of recovery for the method, specific to wrap It includes：Purification system, air compressor, air precooling purifying system are pre-chilled except carbon monoxide remover, oxygen-eliminating device, argon gas for argon gas compressor System and rectifying ice chest, the rectifying ice chest have been built-in with main heat exchanger, pure argon column and nitrogen tower, and the pure argon column bottom is equipped with argon column Reboiler, top are equipped with argon column condenser/evaporator, and the nitrogen tower bottom is equipped with nitrogen tower reboiler, top is equipped with nitrogen tower condensation evaporation Device, wherein：
The argon gas compressor, except carbon monoxide remover, oxygen-eliminating device and argon gas precooling purification system be sequentially communicated, for return It receives argon gas and carries out purified treatment, to remove the carbon monoxide, oxygen, water and the carbon dioxide that recycle in argon gas；
The argon gas precooling purification system is connected to through the main heat exchanger with the argon column reboiler by pipeline, the argon Tower reboiler is connected to the pure argon column middle and upper part by pipeline through crude argon throttle valve, and crude argon is sent into the pure argon column internal reference With rectifying；
The bottom of the pure argon column is connected to the evaporation side of the argon column condenser/evaporator by pipeline through pure liquid argon throttle valve, And the evaporation side of the argon column condenser/evaporator goes out the rectifying ice chest through the main heat exchanger by pipeline and connects pure argon use Family；The argon gas precooling purification system is connected through the main heat exchanger by pipeline respectively at the top of the pure argon column, passes through pipeline Through being connected to forming circuit at the top of the argon column condenser/evaporator and the pure argon column, by pipeline through assisting condenser/evaporator and institute State connection forming circuit at the top of pure argon column；
The air compressor passes sequentially through pipeline through the air precooling purification system, main heat exchanger and nitrogen tower reboiler Connect the gas-liquid separator of tower body side, the gas-liquid separator bottom respectively by pipeline connect the nitrogen tower middle and lower part, The middle and lower part of the nitrogen tower is connected through the auxiliary condenser/evaporator by pipeline, passes through pipeline at the top of the gas-liquid separator The middle and lower part for connecting the nitrogen tower, by the gas of the gas-liquid separator separates and after auxiliary condenser/evaporator vaporization Gas be sent into the nitrogen tower, provide the gas needed for rectifying for the nitrogen tower；
The nitrogen top of tower connects the argon gas precooling purification system through the main heat exchanger by pipeline respectively, passes through pipe Road is connected to forming circuit through the nitrogen tower condenser/evaporator with the nitrogen top of tower；Described in the nitrogen tower bottom is connected by pipeline The evaporation side of nitrogen tower condenser/evaporator, low-temperature receiver is provided for it；And the evaporation side of the nitrogen tower condenser/evaporator by pipeline successively The air precooling purification system is connected through the main heat exchanger, expanding machine, main heat exchanger, for being purified for the air precooling System provides dry gas.
Further, the evaporation side of the argon column condenser/evaporator is by argon source outside plumbing connection system, outside the system Argon source is used to supplement the loss of refrigeration capacity in removal process.
Further, it is provided with the first cooler on the pipeline except between carbon monoxide remover and the oxygen-eliminating device, and Hydrogen Line is accessed on pipeline between first cooler and the oxygen-eliminating device；The oxygen-eliminating device is pre-chilled with the argon gas The second cooler is provided on pipeline between purification system.
Further, the argon gas precooling purification system and the air precooling purification system are by a precooler and two The purifier composition that platform is arranged in parallel.
The present invention is had the following technical effect that compared with prior art using above-mentioned technical proposal：
The device and method of the raising argon gas rate of recovery of the present invention, the facility of liquid argon offer is had using recycling scene, is used Liquid argon provides cold, recycles cryogenic rectification method removing nitrogen, hydrogen, improves the rate of recovery of argon gas and the utilization rate of hydrogen, Flow and the operation for simplifying cryogenic rectification, reduce operation energy consumption；Using integrated air nitrogen flow path, produced by expanding machine Raw food is measured, and self-produced nitrogen in ice chest can reduce the limitation of regeneration gas, improve the recovery rate of recycling argon gas；In addition, cold using assisting The connection function of solidifying evaporator, argon gas recycling flow path have carried out Cooling capacity exchanging with air nitrogen flow path, expanding machine are generated more Waste cold amount is transported to argon gas recycling flow path, can significantly reduce the liquid argon amount of extraneous addition, to reduce the operation of equipment at This.
Description of the drawings
Fig. 1 is a kind of flow diagram for the device improving the argon gas rate of recovery of the present invention；
Wherein, each reference numeral is：
1- argon gas compressor, 2- are except carbon monoxide remover, the first coolers of 3-, 4- oxygen-eliminating devices, 5- the second cooler I, 6- argons Gas be pre-chilled purification system, 7- rectifying ice chest, 8- main heat exchangers, 9- argon columns reboiler, 10- pure argon columns, the thick liquid argon throttle valves of V2-, The pure liquid argon throttle valves of V1-, 11- argon columns condenser/evaporator, 12- auxiliary condenser/evaporator, 13- gas-liquid separators, 14- nitrogen towers boil again Device, 15- nitrogen tower, 16- nitrogen towers condenser/evaporator, 17- air compressors, 18- air precoolings purification system, 19- expanding machines.
Specific implementation mode
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention, But following embodiments are not intended to limit the scope of the invention.
Embodiment 1
As shown in Figure 1, present embodiments providing a kind of device improving the argon gas rate of recovery, specifically include：Argon gas compressor 1, carbon monoxide remover 2, oxygen-eliminating device 4, argon gas precooling purification system 6, air compressor 17, air precooling purification system 18 and essence are removed Ice chest 7 is evaporated, the rectifying ice chest 7 has been built-in with main heat exchanger 8, pure argon column 10 and nitrogen tower 15, and 10 bottom of the pure argon column is equipped with Argon column reboiler 9, top are equipped with argon column condenser/evaporator 11, and 15 bottom of nitrogen tower is equipped with nitrogen tower reboiler 14, top is equipped with Nitrogen tower condenser/evaporator 16, wherein：
The argon gas compressor 1, except carbon monoxide remover 2, oxygen-eliminating device 4 and argon gas precooling purification system 6 be sequentially communicated, be used for Purified treatment is carried out to recycling argon gas, to remove the carbon monoxide, oxygen, water and the carbon dioxide that recycle in argon gas；
The argon gas precooling purification system 6 is connected to through the main heat exchanger 8 with the argon column reboiler 9 by pipeline, institute State argon column reboiler 9 and 10 middle and upper part of pure argon column be connected to through crude argon throttle valve V2 by pipeline, crude argon is sent into described in Rectifying is participated in pure argon column 10；
The bottom of the pure argon column 10 is connected to the argon column condenser/evaporator 11 by pipeline through pure liquid argon throttle valve V1 Evaporation side, and the evaporation side of the argon column condenser/evaporator 11 goes out the rectifying ice chest 7 through the main heat exchanger 8 by pipeline and connects Meet pure argon user；10 top of the pure argon column connects the argon gas precooling purifying by pipeline through the main heat exchanger 8 respectively System 6 is connected to forming circuit with 10 top of the pure argon column through the argon column condenser/evaporator 11 by pipeline, is passed through by pipeline Auxiliary condenser/evaporator 12 is connected to forming circuit with 10 top of the pure argon column；
The air compressor 17 passes sequentially through pipeline through the air precooling purification system 18, main heat exchanger 8 and nitrogen tower Reboiler 14 connects the gas-liquid separator 13 of tower body side, and 13 bottom of the gas-liquid separator connects the nitrogen by pipeline respectively The middle and lower part of tower 15, the middle and lower part for connecting the nitrogen tower 15 through the auxiliary condenser/evaporator 12 by pipeline, the gas-liquid point Top from device 13 connects the middle and lower part of the nitrogen tower 15, the gas and warp that the gas-liquid separator 13 is detached by pipeline Gas after the auxiliary condenser/evaporator 12 vaporizes is sent into the nitrogen tower 15, and the gas needed for rectifying is provided for the nitrogen tower 15 Body；
15 top of the nitrogen tower connects the argon gas precooling purification system 6 through the main heat exchanger 8 by pipeline respectively, leads to Piping is connected to forming circuit through the nitrogen tower condenser/evaporator 16 with 15 top of the nitrogen tower；15 bottom of nitrogen tower passes through pipe Road connects the evaporation side of the nitrogen tower condenser/evaporator 16, and low-temperature receiver is provided for it；And the evaporation of the nitrogen tower condenser/evaporator 16 Side connects the air precooling purification system 18 through the main heat exchanger 8, expanding machine 19, main heat exchanger 8 successively by pipeline, uses In providing dry gas for the air precooling purification system 18.
In the present embodiment, the evaporation side of the argon column condenser/evaporator 11 is described by argon source outside plumbing connection system The outer argon source of system is used to supplement the loss of refrigeration capacity in removal process.
In the present embodiment, it is provided with the first cooling on the pipeline except between carbon monoxide remover 2 and the oxygen-eliminating device 4 Device 3, and access Hydrogen Line on the pipeline between first cooler 3 and the oxygen-eliminating device 4；The oxygen-eliminating device 4 and institute It states and is provided with the second cooler 5 on the pipeline between argon gas precooling purification system 6.
In the present embodiment, the argon gas precooling purification system 6 and the air precooling purification system 18 are pre- by one The purifier composition that cold and Liang Tai are arranged in parallel.
Embodiment 2
A kind of method improving the argon gas rate of recovery is present embodiments provided, it is specific to wrap with reference to flow chart as shown in Figure 1 Include following steps：
(1) by argon gas to be recycled successively through argon gas compressor 1, except carbon monoxide remover 2, oxygen-eliminating device 4 and argon gas precooling purifying After 6 purified treatment of system, carbon monoxide, oxygen, water and the carbon dioxide in recycling argon gas are removed, dry crude argon is obtained；
(2) dry crude argon is sent into rectifying ice chest 7, the argon of 10 bottom of pure argon column is sent into after the cooling of main heat exchanger 8 Tower reboiler 9, the gas-liquid mixture fluid for going out argon column reboiler 9 are sent into through crude argon throttle valve V2 in pure argon column 10 by pipeline Portion participates in rectifying, and gas part rises with gas in pure argon column 10, and liquid portion declines with liquid in pure argon column 10, and in bottom of tower Obtain pure liquid argon；
(3) it extracts pure liquid argon out from 10 bottom of pure argon column, argon column condensation is sent into after pure liquid argon throttle valve V1 reducing pressure by regulating flow and is steamed Send out the evaporation side of device 11；Pure liquid argon is evaporated to argon gas in the evaporation side of argon column condenser/evaporator 11, is recycled through 8 re-heat of main heat exchanger Go out rectifying ice chest 7 after cold and is sent into pure argon user；
(4) argon gas extracted out from 10 top of pure argon column goes out after tower to be divided into three parts, and first part's argon gas is multiple through main heat exchanger 8 Argon gas precooling purification system 6 is sent into after recuperation of heat cold as a regeneration gas part；Second part argon gas enters argon column condensation and steams The gas side of hair device 11 is condensed into liquid, and flows back to pure argon column 10 through pipeline, and the liquid needed for rectifying is provided for pure argon column 10；The Three parts argon gas enters through pipeline in auxiliary condenser/evaporator 12 to exchange heat with partially liq air, after being condensed into liquid, with The liquid joint of second part argon gas condensation is sent into pure argon column 10；
(5) simultaneously, it by air after the compression of air compressor 17, is sent into air precooling purification system 18 and goes removing in air Water and carbon dioxide, the air after drying enter nitrogen tower reboiler 14 by part after the main heat exchanger 8 in rectifying ice chest 7 cools down Liquefaction is then fed into gas-liquid separator 13 and carries out gas-liquid separation；
(6) high-purity nitrogen extracted out from 15 top of nitrogen tower, a part are sent into the high temperature side of nitrogen tower condenser/evaporator 16, quilt For cooling down to send nitrogen tower 15 after liquid nitrogen back to, another part goes out the feeding of rectifying ice chest 7 after cold is recycled in 8 re-heat of main heat exchanger Purification system 6 is pre-chilled in argon gas, is used as regeneration gas；
(7) oxygen-rich liquid extracted out from 15 bottom of nitrogen tower is sent into nitrogen tower condenser/evaporator 16 after pressure regulation, and is vaporizated into richness Oxygen goes out rectifying ice chest 7 after 8 re-heat of main heat exchanger and is sent into air precooling purifying system from the 16 top extraction of nitrogen tower condenser/evaporator System 18, uses as regeneration gas.
In the present embodiment, in step (1), recycling argon gas carries out catalysis reaction in except carbon monoxide remover 2, so that gas In carbon monoxide content ＜ 1ppm, gas is cooled to 40 DEG C through the first cooler 3, and is sent into after being mixed with the hydrogen of addition Oxygen-eliminating device 4 reacts, and temperature rise is no more than 200 DEG C；High temperature argon after deoxygenation is cooled to 40 DEG C through the second cooler 5 again It is sent into argon gas precooling purification system 6 afterwards and is cooled to 5-8 DEG C, and removes water and carbon dioxide.
In the present embodiment, in step (3), further include：From the external world, supplement liquid argon is sent into argon column condenser/evaporator 11 together Evaporation side, to supplement the loss of refrigeration capacity in removal process.
In the present embodiment, in step (5), air is compressed to 0.7-1.2MPaG through air compressor 17, through air precooling After system 18 removes water and carbon dioxide, it is sent into the main heat exchanger 8 entered in rectifying ice chest 7, is cooled to -160 DEG C to -170 DEG C.
In the present embodiment, in step (5), after the liquid in gas-liquid separator 13 after gas-liquid separation is flowed out from bottom, one Nitrogen tower 15 is sent into part, and another part is sent into auxiliary condenser/evaporator 12, cold is provided for it, and to liquefy, 10 top of pure argon column goes out The gas come, the gas being vaporized participate in essence with from 15 bottom of feeding nitrogen tower after the gas mixing that 13 top of gas-liquid separator comes out It evaporates, and high-purity nitrogen is obtained at 10 top of pure argon column, oxygen-rich liquid is obtained in 10 bottom of pure argon column.
In the present embodiment, in step (7), the oxygen rich air extracted out from 16 top of nitrogen tower condenser/evaporator, first through main heat exchange After 8 re-heat of device be sent into expanding machine 19 carry out swell refrigeration, go out the oxygen rich air after expanding machine 19 again from the low temperature side of main heat exchanger 8 into Enter, rectifying ice chest 7 is gone out after re-heat and is sent into air precooling purification system 18.
Embodiment 3
A kind of application for the device improving the argon gas rate of recovery using the present invention is present embodiments provided, please continue to refer to such as figure Process flow chart shown in 1, main argon gas recycling flow path and air nitrogen recycling flow path two parts：
(1) argon gas recycles flow path：
Argon gas (O to be recycled2<~0.8%, N2<~4%, CO：~1000ppm, remaining is Ar) pressure it is very low, pass through first Cross argon gas compressor 1 be forced into~1.0MPa after, after removing oil removing and dust, through piping GAr-101 enter remove carbon monoxide remover 2.The loading catalyst in except carbon monoxide remover 2 is reacted by being catalyzed, and is carbon dioxide catalyzing carbon monoxide.The outlets CO contain Amount<1ppm.The argon gas of removal CO through piping GAr-102 pipelines is cooled to about 40 DEG C after coming out into the first cooler 3, in pipe Enter oxygen-eliminating device 4 after being mixed with the hydrogen of addition in road GAr-103, in oxygen-eliminating device 4, oxygen reacts with hydrogen, generates Water simultaneously discharges heat, and difference is had depending on amount of oxygen temperature rise, and when O2 contents are not higher than 0.8%, temperature can be<200℃.It is logical Piping GA-104 high temperature argons are cooled to 40 DEG C into the second cooler 5, enter argon gas precooling purifying by pipeline GAr-105 Argon gas precooler in system 6 is cooled to 5-8 DEG C and purifier removes water and carbon dioxide.Remaining argon gas is mainly： Ar、N2、H2Deng.
Dry crude argon enters rectifying ice chest 7 by pipeline GAr-106, initially enters main heat exchanger 8 and is cooled to liquefaction Point, it is most of in argon column reboiler 9 into the argon column reboiler 9 for being built in 10 bottom of pure argon column through piping GAr-107 Gas (80%~95%) is liquefied, and the gas-liquid mixture fluid for going out argon column reboiler 9 is flowed out from GAr-108, through crude argon throttle valve V2 reducing pressure by regulating flow is sent into 10 middle and upper part of pure argon column and participates in rectifying.The operating pressure of argon column reboiler 9 is about 0.95MPaG, pure argon column 10 pressure is 0.7MPaG since there are pressure difference, medium boiling temperature can make according to pressure change inside and outside argon column reboiler 9 Side forms about 1~1.5 DEG C of the temperature difference, ensures the heat exchange of argon column reboiler 9.
Into the fluid of pure argon column 10, gas part therein is with gas rising in tower, and liquid is under liquid in tower Drop, heat and mass transfer process occurs for gas-liquid in ascending and descending process, and the Ar contents of liquid portion are higher and higher, obtained in bottom of tower pure Liquid argon (depending on national standard or customer requirement, routinely can reach N2<4ppm).It is taken out from rectifier bottoms by LARS-201 pipelines Go out the evaporation side that pure liquid argon is sent into argon column condenser/evaporator 11 through pure liquid argon throttle valve V1 reducing pressure by regulating flow.External world's supplement liquid argon passes through Pipeline LAr-305 enters the evaporation side of condenser/evaporator 11 together, and loss of refrigeration capacity is supplemented for whole system.Pure liquid argon is cold in argon column Solidifying 11 evaporation side of evaporator is evaporated to argon gas, recycles cold by main heat exchanger re-heat, sends out rectifying ice chest, can be according to user's need It asks pressurization or directly supplies gas.The operating pressure of argon column condenser/evaporator 11 is related with process organization, is in 10 pressure of pure argon column When~0.7MPaG, pressure is about 0.35~0.37MPaG.If cooling box pressure requirements reduce, the pressure of whole system is (containing essence The pressure of argon column 10 and argon gas compressor 1) operation can be reduced.
The gas at 10 top of pure argon column is mainly hydrogen and nitrogen, is divided into three parts after going out tower from pipeline GAr-301 pipelines, A part is extracted out from pipeline GAr-302, through 8 re-heat of main heat exchanger to room temperature, is generally recycled with 1.5~3 DEG C lower than intake air temperature It is sent out outside tower after cold, a regeneration gas part for purification system 6 is pre-chilled as argon gas, the nitrogen come out with rectifying ice chest 7 is together It regenerates and uses for purifier.The second part gas of tower top enters the gas side condensation of argon column condenser/evaporator 11 by GAr-301 For liquid, pure argon column 10 is flowed back to by LAr-306, liquid is provided for rectifying.Part III gas enters auxiliary by GAr-304 Condenser/evaporator 12 exchanges heat with part liquid air, after being condensed into liquid, enters LAr-306 and second part by LAr-305 Pure argon column 10 is sent into after liquid joint.
(2) air nitrogen flow path：
Air is compressed to 0.7~1.2MPaG by air compressor machine 17, enters air precooling purification system 18 by GA-101, Remove water removal and carbon dioxide.In GAr-102 be it is dry after air, cool down into the main heat exchanger 8 in rectifying ice chest 7, In GA-103, the micro band liquid of air, temperature is -160~-170 DEG C.Cryogenic air enters nitrogen tower reboiler 14 by partial liquefaction, Enter gas-liquid separator 13 after out.In gas-liquid separator 13, liquid is divided into two strands after bottom LA-105 outflows, one LA-105 is sent directly into nitrogen tower 15.Another gang of LA-106 is sent into auxiliary condenser/evaporator 12, and cold is provided for it, and liquefy pure argon column The gas GAr-304 of 10 tops out, the gas after itself being vaporized pass through GA-107 and the gas from gas-liquid separator 13 out It is sent into 15 bottom of nitrogen tower after body GA-108 mixing, the rectifying for nitrogen tower 15 provides gas.
In the polylith column plate of nitrogen tower 15 (or filler) contacts uprising gas with dropping liq, heavy constituent (oxygen, argon Gas) it can gather in a liquid, light component (mainly nitrogen) can be gathered in gas, be finally to obtain high-purity nitrogen in tower top (oxygen content is<1ppm), the liquid of bottom of tower becomes oxygen rich air because of the increase of liquid oxygen content (oxygen content is about 30%~40%).Nitrogen The pressure of tower is 0.6~0.8MPaG, and temperature is the boiling point of liquid under the pressure.After 15 tower top of nitrogen tower extracts nitrogen out, it is divided into two Stock, one GN-301 are sent into the high temperature side of nitrogen tower condenser/evaporator 16, are to send nitrogen back to by LN-302 after liquid nitrogen by cooling down Tower participates in the rectifying of nitrogen tower 15 as the liquid of decline.Another gang of GN-302, after cold is recycled in 8 re-heat of main heat exchanger, Rectifying ice chest 7 is sent out, Argon Purifier 6 is sent into, is used as regeneration gas.
It is cold to be sent into nitrogen tower after throttle valve V6 adjusts pressure for the oxygen-enriched liquid air that the bottom of nitrogen tower 15 is extracted out by LA-201 Solidifying evaporator 16, provides low-temperature receiver for it, itself is vaporizated into oxygen rich air and goes out nitrogen tower condenser/evaporator 16, enter master through GRO-202 Heat exchanger 8.After re-heat, it is -145~-155 DEG C from 8 middle part extraction temperature of main heat exchanger, expanding machine is sent by GRO-203 19, make full use of residual compression (about 0.2~0.3MPaG) swell refrigeration of oxygen rich air.Go out the oxygen rich air after expanding machine 19 from After low temperature side enters 8 re-heat to room temperature of main heat exchanger, rectifying ice chest 7 is sent out.It is delivered to air precooling purification system 18, as dry Pathogenic dryness body participates in the regeneration of purifier.
The present embodiment utilizes the connection function of auxiliary condenser/evaporator 12, argon gas recycling flow path (GAr-304, LAr-305) Cooling capacity exchanging has been carried out with air nitrogen flow path (LA-306, GA-107), the extra cold that expanding machine 19 generates is transported to argon Gas recycles flow path, the liquid argon amount of extraneous addition can be significantly reduced, to reduce the operation cost of equipment.
Specific embodiments of the present invention are described in detail above, but it is intended only as example, the present invention is simultaneously unlimited It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and It substitutes also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by impartial conversion and Modification, all should be contained within the scope of the invention.

Claims (10)

1. a kind of method improving the argon gas rate of recovery, which is characterized in that including step：
(1) by argon gas to be recycled successively through argon gas compressor (1), except carbon monoxide remover (2), oxygen-eliminating device (4) and argon gas be pre-chilled it is pure After change system (6) purified treatment, carbon monoxide, oxygen, water and the carbon dioxide in recycling argon gas are removed, dry crude argon is obtained；
(2) dry crude argon is sent into rectifying ice chest (7), pure argon column (10) bottom is sent into after main heat exchanger (8) cooling Argon column reboiler (9), the gas-liquid mixture fluid for going out argon column reboiler (9) are sent into smart argon by pipeline through crude argon throttle valve (V2) Tower (10) middle and upper part participates in rectifying, and gas part rises with the interior gas of pure argon column (10), and liquid portion is with pure argon column (10) interior liquid Body declines, and obtains pure liquid argon in bottom of tower；
(3) it extracts pure liquid argon out from pure argon column (10) bottom, argon column condensation is sent into after pure liquid argon throttle valve (V1) reducing pressure by regulating flow and is steamed Send out the evaporation side of device (11)；Evaporation side of the pure liquid argon in argon column condenser/evaporator (11) is evaporated to argon gas, multiple through main heat exchanger (8) Go out rectifying ice chest (7) after recuperation of heat cold and is sent into pure argon user；
(4) argon gas extracted out at the top of pure argon column (10) goes out after tower to be divided into three parts, and first part's argon gas is multiple through main heat exchanger (8) Argon gas precooling purification system (6) is sent into after recuperation of heat cold as a regeneration gas part；Second part argon gas enters argon column condensation The gas side of evaporator (11) is condensed into liquid, and flows back to pure argon column (10) through pipeline, is provided needed for rectifying for pure argon column (10) Liquid；Part III argon gas enters through pipeline in auxiliary condenser/evaporator (12) to exchange heat with partially liq air, condenses After liquid, pure argon column (10) is sent into the liquid joint of second part argon gas condensation；
(5) simultaneously, it by air after air compressor (17) compression, is sent into air precooling purification system (18) and goes removing in air Water and carbon dioxide, the air after drying enter nitrogen tower reboiler (14) after main heat exchanger (8) cooling in rectifying ice chest (7) By partial liquefaction, it is then fed into gas-liquid separator (13) and carries out gas-liquid separation；
(6) high-purity nitrogen extracted out at the top of nitrogen tower (15), a part are sent into the high temperature side of nitrogen tower condenser/evaporator (16), quilt For cooling down to send nitrogen tower (15) after liquid nitrogen back to, another part goes out rectifying ice chest after cold is recycled in main heat exchanger (8) re-heat (7) it is sent into argon gas precooling purification system (6), is used as regeneration gas；
(7) oxygen-rich liquid extracted out from nitrogen tower (15) bottom is sent into nitrogen tower condenser/evaporator (16) after pressure regulation, and is vaporizated into richness Oxygen is extracted out at the top of nitrogen tower condenser/evaporator (16), and rectifying ice chest (7) is gone out after main heat exchanger (8) re-heat and is sent into air precooling Purification system (18), uses as regeneration gas.
2. the method according to claim 1 for improving the argon gas rate of recovery, which is characterized in that in step (1), recycling argon gas exists Except catalysis reaction is carried out in carbon monoxide remover (2), so that the content ＜ 1ppm of the carbon monoxide in gas, gas is through the first cooling Device (3) is cooled to 40 DEG C, and is sent into oxygen-eliminating device (4) after being mixed with the hydrogen of addition and reacts, and temperature rise is no more than 200 ℃；High temperature argon after deoxygenation is sent into argon gas precooling purification system (6) again after the second cooler (5) is cooled to 40 DEG C and is cooled to 5-8 DEG C, and remove water and carbon dioxide.
3. the method according to claim 1 for improving the argon gas rate of recovery, which is characterized in that in step (3), further include：From External world's supplement liquid argon is sent into the evaporation side of argon column condenser/evaporator (11) together, to supplement the loss of refrigeration capacity in removal process.
4. the method according to claim 1 for improving the argon gas rate of recovery, which is characterized in that in step (5), air is through air Compressor (17) is compressed to 0.7-1.2MPaG, after air precooling system (18) removes water and carbon dioxide, is sent into and enters rectifying Main heat exchanger (8) in ice chest (7), is cooled to -160 DEG C to -170 DEG C.
5. the method according to claim 1 for improving the argon gas rate of recovery, which is characterized in that in step (5), gas-liquid separator (13) after the liquid after interior gas-liquid separation is flowed out from bottom, a part is sent into nitrogen tower (15), and another part is sent into auxiliary condensation and is steamed Send out device (12), cold provided for it, with the gas at the top of the pure argon column that liquefies (10) out, the gas being vaporized with from gas-liquid separation It is sent into nitrogen tower (15) bottom after gas mixing at the top of device (13) out and participates in rectifying, and obtains at the top of pure argon column (10) high-purity Nitrogen is spent, oxygen-rich liquid is obtained in pure argon column (10) bottom.
6. the method according to claim 1 for improving the argon gas rate of recovery, which is characterized in that in step (7), condensed from nitrogen tower The oxygen rich air extracted out at the top of evaporator (16) is first sent into expanding machine (19) after main heat exchanger (8) re-heat and carries out swell refrigeration, goes out Oxygen rich air after expanding machine (19) enters from the low temperature side of main heat exchanger (8) again, and rectifying ice chest (7) is gone out after re-heat and is sent into air Purification system (18) is pre-chilled.
7. a kind of device of raising argon gas rate of recovery for any one of claim 1-6 the methods, which is characterized in that packet It includes：Argon gas compressor (1) removes carbon monoxide remover (2), oxygen-eliminating device (4), argon gas precooling purification system (6), air compressor (17), air precooling purification system (18) and rectifying ice chest (7), the rectifying ice chest (7) have been built-in with main heat exchanger (8), essence Argon column (10) and nitrogen tower (15), pure argon column (10) bottom is equipped with argon column reboiler (9), top is equipped with argon column condenser/evaporator (11), nitrogen tower (15) bottom is equipped with nitrogen tower reboiler (14), top is equipped with nitrogen tower condenser/evaporator (16), wherein：
The argon gas compressor (1) is pre-chilled purification system (6) and is sequentially communicated except carbon monoxide remover (2), oxygen-eliminating device (4) and argon gas, For carrying out purified treatment to recycling argon gas, to remove the carbon monoxide, oxygen, water and the carbon dioxide that recycle in argon gas；
The argon gas precooling purification system (6) is connected to through the main heat exchanger (8) with the argon column reboiler (9) by pipeline, The argon column reboiler (9) is connected to pure argon column (10) middle and upper part by pipeline through crude argon throttle valve (V2), by crude argon It is sent into the pure argon column (10) and participates in rectifying；
The bottom of the pure argon column (10) is connected to the argon column condenser/evaporator (11) by pipeline through pure liquid argon throttle valve (V1) Evaporation side, and the evaporation side of the argon column condenser/evaporator (11) goes out the rectifying by pipeline through the main heat exchanger (8) Ice chest (7) connects pure argon user；Respectively by pipeline through described in the main heat exchanger (8) connection at the top of the pure argon column (10) Argon gas precooling purification system (6) is connected to by pipeline through the argon column condenser/evaporator (11) and the pure argon column (10) top Forming circuit is connected to forming circuit through assisting by pipeline at the top of condenser/evaporator (12) and the pure argon column (10)；
The air compressor (17) passes sequentially through pipeline through the air precooling purification system (18), main heat exchanger (8) and nitrogen Tower reboiler (14) connects the gas-liquid separator (13) of tower body side, and gas-liquid separator (13) bottom is connected by pipeline respectively Under connecing the middle and lower part of the nitrogen tower (15), being connected in the nitrogen tower (15) through the auxiliary condenser/evaporator (12) by pipeline Portion, the top of the gas-liquid separator (13) connects the middle and lower part of the nitrogen tower (15) by pipeline, by the gas-liquid separation The gas of device (13) separation and the gas after the auxiliary condenser/evaporator (12) vaporizes are sent into the nitrogen tower (15), are described Nitrogen tower (15) provides the gas needed for rectifying；
At the top of the nitrogen tower (15) respectively by pipeline through the main heat exchanger (8) connect the argon gas be pre-chilled purification system (6), By pipeline through being connected to forming circuit at the top of the nitrogen tower condenser/evaporator (16) and the nitrogen tower (15)；Nitrogen tower (15) bottom Portion connects the evaporation side of the nitrogen tower condenser/evaporator (16) by pipeline, and low-temperature receiver is provided for it；And the nitrogen tower condensation evaporation The evaporation side of device (16) connects the sky through the main heat exchanger (8), expanding machine (19), main heat exchanger (8) successively by pipeline Purification system (18) is pre-chilled in gas, for providing dry gas for the air precooling purification system (18).
8. the device according to claim 7 for improving the argon gas rate of recovery, which is characterized in that the argon column condenser/evaporator (11) evaporation side is used to supplement the cold damage in removal process by argon source outside plumbing connection system, the outer argon source of the system It loses.
9. the device according to claim 7 for improving the argon gas rate of recovery, which is characterized in that described to remove carbon monoxide remover (2) It is provided with the first cooler (3) on pipeline between the oxygen-eliminating device (4), and is removed with described in first cooler (3) Hydrogen Line is accessed on pipeline between oxygen device (4)；Between the oxygen-eliminating device (4) and argon gas precooling purification system (6) The second cooler (5) is provided on pipeline.
10. the device according to claim 7 for improving the argon gas rate of recovery, which is characterized in that the argon gas precooling purifying system System (6) and the air precooling purification system (18) are made of a precooler and the Liang Tai purifier being arranged in parallel.
CN201810580354.6A 2018-06-07 2018-06-07 A kind of device and method improving the argon gas rate of recovery Pending CN108645118A (en)

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CN110207460A (en) * 2019-07-10 2019-09-06 上海联风能源科技有限公司 A kind of recyclable device and its recovery method of integrated High Purity Nitrogen and argon gas
CN110207462A (en) * 2019-07-10 2019-09-06 上海联风能源科技有限公司 A kind of recovery system and recovery method of integrated high pure nitrogen and argon gas
CN110542279A (en) * 2019-09-10 2019-12-06 苏州市兴鲁空分设备科技发展有限公司 argon tail gas recovery and purification device containing methane and hydrocarbon
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