CN107606874A - A kind of device of Full distillation purification recovery argon gas and its method for reclaiming argon gas - Google Patents
A kind of device of Full distillation purification recovery argon gas and its method for reclaiming argon gas Download PDFInfo
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- CN107606874A CN107606874A CN201711014301.XA CN201711014301A CN107606874A CN 107606874 A CN107606874 A CN 107606874A CN 201711014301 A CN201711014301 A CN 201711014301A CN 107606874 A CN107606874 A CN 107606874A
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Abstract
The present invention relates to the device that a kind of Full distillation purifies recovery argon gas, it includes crude argon purification recovery system and the argon gas circulatory system, crude argon purification recovery system includes feed gas compressor group, main heat exchanger, deoxidation tower, pure argon column, subcooler, the argon gas circulatory system includes cycle compressor unit and expanding machine, and each equipment is attached by respective line；The argon gas circulatory system provides low temperature not argon gas liquefaction offer cold for ice chest；The invention further relates to the method using said apparatus recovery argon gas, it includes the supercharging cooling of crude argon and the rectification and purification of crude argon, oxygen content ＜ 1.5ppm, nitrogen content ＜ 4ppm in obtained high liquid nitrogen.The present invention provides cold by circulator, while argon gas is purified, also argon gas is liquefied, compensate for the deficiency of the supporting space division of coal chemical industry；And pass through reasonable disposition heat exchange process so that energy utilization optimizes, and reduces the loss of cold, farthest reclaims argon gas, reduces and wastes, has certain economic benefit.
Description
Technical field
The present invention relates to gas separation technique field, more particularly to a kind of purification of Full distillation to reclaim the device of argon gas and its return
The method for receiving argon gas.
Background technology
Argon gas is a kind of inert gas of no color or smell, and its molecular formula is Ar, molecular weight 39.95, and vapour pressure is
202.64kPa (- 179 DEG C), -189.2 DEG C of fusing point, -185.7 DEG C of boiling point.In the industrial production, argon gas is often used as a kind of height
The protective gas of effect, use are quite varied.
The main source of argon gas is that byproduct output is used as from big space division.Typically had in the supporting space division of steel plant
Pure argon produces.But in the air separation plant that coal chemical industry technique uses, because coal chemical industry technique does not need argon gas in itself, so matching somebody with somebody
Set space division does not produce pure argon typically, this space division can supporting synergy tower, the crude argon that synergy top of tower comes out, typically amount containing argon is
85%, it is oxygen that remaining is most of, and few part is nitrogen, without other impurity.This part crude argon can be directly vented, and be caused
Waste.
The content of the invention
It is the defects of the invention reside in overcoming in the prior art, entirely smart with low temperature for the supporting space division feature of coal chemical industry, exploitation
The Methods For Purification crude argon evaporated obtains pure argon, accurately says it is to obtain pure liquid argon, and it specifically provides a kind of Full distillation purification
The device and its recovery argon gas method of argon gas are reclaimed, is wasted with reducing.
To achieve the above object, the present invention adopts the following technical scheme that：
First purpose of the present invention is to provide a kind of device of Full distillation purification recovery argon gas, and it includes：Crude argon air lift
Pure recovery system, it is included by the feed gas compressor group of pipeline connection, main heat exchanger, deoxidation tower, pure argon column, subcooler,
Wherein, the main heat exchanger, deoxidation tower, pure argon column and subcooler are arranged in ice chest, and the deoxidation tower is de- including being arranged at
The deoxidation tower reboiler of oxygen column bottom and the deoxidation tower condenser/evaporator being arranged at the top of deoxidation tower, the pure argon column include setting
Pure argon column reboiler and the pure argon column condenser/evaporator that is arranged at the top of pure argon column in pure argon column bottom；The argon gas circulatory system,
It includes the cycle compressor unit and expanding machine connected by pipeline, and the cycle compressor unit and expanding machine pass through corresponding
Pipeline respectively with crude argon purify recovery system in corresponding equipment be attached.
In order to further optimize said apparatus, the technical measures that the present invention is taken also include：
Further, the feed gas compressor group includes the feed gas compressor of pipeline connection successively and unstripped gas compression
Machine aftercooler, the cycle compressor unit are cold after recycle gas compressor and recycle gas compressor including the connection of pipeline successively
But device, the expanding machine include the expanding machine pressurized end of pipeline connection, supercharging aftercooler and expander end successively；Wherein
The expander end is arranged in the ice chest.
Further, the deoxidation tower reboiler, deoxidation tower condenser/evaporator, pure argon column reboiler, pure argon column condensation are steamed
It is immersion heat exchanger to send out device.
Further, the deoxidation tower and pure argon column use structured packing structure, random packing structure or sieve plate tower structure.
Further, the connecting line of each equipment in the crude argon purification recovery system includes：
For crude argon to be passed sequentially through into feed gas compressor group, main heat exchanger deliver to the feed pipe of deoxidation tower middle and upper part；
For the deoxidation crude argon tracheae of delivering to deoxidation crude argon in the middle part of pure argon column at the top of the deoxidation tower and will be high-purity
The liquid argon pipe that liquid argon is sent out from pure argon column bottom；
For deoxidation crude argon in part to be delivered to the deoxidation crude argon branch of deoxidation tower condenser/evaporator from deoxidation crude argon tracheae
Pipe and the deoxidation crude argon condensate liquid return duct for returning to deoxidation crude argon condensate liquid at the top of deoxidation tower；
For nitrogen to be sent out at the top of the pure argon column to the nitrogen tube by main heat exchanger recovery cold discharge, for by part
Nitrogen delivers to the nitrogen branch pipe of pure argon column condenser/evaporator from nitrogen tube and returns to nitrogen condensate liquid at the top of pure argon column
Nitrogen condensate liquid return duct.
For the gaseous mixture of nitrogen and oxygen to be sent out into what is discharged after main heat exchanger reclaims cold from denitrification column bottom
Mixture pipe, for the oxygen-bearing liquid pipe by oxygen-bearing liquid from deoxidation tower bottom discharge.
Further, each equipment purifies the company of each equipment in recovery system with the crude argon in the argon gas circulatory system
Adapter road includes：
For the mixed argon gas circulation for discharging the top of deoxidation tower condenser/evaporator and pure argon column condenser/evaporator
Gas is via the circulating gas pipe that cycle compressor unit is delivered to after subcooler, main heat exchanger recovery cold；
For circulating air to be delivered to the circulating air recurrent canal of main heat exchanger from cycle compressor unit；
For part circulating air to be delivered into the first circulation gas recurrent canal of deoxidation tower reboiler from main heat exchanger and is used for
Part circulating air condensate liquid is back to the first circulation airsetting liquid recurrent canal of deoxidation tower condenser/evaporator；
For part circulating air to be delivered into the second circulation gas recurrent canal of pure argon column reboiler from main heat exchanger and is used for
Part circulating air condensate liquid is back to the second circulation airsetting liquid recurrent canal of pure argon column condenser/evaporator.
Further, circulating air is set to return to branch pipe on the circulating air recurrent canal, circulating air return branch pipe is used for will
Part circulating air is sent back to and is incorporated into via expanding machine pressurized end, supercharging aftercooler, main heat exchanger, expander end successively
The circulating gas pipe of subcooler outlet；Further, draw circulating air from the middle part of main heat exchanger and be communicated to expander end.
Further, the first circulation gas for being connected to pure argon column condenser/evaporator is set on first circulation airsetting liquid recurrent canal
Lime set returns to branch pipe.
Further, the feed pipe of main heat exchanger outlet, deoxidation crude argon tracheae, first circulation airsetting liquid recurrent canal,
Second circulation airsetting liquid recurrent canal, first circulation airsetting liquid return and are respectively provided with regulating valve on branch pipe.
Further, the device also includes being used for the liquid nitrogen storage tank for storing high-purity liquid nitrogen.
Second object of the present invention is to provide a kind of method that Full distillation purification recovery argon gas is carried out using said apparatus,
It comprises the following steps：
The supercharging cooling of step 1) crude argon：Crude argon containing oxygen and hydrogen is increased into feed gas compressor group
Pressure and preliminary cooling, and condensing temperature is cooled further to by main heat exchanger；
The rectification and purification of step 2) crude argon：The middle and lower part that crude argon under condensing temperature enters deoxidation tower carries out rectifying point
From, deoxidation tower top obtain deoxidation crude argon, deoxidation tower bottom discharge oxygen-bearing liquid；Deoxidation crude argon is from deoxidation tower
Top be discharged into the middle part of pure argon column and carry out rectifying separation, high-purity liquid argon is obtained in the bottom of pure argon column, in pure argon column
Discharge nitrogen in top；
Wherein, the main heat exchanger, deoxidation tower, pure argon column are arranged in ice chest, and the argon gas circulatory system is the ice chest
Low temperature is provided and provides cold for argon gas liquefaction.
In order to further optimize the above method, technical measures of the invention include：
Further, the composition (volume content) of the crude argon is Ar：82~87%；O2：12~18%；N2：0.01~
0.03%, further, the composition (volume content) of the crude argon is Ar：85%；O2：14.98%；N2：0.02%.
Further, the pressure of the crude argon of the feed gas compressor group outlet is 0.6MPaA, and temperature is 40 DEG C.
Further, in the step 2), in the rectifying separation of deoxidation tower, the deoxidation tower reboiler of deoxidation tower bottom
The gas required for deoxidation tower rectifying is provided, the deoxidation tower condenser/evaporator at the top of deoxidation tower is provided required for deoxidation tower rectifying
Liquid；In the rectifying separation of pure argon column, the pure argon column reboiler of pure argon column bottom provides the gas required for pure argon column rectifying,
Pure argon column condenser/evaporator at the top of pure argon column provides the liquid required for pure argon column rectifying；
Wherein, the thermal source of the deoxidation tower reboiler and pure argon column reboiler is the circulation argon from the argon gas circulatory system
Gas, low-temperature receiver is respectively the liquid of deoxidation tower bottom and the liquid of pure argon column bottom, and in heat transfer process, circulation argon gas liquefaction is liquid
Body, the vaporizing liquid of tower bottom produce gas；
Wherein, the thermal source of the deoxidation tower condenser/evaporator and pure argon column condenser/evaporator is respectively deoxidation crude argon and nitrogen
Gas, low-temperature receiver is liquid argon, and in heat transfer process, deoxidation crude argon and nitrogen are condensed into liquid respectively, and liquid argon vaporization produces gas,
Mixed from the bog of deoxidation tower condenser/evaporator and pure argon column condenser/evaporator and be sent into the argon gas circulatory system.
Further, the operating procedure of the nitrogen circulating system includes：
From the circulating air that ice chest comes out after the compression cooling of recycle compressor group, it is divided into two parts：
It is partly into after the supercharging of expanding machine pressurized end and enters main heat exchanger by being pressurized aftercooler cooling, from main heat exchange
Extract out in the middle part of device and expanded into expander end, main heat exchanger re-heat is entered after decrease temperature and pressure and returns recycle compressor；
Another part enters main heat exchanger, after the circulating air cooling backflowed, is divided into two parts：It is partly into deoxidation tower
For reboiler as thermal source, it discharges heat by phase transformation, vaporizes the liquid of deoxidation tower bottom, itself is liquefied as liquid；It is another
Part enters pure argon column reboiler as thermal source, discharges heat by phase transformation, the liquid of vaporization pure argon column bottom, itself is liquefied
For liquid；Deoxidation tower condenser/evaporator is respectively enterd after the liquefied liquid throttling of deoxidation tower reboiler and the discharge of pure argon column reboiler
With pure argon column condenser/evaporator, deoxidation crude argon and nitrogen are then cooled down respectively and provides rectifying to be respectively deoxidation tower and pure argon column
Liquid；
Wherein, the liquid argon in deoxidation tower condenser/evaporator and pure argon column condenser/evaporator vaporizes generation gas respectively, the gas
The liquefied liquid not throttled that body is discharged respectively with deoxidation tower reboiler and pure argon column reboiler after mixing enters in subcooler
Row heat exchange, the gas from subcooler turn into circulating air with the gas mixing after the expansion of expander end, pass through main heat exchanger
Re-heat cooling box, into recycle compressor group pressurized circulation.
Further, the pressure of the circulating air of recycle compressor group outlet is 1MPaA, 40 DEG C of temperature.
Further, the temperature of the part circulating air of the supercharging aftercooler outlet is 40 DEG C, and supercharging aftercooler goes out
The part circulating air of mouth enters main heat exchanger, and is retracted to expander end with about -90 DEG C in the middle part of main heat exchange and is expanded to
0.12MPaA。
Further, the recovery of step 3) crude argon is also included after step 2)：High-purity liquid argon is delivered to liquid argon storage tank
Carry out storage recovery；Further, also include the high-purity liquid nitrogen being pumped to respectively from liquid argon storage tank after step 3)
The step of deoxidation tower condenser/evaporator and pure argon column condenser/evaporator.
Further, the oxygen content ＜ 1.5ppm in the deoxidation crude argon；Oxygen content in high-purity liquid argon
＜ 1.5ppm, nitrogen content ＜ 4ppm.
Compared with prior art, the invention has the advantages that：
The present invention provides cold by circulator, while argon gas is purified, also argon gas is liquefied, compensate for coal
The deficiency of the supporting space division of chemical industry；The present invention passes through reasonable disposition heat exchange process so that energy utilization optimizes, and reduces the damage of cold
Lose, and farthest reclaim argon gas, reduce and waste, it has certain economic benefit.
Brief description of the drawings
Fig. 1 is a kind of schematic flow sheet of the device of Full distillation purification recovery argon gas in one embodiment of the invention；
Reference in figure is as follows：
Feed gas compressor group 11, feed gas compressor 111, feed gas compressor aftercooler 112, main heat exchanger 12,
Deoxidation tower 13, deoxidation tower reboiler 131, deoxidation tower condenser/evaporator 132, pure argon column 14, pure argon column reboiler 141, pure argon column
Condenser/evaporator 142, subcooler 15, cycle compressor unit 21, recycle gas compressor 211, recycle gas compressor aftercooler
212nd, expanding machine 22, expanding machine pressurized end 221, supercharging aftercooler 222, expander end 223；
Feed pipe L1, deoxidation crude argon tracheae L2, deoxidation crude argon gas branch pipe L21, deoxidation crude argon condensate liquid return duct L22,
Liquid argon pipe L3, nitrogen tube L4, nitrogen branch pipe L41, nitrogen condensate liquid return duct L42, mixture pipe L5, oxygen-bearing liquid pipe L6, follow
Ring tracheae L7, circulating air recurrent canal L8, first circulation gas recurrent canal L81, first circulation airsetting liquid recurrent canal L82, second circulation
Gas recurrent canal L83, second circulation airsetting liquid recurrent canal L84, circulating air return to branch pipe L85, first circulation airsetting liquid returns to branch pipe
L86, regulating valve V1-V5.
Embodiment
The present invention provides a kind of device of Full distillation purification recovery argon gas, and it includes：Crude argon purifies recovery system,
It is included by the feed gas compressor group of pipeline connection, main heat exchanger, deoxidation tower, pure argon column, subcooler；Argon gas cyclic system
System, it includes the cycle compressor unit and expanding machine connected by pipeline, and the cycle compressor unit and expanding machine pass through
Corresponding pipeline purifies corresponding equipment in recovery system with crude argon and is attached respectively；Pass through the invention further relates to one kind upper
State the method that device carries out reclaiming argon gas.
With reference to the accompanying drawings and examples, the embodiment of the present invention is further described.Following examples are only
For clearly illustrating technical scheme, and can not be limited the scope of the invention with this.
Embodiment 1
As shown in figure 1, the crude argon that the synergy top of tower from coal chemical industry process matching space division comes out (contains Ar:~
85mol%, O2：~14.98%；N2：~0.02%) via feed pipe L1, be compressed to by feed gas compressor 111~
0.6MPaA, and~40 DEG C are cooled to by feed gas compressor cooler 112, into the main heat exchanger 12 in ice chest 1, at it
Condensing temperature is inside cooled to, enters the middle and lower part of deoxidation tower 13 after adjusted valve V1 throttlings.In deoxidation tower 13, the deoxidation of its bottom of towe
Tower reboiler 131 provides the gas required for the rectifying of deoxidation tower 13, and the deoxidation tower condenser/evaporator 132 of its tower top is deoxidation tower 13
Liquid needed for rectifying is provided.Crude argon condenses with the gas mixing that deoxidation tower reboiler 131 provides as gas, deoxidation tower is risen
For the liquid that evaporator 132 provides as lower descending liquid, both carry out rectifying in deoxidation tower.Oxygen component is split into the liquid of bottom of towe
In pass through oxygen-bearing liquid pipe L6 discharge.Oxygen content is obtained from the top of deoxidation tower 13<1.5ppm deoxidation crude argon is thick by deoxidation
Tunger tube L2, and after regulating valve V2 controls, into the middle part of pure argon column 14.In order to maintain the separative efficiency in deoxidation tower 13,
The oxygen of its bottom of towe and the gaseous mixture of argon gas discharge after reclaiming cold by main heat exchanger 12 via mixture pipe L5.
The foundation of the rectifying operating mode of pure argon column 14 and the offer liquid of pure argon column condenser/evaporator 142 and tower for passing through top of tower
The pure argon column reboiler 141 of bottom provides gas.The gas mixing that deoxidation crude argon provides with pure argon column reboiler 141 is as upper
Gas is risen, for the liquid that pure argon column condenser/evaporator 142 provides as lower descending liquid, both carry out rectifying in pure argon column.In pure argon column
What is mainly removed in 14 is the component than argon gas low boiling point such as nitrogen component, is obtained in the bottom of pure argon column 14 satisfactory high-purity
Liquid argon (oxygen-containing 1.5ppm, nitrogenous 4ppm), it is sent out ice chest and is sent into liquid argon storage tank progress after being extracted by high-purity liquid nitrogen pipe L3
Store, liquid argon can be pumped to deoxidation tower condenser/evaporator 132 and pure argon column condenser/evaporator 142 as cold in the liquid argon storage tank
Source.
The cold required for low temperature, argon gas liquefaction in ice chest 1 is mainly provided by the argon gas circulatory system.Go out from ice chest 1
The argon gas come is compressed to 1MPaA by recycle compressor 211, cools to 40 DEG C by recycle compressor cooler 212, is then divided into
Two parts, by supercharging after a part of supercharging of expanding machine pressurized end 221 for entering expanding machine 22 by circulating air return branch pipe L85
Aftercooler 222 is cooled to 40 DEG C of main heat exchangers 12 entered in ice chest 1, is retracted to from the middle part of main heat exchanger 12 (about -90 DEG C)
The expander end 223 of expanding machine 21 is expanded to 0.12MPaA, and the re-heat of main heat exchanger 12 is entered after decrease temperature and pressure and returns circulation pressure
Contracting unit 21.
Another part enters the main heat exchanger 12 of ice chest 1 by circulating air recurrent canal L8, and the gas to be backflowed is cooled to liquid
Change point, be divided into two parts, a part enters the high temperature side of deoxidation tower reboiler 131 by first circulation gas recurrent canal L81, passes through phase
Become release heat, vaporize the liquid of low temperature side, provide gas for the rectifying of deoxidation tower 13, itself be liquefied as liquid.Another part
The high temperature side of pure argon column reboiler 141 is entered by second circulation gas recurrent canal L82, heat is discharged by phase transformation, vaporizes low temperature side
Liquid, provide gas for the rectifying of pure argon column 14, itself be liquefied as liquid.The liquefier that two reboilers 131,141 come out
Body is respectively via first circulation airsetting liquid recurrent canal L82 and second circulation airsetting liquid recurrent canal L84, and pass through regulating valve V3 respectively
Enter deoxidation tower condenser/evaporator 132 and pure argon column condenser/evaporator 142 after being throttled with regulating valve V4, cool down deoxidation tower 13 and essence
The gas at the top of argon column 14, rectifying liquid is provided for two towers；The part deoxidation crude argon at the wherein top of deoxidation tower 13 passes through de-
Oxygen crude argon tracheae L2 branch road-deoxidation crude argon gas branch pipe L21 enters deoxidation tower condenser/evaporator 132, and its lime set is thick by deoxidation
Argon gas condensate liquid return duct L22 is back to deoxidation tower 13；Branch road-nitrogen that the part nitrogen at the top of pure argon column 14 passes through nitrogen tube L4
Gas branch pipe L41 enters pure argon column condenser/evaporator 142, and its lime set is back to pure argon column 14 by nitrogen condensate liquid return duct L42,
Remaining nitrogen discharges after reclaiming cold via main heat exchanger 12 by nitrogen tube L4.Deoxidation tower condenser/evaporator 132 and pure argon column
It is blended with deoxidation tower reboiler and pure argon column reboiler discharges respectively after liquid in condenser/evaporator 142 vaporizes in itself
The liquefied liquid not throttled is exchanged heat in subcooler 17, passes through circulating gas pipe L7 and expansion from the gas that subcooler 17 is discharged
The gas mixing that machine expanding end 223 exports, by the re-heat cooling box 1 of main heat exchanger 12, followed into the pressurization of recycle compressor group 21
Ring.
In the above-described embodiments, first circulation airsetting liquid recurrent canal L82 sets the towards pure argon column condenser/evaporator 142
One circulating air lime set returns to branch pipe L86, and the first circulation airsetting liquid returns to branch pipe L86 and sets regulating valve V5；The deoxidation tower
Reboiler 131, deoxidation tower condenser/evaporator 132, pure argon column reboiler 133, pure argon column condenser/evaporator 134 are that immersion changes
Hot device；The deoxidation tower 13 and pure argon column 14 use structured packing structure, and it is respectively provided with two sections of fillers (also can be according to actual conditions
It is adjusted).
From above-described embodiment, the present invention provides cold by circulator, while argon gas is purified, also argon gas is entered
Go liquefaction, compensate for the deficiency of theme space division；Pass through reasonable disposition heat exchange process simultaneously so that energy utilization optimizes, and subtracts
The loss of few cold, and argon gas is farthest reclaimed, reduce and waste, it has certain economic benefit.
The specific embodiment of the present invention is described in detail above, but it is intended only as example, it is of the invention and 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
Substitute also all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and
Modification, all should be contained within the scope of the invention.
Claims (10)
- A kind of 1. device of Full distillation purification recovery argon gas, it is characterised in that including：Crude argon purifies recovery system, its feed gas compressor group (11) for including connecting by pipeline, main heat exchanger (12), takes off Oxygen column (13), pure argon column (14), subcooler (15)；Wherein, the main heat exchanger (12), deoxidation tower (13), pure argon column (14) and Subcooler (15) is arranged in ice chest (1), and the deoxidation tower (13) is including being arranged at the deoxidation tower of deoxidation tower (13) bottom again Device (131) and the deoxidation tower condenser/evaporator (132) being arranged at the top of deoxidation tower (13) are boiled, the pure argon column (14) includes setting Pure argon column reboiler (141) and the pure argon column condenser/evaporator that is arranged at the top of pure argon column (14) in pure argon column (14) bottom (142)；The argon gas circulatory system, it includes the cycle compressor unit (21) and expanding machine (22) connected by pipeline, the circulation Air compressor group (21) and expanding machine (22) purify corresponding equipment in recovery system with crude argon respectively by corresponding pipeline It is attached.
- A kind of 2. device of Full distillation purification recovery argon gas according to claim 1, it is characterised in that the material pressure Contracting unit (11) includes the feed gas compressor (111) and feed gas compressor aftercooler (112) of pipeline connection successively, described Cycle compressor unit (21) includes the recycle gas compressor (211) and recycle gas compressor aftercooler of pipeline connection successively (212), the expanding machine (22) includes the expanding machine pressurized end (221) of pipeline connection, supercharging aftercooler (222) and swollen successively Swollen machine expanding end (223)；Wherein described expander end (223) is arranged in the ice chest (1).
- 3. the device of a kind of Full distillation purification recovery argon gas according to claim 1, it is characterised in that the deoxidation tower is again It is heavy to boil device (131), deoxidation tower condenser/evaporator (132), pure argon column reboiler (133), pure argon column condenser/evaporator (134) Immersion heat exchanger.
- A kind of 4. device of Full distillation purification recovery argon gas according to claim 1, it is characterised in that the deoxidation tower (13) and pure argon column (14) uses structured packing structure, random packing structure or sieve plate tower structure.
- 5. the device of a kind of Full distillation purification recovery argon gas according to claim 1, it is characterised in that the device also includes For storing the liquid nitrogen storage tank of high-purity liquid nitrogen.
- 6. a kind of method using such as device Full distillation according to any one of claims 1 to 5 purification recovery argon gas, its feature It is, comprises the following steps：The supercharging cooling of step 1) crude argon：Crude argon containing oxygen and hydrogen into feed gas compressor group carry out supercharging and Preliminary cooling, and condensing temperature is cooled further to by main heat exchanger；The rectification and purification of step 2) crude argon：The middle and lower part that crude argon under condensing temperature enters deoxidation tower carries out rectifying separation, Deoxidation crude argon is obtained at the top of deoxidation tower, oxygen-bearing liquid is discharged in the bottom of deoxidation tower；Deoxidation crude argon is from deoxidation tower The middle part that top is discharged into pure argon column carries out rectifying separation, high-purity liquid argon is obtained in the bottom of pure argon column, on the top of pure argon column Discharge nitrogen in portion；Wherein, the main heat exchanger, deoxidation tower, pure argon column are arranged in ice chest, and the argon gas circulatory system provides for the ice chest Low temperature and for argon gas liquefaction cold is provided.
- 7. the method for Full distillation purification recovery argon gas according to claim 6, it is characterised in that in the step 2), In the rectifying separation of deoxidation tower, the deoxidation tower reboiler of deoxidation tower bottom provides the gas required for deoxidation tower rectifying, deoxidation The deoxidation tower condenser/evaporator of top of tower provides the liquid required for deoxidation tower rectifying；In the rectifying separation of pure argon column, smart argon The pure argon column reboiler of tower bottom provides the gas required for pure argon column rectifying, and the pure argon column condenser/evaporator at the top of pure argon column carries For the liquid required for pure argon column rectifying；Wherein, the thermal source of the deoxidation tower reboiler and pure argon column reboiler is the circulation argon gas from the argon gas circulatory system, Low-temperature receiver is respectively the liquid of deoxidation tower bottom and the liquid of pure argon column bottom, and in heat transfer process, circulation argon gas liquefaction is liquid, The vaporizing liquid of tower bottom produces gas；Wherein, the thermal source of the deoxidation tower condenser/evaporator and pure argon column condenser/evaporator is respectively deoxidation crude argon and nitrogen, Low-temperature receiver is liquid argon, and in heat transfer process, deoxidation crude argon and nitrogen are condensed into liquid respectively, and liquid argon vaporization produces gas, comes Mixed from the bog of deoxidation tower condenser/evaporator and pure argon column condenser/evaporator and be sent into the argon gas circulatory system.
- 8. the method for Full distillation purification recovery argon gas according to claim 7, it is characterised in that the nitrogen circulating system Operating procedure include：From the circulating air that ice chest comes out after the compression cooling of recycle compressor group, it is divided into two parts：It is partly into after the supercharging of expanding machine pressurized end and enters main heat exchanger by being pressurized aftercooler cooling, from main heat exchanger Portion is extracted out to be expanded into expander end, and main heat exchanger re-heat is entered after decrease temperature and pressure and returns recycle compressor；Another part enters main heat exchanger, after the circulating air cooling backflowed, is divided into two parts：Deoxidation tower is partly into boil again For device as thermal source, it discharges heat by phase transformation, vaporizes the liquid of deoxidation tower bottom, itself is liquefied as liquid；Another part Into pure argon column reboiler as thermal source, heat is discharged by phase transformation, the liquid of vaporization pure argon column bottom, itself is liquefied as liquid Body；Deoxidation tower condenser/evaporator and essence are respectively enterd after the liquefied liquid throttling of deoxidation tower reboiler and the discharge of pure argon column reboiler Argon column condenser/evaporator, deoxidation crude argon and nitrogen are then cooled down respectively and provides rectifying liquid to be respectively deoxidation tower and pure argon column Body；Wherein, the liquid argon in deoxidation tower condenser/evaporator and pure argon column condenser/evaporator vaporizes generation gas respectively, gas warp The liquefied liquid not throttled discharged respectively with deoxidation tower reboiler and pure argon column reboiler after mixing is changed in subcooler Heat, the gas from subcooler turn into circulating air with the gas mixing after the expansion of expander end, pass through main heat exchanger re-heat Cooling box, into recycle compressor group pressurized circulation.
- 9. the method for Full distillation purification recovery argon gas according to claim 6, it is characterised in that also wrapped after step 2) Include the recovery of step 3) crude argon：High-purity liquid argon is delivered to liquid argon storage tank and carries out storage recovery.
- 10. the method for Full distillation purification recovery argon gas according to claim 6, it is characterised in that the deoxidation crude argon In oxygen content ＜ 1.5ppm；Oxygen content ＜ 1.5ppm, nitrogen content ＜ 4ppm in high-purity liquid argon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711014301.XA CN107606874B (en) | 2017-10-26 | 2017-10-26 | Device for recycling argon through full rectification purification and argon recycling method thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108224900A (en) * | 2018-01-24 | 2018-06-29 | 北京拓首能源科技股份有限公司 | A kind of oxygen nitrogen and argon piece-rate system using cold energy of liquefied natural gas |
| CN108413706A (en) * | 2018-05-15 | 2018-08-17 | 瀚沫能源科技（上海）有限公司 | A kind of concentration of krypton xenon and neon helium concentrate integrating apparatus and method containing circulating nitrogen gas |
| CN108507276A (en) * | 2018-06-05 | 2018-09-07 | 上海联风能源科技有限公司 | A kind of Full distillation purification recycling argon system and method without expanding machine |
| CN109253583A (en) * | 2018-09-03 | 2019-01-22 | 杭州杭氧股份有限公司 | A kind of device and its method of purification of normal temperature and pressure crude argon recycling purification |
| CN109506419A (en) * | 2017-09-15 | 2019-03-22 | 修国华 | For producing the method and system of liquid argon and/or argon gas product |
| CN109737690A (en) * | 2019-01-18 | 2019-05-10 | 侨源气体（福州）有限公司 | Compression large scale liquid space division device and its application method in a kind of |
| CN110451467A (en) * | 2019-08-30 | 2019-11-15 | 苏州成于思气体科技有限公司 | A kind of multi-state argon gas recyclable device |
| 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 |
| CN110608582A (en) * | 2019-09-10 | 2019-12-24 | 苏州市兴鲁空分设备科技发展有限公司 | Argon tail gas recycling and purifying device |
| CN111928573A (en) * | 2020-07-14 | 2020-11-13 | 国家能源集团宁夏煤业有限责任公司 | Argon preparation method |
| CN113557401A (en) * | 2019-03-11 | 2021-10-26 | 环球油品有限责任公司 | Hydrocarbon gas processing |
| CN113739515A (en) * | 2021-09-06 | 2021-12-03 | 乔治洛德方法研究和开发液化空气有限公司 | Method and device for extracting high-purity liquid argon through rich argon |
| CN114646188A (en) * | 2022-05-18 | 2022-06-21 | 河南心连心深冷能源股份有限公司 | Crude argon purifying and liquefying device and purifying method used by separation from air separation system |
| CN114791204A (en) * | 2022-05-05 | 2022-07-26 | 杭州制氧机集团股份有限公司 | Nitrogen circulating low-temperature rectification crude argon purification and liquefaction device and use method thereof |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109506419A (en) * | 2017-09-15 | 2019-03-22 | 修国华 | For producing the method and system of liquid argon and/or argon gas product |
| CN108224900B (en) * | 2018-01-24 | 2024-01-09 | 北京拓首能源科技股份有限公司 | Oxygen-nitrogen-argon separation system utilizing liquefied natural gas cold energy |
| CN108224900A (en) * | 2018-01-24 | 2018-06-29 | 北京拓首能源科技股份有限公司 | A kind of oxygen nitrogen and argon piece-rate system using cold energy of liquefied natural gas |
| CN108413706A (en) * | 2018-05-15 | 2018-08-17 | 瀚沫能源科技（上海）有限公司 | A kind of concentration of krypton xenon and neon helium concentrate integrating apparatus and method containing circulating nitrogen gas |
| CN108413706B (en) * | 2018-05-15 | 2023-10-03 | 瀚沫能源科技（上海）有限公司 | Integrated device and method for concentrating krypton and xenon and concentrating neon and helium with circulating nitrogen |
| CN108507276A (en) * | 2018-06-05 | 2018-09-07 | 上海联风能源科技有限公司 | A kind of Full distillation purification recycling argon system and method without expanding machine |
| CN109253583A (en) * | 2018-09-03 | 2019-01-22 | 杭州杭氧股份有限公司 | A kind of device and its method of purification of normal temperature and pressure crude argon recycling purification |
| CN109737690A (en) * | 2019-01-18 | 2019-05-10 | 侨源气体（福州）有限公司 | Compression large scale liquid space division device and its application method in a kind of |
| CN113557401A (en) * | 2019-03-11 | 2021-10-26 | 环球油品有限责任公司 | Hydrocarbon gas processing |
| CN110451467A (en) * | 2019-08-30 | 2019-11-15 | 苏州成于思气体科技有限公司 | A kind of multi-state argon gas recyclable device |
| CN110608582A (en) * | 2019-09-10 | 2019-12-24 | 苏州市兴鲁空分设备科技发展有限公司 | Argon tail gas recycling and purifying device |
| 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 |
| CN111928573A (en) * | 2020-07-14 | 2020-11-13 | 国家能源集团宁夏煤业有限责任公司 | Argon preparation method |
| CN113739515A (en) * | 2021-09-06 | 2021-12-03 | 乔治洛德方法研究和开发液化空气有限公司 | Method and device for extracting high-purity liquid argon through rich argon |
| CN113739515B (en) * | 2021-09-06 | 2022-10-21 | 乔治洛德方法研究和开发液化空气有限公司 | Method and device for extracting high-purity liquid argon through rich argon |
| CN114791204A (en) * | 2022-05-05 | 2022-07-26 | 杭州制氧机集团股份有限公司 | Nitrogen circulating low-temperature rectification crude argon purification and liquefaction device and use method thereof |
| CN114646188A (en) * | 2022-05-18 | 2022-06-21 | 河南心连心深冷能源股份有限公司 | Crude argon purifying and liquefying device and purifying method used by separation from air separation system |
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