CN106123490B - A kind of devices and methods therefor that pure neon is produced by ne-He mixture - Google Patents

A kind of devices and methods therefor that pure neon is produced by ne-He mixture Download PDF

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CN106123490B
CN106123490B CN201610528196.0A CN201610528196A CN106123490B CN 106123490 B CN106123490 B CN 106123490B CN 201610528196 A CN201610528196 A CN 201610528196A CN 106123490 B CN106123490 B CN 106123490B
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liquid
gas
helium
adsorption device
neon
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CN106123490A (en
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李琦
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/028Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/028Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases
    • F25J3/029Processes 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 helium
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/02Processes or apparatus using separation by rectification in a single pressure main column system
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/70Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00Processes or apparatus using other separation and/or other processing means
    • F25J2205/02Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F25J2205/04Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum in the feed line, i.e. upstream of the fractionation step
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00Processes or apparatus using other separation and/or other processing means
    • F25J2205/40Processes or apparatus using other separation and/or other processing means using hybrid system, i.e. combining cryogenic and non-cryogenic separation techniques
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00Processes or apparatus using other separation and/or other processing means
    • F25J2205/60Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00Processes characterised by the type or other details of the product stream
    • F25J2215/04Recovery of liquid products
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00Processes characterised by the type or other details of the product stream
    • F25J2215/30Helium
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00Processes characterised by the type or other details of the product stream
    • F25J2215/32Neon
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00Refrigeration techniques used
    • F25J2270/14External refrigeration with work-producing gas expansion loop
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00Refrigeration techniques used
    • F25J2270/30Quasi-closed internal or closed external helium refrigeration cycle

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation Of Gases By Adsorption (AREA)

Abstract

The invention discloses a kind of devices and methods therefors that pure neon is produced by ne-He mixture, the device includes ice chest, the first N2 adsorption device, the second N2 adsorption device, vacuum pump, helium compressor, helium expanding machine, helium expanding machine dog point, liquid neon Dewar, liquid neon pump and air-bathing gasifier, and the first gas-liquid separator, the second gas-liquid separator, the first plate-fin heat exchanger, the second plate-fin heat exchanger, third gas-liquid separator, rectifying column, helium expanding machine and vacuum liquid nitrogen heat exchanger are wherein provided in ice chest;First N2 adsorption device, the second N2 adsorption device, vacuum pump, helium compressor, helium expanding machine dog point, liquid neon Dewar, liquid neon pump and air-bathing gasifier are arranged at the outside of ice chest.The device is by the way that absorber is placed on except ice chest, avoid the process of hot reactivation in the cold state, the violent operating mode variation in ice chest is avoided, so as to significantly improve the design of the thermal stress of ice chest, also avoids leaking caused by possible because of the hot reactivation repeated.

Description

A kind of devices and methods therefor that pure neon is produced by ne-He mixture
Technical field
The present invention relates to rare gas manufacture and chemical industry deep refrigerating project technical fields, and in particular to one kind is by ne-He mixture Produce the devices and methods therefor of pure neon.
Background technology
In the prior art, by ne-He mixture produce pure neon the technological process of production as shown in Figure 1, whole flow process by mutual Two of switching independently denitrogenate unit ice chest (the first ice chest 1 and the second ice chest 2) and neon helium rectifying ice chest 3 forms.
In Fig. 1, the liquid nitrogen of negative pressure is filled in the first ice chest 1, temperature is about 65K, and the first N2 adsorption device A is just in work Make, the liquid nitrogen in the second ice chest 2 has been pumped, and restore room temperature, and the second N2 adsorption device B is regenerating.
(1 kilogram of pressure refers to that the object of 1 kilogram weight acts on 1 square centimeter of area to 30 kilograms or so gauges Pressure caused by upper, 1 kilogram of pressure is equal to the pressure of 0.1Mpa, while 1 kilogram of pressure is equal to the pressure of 1000mbar, gauge pressure That is the pressure differential of the relatively residing atmospheric pressure of medium) the crude Ne-He body containing nitrogen enter the first ice chest 1 in, by first around Heat exchange of heat pipe 3A causes temperature to be reduced to 65k or so so that the part nitrogen liquefaction wherein contained passes through the first gas-liquid separator 1A obtains the ne-He mixture containing less nitrogen into the first N2 adsorption device A, absorption fall return to after remaining nitrogen first around Heat exchange of heat pipe 3A re-heats obtain pure ne-He mixture to room temperature, and the liquid obtained in the first gas-liquid separator 1A is then throttled to 1.5 kilograms or so of pressure enters the second gas-liquid separator 2A, obtains the liquid containing 99% or so nitrogen and is drained into the first ice chest 1 In, vacuumize caused liquid nitrogen loss partly to make up.
Pure ne-He mixture a portion after re-heat to room temperature enters in the second ice chest 2, blowback the second N2 adsorption device B To regenerate nitrogen absorber, the pressure that another part is then pressurized to 180 kilograms by the first compressor 4 enters neon helium rectifying ice chest 3, warp It crosses liquid nitrogen heat exchange of the third more than heat exchange of heat pipe postcooling to liquid nitrogen temperature and in liquid nitrogen heat exchanger 31 and arrives 78K or so, continue The 4th into next stage causes temperature to be further decreased to 40K or so around heat exchange of heat pipe 3D, is then throttled to 30 kilograms or so Pressure, exchange heat into liquid neon heat exchanger 32 and liquid neon, gasify liquid neon, and temperature drops to 25K or so so that thick neon helium part liquid Change, subsequently into knockout drum 33, the cold conditions raw helium gas containing 90% or so helium and the rich neon liquid rich in neon are obtained, wherein cold Lower one of work is taken out or entered to state raw helium gas by obtaining raw helium gas after two-stage wound tube heat exchanger re-heat for filling bottle packaging Sequence further purifies, and the pressure that rich neon liquid is then throttled to 1.5 kilograms or so enters rectifying column 34, and part is obtained in tower top Rich neon recycles after re-heat and removes air bag, the pure neon liquid obtained in bottom of towe return to before liquid neon heat exchanger 32 gasify after pass through Pure neon is obtained after heat exchange of heat pipe re-heat, pure neon fills bottle packaging and takes out after being compressed by the second compressor 5.
The shortcomings that producing the technological process of production of pure neon by ne-He mixture in the prior art includes:
For denitrogenating unit:One of them denitrogenate unit when denitrogenating inside need to fill liquid nitrogen for cooling down each flow Unit, another, which then needs to discharge liquid nitrogen, is restored to room temperature and denitrogenates absorber to regenerate, because of the flow sheet equipment being related to More, thermal capacity is big, and being denitrogenated after absorber completes regeneration in regeneration needs to cool down a large amount of flow sheet equipment with liquid nitrogen, so as to consume A large amount of liquid nitrogen, on the other hand so that container thermal stress, which often changes, is easy to cause leakage;In addition, more sleeve containes need bigger Place is placed and higher investment.
For neon helium rectification cell:1) extra-high throttling is needed to generate cold, it is this to be throttled by high pressure gas Mode to freeze be extremely inefficient;2) due to the presence of extra-high can only use inefficient coil exchanger (around Heat exchange of heat pipe);3) due to the presence of the extra-high of 180 kilograms of pressure, the requirement to manufacture and the safety of system is very high.
Need two compressors that 200 kilograms, gas compression is increased additional investment in flow.
Generally speaking, flow system of the prior art is complicated, and inefficiency needs more high pressure compressors, there is also Some potential safety problems;The neon most importantly finally produced can only be pressed into steel by the compressor in downstream in gaseous form Bottle easilys lead to leak and introduce oil and moisture in this process, finally results in the decline of product quality.
Invention content
The purpose of the present invention is to provide a kind of new devices and methods therefors that pure neon is produced by ne-He mixture, reduce system The complexity of system removes the super-pressure process gas there are security risk, reduces investment, improves efficiency and product quality.
To achieve the above object, the device of the present invention that pure neon is produced by ne-He mixture includes ice chest, the first nitrogen Absorber, the second N2 adsorption device, vacuum pump, helium compressor, helium expanding machine, helium expanding machine dog point, liquid neon Dewar, liquid neon pump And air-bathing gasifier, the first gas-liquid separator, the second gas-liquid separator, the first plate fin heat-exchanging are wherein provided in ice chest Device, the second plate-fin heat exchanger, third gas-liquid separator, rectifying column, helium expanding machine and vacuum liquid nitrogen heat exchanger;First N2 adsorption Device, the second N2 adsorption device, vacuum pump, helium compressor, helium expanding machine dog point, liquid neon Dewar, liquid neon pump and empty bath gasification Device is arranged at the outside of ice chest;The entrance of first gas-liquid separator is connect with crude Ne-He input channel;First gas The first outlet of liquid/gas separator is connect with the entrance of the second gas-liquid separator;The first outlet of second gas-liquid separator with first time Getter output channel connects;The second outlet of second gas-liquid separator is connect with dirty nitrogen output channel;First gas-liquid separator Second outlet is connect with the entrance of the first N2 adsorption device and the entrance of the second N2 adsorption device;The outlet of first N2 adsorption device and Entrance of the outlet of phenodiazine absorber with third gas-liquid separator is connect;The first outlet of third gas-liquid separator and raw helium are defeated Go out pipeline connection;The second outlet of third gas-liquid separator and the entrance of rectifying column connect;The first outlet of rectifying column and second Recycle the connection of gas output channel;The second outlet of rectifying column is connect with the pure neon entrance of liquid neon Dewar;The liquid neon of liquid neon Dewar goes out Mouth is connect with the entrance of liquid neon pump;The outlet of liquid neon pump and the entrance of air-bathing gasifier connect;The outlet of air-bathing gasifier It is connect with gas cylinder;The helium outlet of liquid neon Dewar is connected by the entrance of the first helium pipeline and helium compressor;Helium compresses The outlet of machine is connect with the entrance of vacuum liquid nitrogen heat exchanger;The outlet of vacuum liquid nitrogen heat exchanger is connect with the entrance of helium expanding machine; The outlet of helium expanding machine is connect with the helium entrance of liquid neon Dewar;The first end of first valve and the entrance of the first N2 adsorption device connect It connects;The second end of first valve is connected with the first end of the second valve, and the second end of the second valve enters with the second N2 adsorption device Mouth connection;The first end of third valve is connect with the entrance of the first N2 adsorption device;The second end of third valve and the 4th valve First end is connected, and the second end of the 4th valve is connect with the entrance of the second N2 adsorption device;The second outlet of first gas-liquid separator It is connected between the first valve and the second valve by ne-He mixture N2 adsorption device pipeline;4th recycling gas output channel connection Between third valve and the 4th valve;The other end of 4th recycling gas output channel and the entrance of vacuum pump connect;Vacuum pump Outlet and third recycling gas output channel connect;The first end of 5th valve is connect with the outlet of the first N2 adsorption device;5th The second end of valve is connected with the first end of the 6th valve, and the second end of the 6th valve is connect with the outlet of the second N2 adsorption device; The pure ne-He mixture discharge line being connect with the entrance of third gas-liquid separator is connected between the 5th valve and the 6th valve; Ne-He mixture N2 adsorption device pipeline, the entrance with third gas-liquid separator being connect with the second outlet of the first gas-liquid separator The pure ne-He mixture discharge line of connection, the crude Ne-He input channel being connect with the entrance of the first gas-liquid separator and the The dirty nitrogen output channel of the second outlet connection of two gas-liquid separators, the raw helium being connect with the first outlet of third gas-liquid separator Output channel, the first helium pipeline being connected between the helium outlet of liquid neon Dewar and the entrance of helium compressor and connection The second helium pipeline between the entrance of the outlet of helium compressor and vacuum liquid nitrogen heat exchanger with the first plate fin heat-exchanging Device connects and forms heat exchanging relation with the first plate-fin heat exchanger;The pure neon helium being connect with the entrance of third gas-liquid separator mixes Conjunction gas discharge line, the raw helium output channel being connect with the first outlet of third gas-liquid separator, the helium for being connected to liquid neon Dewar Gas exports the first helium pipeline between the entrance of helium compressor and is connected to outlet and the helium of vacuum liquid nitrogen heat exchanger Third helium pipeline between the entrance of expanding machine connect with the second plate-fin heat exchanger and with the second plate-fin heat exchanger Form heat exchanging relation.
The first N2 adsorption device and the second N2 adsorption device work alternatively, when the first N2 adsorption device works, the Phenodiazine absorber is reversely depressured to vacuum by vacuum pump to regenerate the second N2 adsorption device;It is discharged by the outlet of the first N2 adsorption device The ne-He mixture for having removed nitrogen enters pure ne-He mixture discharge line, another part quilt by a 5th valve part Vacuum pump by the 6th valve suck the second N2 adsorption device, to the second N2 adsorption device carry out pulse cleaning, then through the 4th valve, 4th recycling gas output channel, vacuum pump remove air bag by third recycling gas output channel recycling;When the work of the second N2 adsorption device When, the first N2 adsorption device is depressured to vacuum to regenerate the first N2 adsorption device by vacuum pump;It is arranged by the outlet of the second N2 adsorption device The ne-He mixture for having removed nitrogen gone out enters pure ne-He mixture discharge line, another portion by a 6th valve part Divide and the first N2 adsorption device is sucked by the 5th valve by vacuum pump, pulse cleaning is carried out to the first N2 adsorption device, then through third Valve, the 4th recycling gas output channel, vacuum pump remove air bag by third recycling gas output channel recycling.
The vacuum liquid nitrogen heat exchanger is extracted into vacuum pressure 50mbarA (5kPaA) hereinafter, vacuum liquid nitrogen heat exchanger, helium Compressor and helium expanding machine composition recycle to provide the cold needed for device.
The first gas-liquid separator and the second gas-liquid separator are installed in 65K warm areas, the first nitrogen is installed in room temperature warm area Absorber and the second N2 adsorption device, for removing the nitrogen component in thick ne-He mixture.
The first N2 adsorption device and the second N2 adsorption device adsorbs nitrogen present in ne-He mixture and oxygen respectively Gas.
The vacuum liquid nitrogen heat exchanger is pumped to vacuum pressure 50mbar A (5kPaA) hereinafter, vacuum liquid nitrogen heat exchanger In liquid nitrogen temperature be less than 65K.
Pipeline with helium entrance and helium the outlet connection of liquid neon Dewar is vacuum heat-insulated pipe.
Included the following steps using device of the present invention by the method that ne-He mixture produces pure neon:
Crude Ne-He containing nitrogen inputs ice chest through crude Ne-He input channel, cold by the first plate-fin heat exchanger first But so that enter the first gas-liquid separator after the nitrogen partial liquefaction wherein contained, obtained ne-He mixture passes through the first gas The second outlet of liquid/gas separator enters ne-He mixture N2 adsorption device pipeline, laggard subsequently into the first plate-fin heat exchanger re-heat Enter the first N2 adsorption device or the second N2 adsorption device, the first N2 adsorption device and the second N2 adsorption device are equipped with adsorption of nitrogen and oxygen Adsorbent, for adsorbing nitrogen present in ne-He mixture and oxygen;The first N2 adsorption device and the second N2 adsorption Device works alternatively, and when the first N2 adsorption device works, the second N2 adsorption device is reversely depressured to vacuum by vacuum pump to regenerate Second N2 adsorption device;The ne-He mixture for having removed nitrogen discharged by the outlet of the first N2 adsorption device passes through the 5th valve one Part enters pure ne-He mixture discharge line, and another part sucks the second N2 adsorption device by vacuum pump by the 6th valve, right Second N2 adsorption device carries out pulse cleaning, then recycles gas by third through the 4th valve, the 4th recycling gas output channel, vacuum pump Air bag is removed in output channel recycling;When the second N2 adsorption device works, the first N2 adsorption device by vacuum pump be depressured to vacuum with Regenerate the first N2 adsorption device;The ne-He mixture for having removed nitrogen discharged by the outlet of the second N2 adsorption device passes through the 6th valve A door part enters pure ne-He mixture discharge line, and another part sucks the first N2 adsorption by vacuum pump by the 5th valve Device carries out pulse cleaning to the first N2 adsorption device, then through third valve, the 4th recycling gas output channel, vacuum pump by third Air bag is removed in the output channel recycling of recycling gas;
After the nitrogen-rich liquid throttling obtained by the first gas-liquid separator, by the first outlet of the first gas-liquid separator into Enter the second gas-liquid separator, the obtained gas containing neon flashed off by the first outlet of the second gas-liquid separator into Enter the first recycling gas output channel, air bag is removed in direct cooling box recycling;Obtained from the liquid nitrogen fraction that is further enriched with then by The first outlet of two gas-liquid separators enters dirty nitrogen output channel, by direct as dirty nitrogen after the first plate-fin heat exchanger re-heat Emptying;
It is discharged by the pure ne-He mixture of the first N2 adsorption device or the second N2 adsorption device after purification into pure ne-He mixture Pipeline is cooled down via the first plate-fin heat exchanger and the second plate-fin heat exchanger so that its temperature declines, so that therein Neon component liquefaction subsequently into third gas-liquid separator, obtains raw helium gas and the thick liquid neon rich in neon component, and wherein raw helium gas leads to The first outlet for crossing third gas-liquid separator enters raw helium output channel, is changed via the second plate-fin heat exchanger and the first plate-fin Bottle is filled by compressor after hot device re-heat or enters lower purification procedures together;And thick liquid neon then passes through third gas-liquid separator Second outlet flows out, and into rectifying column, further rectifying obtains pure liquid neon and the neon containing part helium;Wherein contain helium Neon the second recycling gas output channel, direct cooling box recycling are entered by the first outlet of rectifying column;And pure liquid neon then leads to The second outlet outflow of rectifying column is crossed, the storage of liquid neon Dewar is sent by vacuum heat-insulated pipe.
When needing to take out neon, then the liquid neon in liquid neon Dewar by liquid neon pump is pressurized to 200 kilograms of pressure, is sent into Gas cylinder is sent into after the air-bathing gasifier gasification in downstream, packaging is taken out.
The cold of ice chest is low by the temperature being extracted into the vacuum liquid nitrogen heat exchangers of vacuum pressure 50mbarA (5kPaA) below It is provided in liquid nitrogen and helium the compression expansion cycles of 65K, helium enters helium compressor by the first helium pipeline, via helium After compressor compresses, the first plate-fin heat exchanger is entered by the second helium pipeline, it is by the first plate-fin heat exchanger that helium is cold But, subsequently into the vacuum liquid nitrogen heat exchanger for having vacuum liquid nitrogen, vacuum liquid nitrogen heat exchanger is pumped to vacuum pressure 50mbarA (5kPaA) hereinafter, the liquid nitrogen in vacuum liquid nitrogen heat exchanger is less than the low temperature liquid nitrogen of 65K for temperature, helium exchanges heat with low temperature liquid nitrogen After cooling, further cooled down into the second plate-fin heat exchanger by third helium pipeline, subsequently into helium expander, made The temperature for obtaining helium further declines, and then enters liquid neon Dewar via vacuum heat-insulated pipe, to be evaporated in coolant neon Dewar Liquid neon, then exchange heat after helium by liquid neon Dewar helium export outflow, by vacuum heat-insulated pipe return ice chest, enter First helium pipeline via the second plate-fin heat exchanger and the first plate-fin heat exchanger re-heat to room temperature, enters back into helium compression Machine.
The invention has the advantages that:It is of the present invention that the devices and methods therefor of pure neon is produced with showing by ne-He mixture There is technology to compare, whole flow process denitrogenate ice chest and rectifying ice chest is combined into one, cold is swollen by the liquid nitrogen under vacuum and helium respectively Swollen machine provides, and the extra-high for avoiding 180 kilograms of pressure enters ice chest, the pressure of whole flow process maintain 32 kilograms with Under, heat exchanger is reduced to efficient plate-fin heat exchanger;By the way that absorber is placed on except ice chest, heating in the cold state is avoided Regenerated process avoids the violent operating mode variation in ice chest, so as to greatly improve the design of the thermal stress of ice chest, also keeps away Exempt from caused to leak because of the hot reactivation of repetition, it is no longer necessary to the mutual switching of liquid nitrogen container, so as to save A large amount of liquid nitrogen;Adsorption system is placed on outside ice chest, more easily adsorption system can be repaired, it is only remaining in ice chest Rectifying column, heat exchanger and gas-liquid separator, operating mode are easy to stablize, and are conducive to steadily run whole device;Because only that One ice chest is so as to greatly reduce floor space;Because having used plate-fin heat exchanger and expanding machine, greatly improve and change The thermal efficiency and equipment refrigerating efficiency;Finally, the neon produced is stored in fluid form in Dewar tank, further to save Place facilitates transport, while is reduced to 200 kilograms of pressure by liquid neon pump pressure when needing to charge steel cylinder and is changed by empty baths Steel cylinder is filled with after hot device re-heat, whole process has completely cut off grease and moisture, so as to obtain the neon product of high quality.
Description of the drawings
Fig. 1 is the process flow diagram that ne-He mixture produces pure neon in the prior art.
Fig. 2 is the flow diagram for the method that ne-He mixture of the present invention produces pure neon.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
As shown in Fig. 2, the device of the present invention that pure neon is produced by ne-He mixture includes ice chest 30, the first N2 adsorption Device 33A, the second N2 adsorption device 33B, vacuum pump 34, helium compressor 301, helium expanding machine 3021, helium expanding machine dog point 3022, Liquid neon Dewar 303, liquid neon pump 304 and air-bathing gasifier 305 are wherein provided with the first gas-liquid separator 31, the in ice chest 30 Two gas-liquid separators 32, the first plate-fin heat exchanger 35, the second plate-fin heat exchanger 36, third gas-liquid separator 37, rectifying column 38th, helium expanding machine 3021 and vacuum liquid nitrogen heat exchanger 39;First N2 adsorption device 33A, the second N2 adsorption device 33B, vacuum pump 34, helium Air compressor 301, helium expanding machine dog point 3022, liquid neon Dewar 303, liquid neon pump 304 and air-bathing gasifier 305 are arranged at The outside of ice chest 30;The entrance of first gas-liquid separator 31 is connect with crude Ne-He input channel 310;First gas-liquid point First outlet from device 31 is connect with the entrance of the second gas-liquid separator 32;The first outlet and first of second gas-liquid separator 32 Recycling gas output channel 306 connects;The second outlet of second gas-liquid separator 32 is connect with dirty nitrogen output channel 311;First gas The second outlet of liquid/gas separator 31 is connect with the entrance of the first N2 adsorption device 33A and the entrance of the second N2 adsorption device 33B;First The entrance of the outlet of N2 adsorption device 33A and the outlet of the second N2 adsorption device 33B with third gas-liquid separator 37 is connect;Third gas The first outlet of liquid/gas separator 37 is connect with raw helium output channel 312;The second outlet and rectifying column of third gas-liquid separator 37 38 entrance connection;The first outlet of rectifying column 38 is connect with the second recycling gas output channel 307;The second outlet of rectifying column 38 It is connect with the pure neon entrance of liquid neon Dewar 303;The liquid neon outlet of liquid neon Dewar 303 is connect with the entrance of liquid neon pump 304;Liquid neon pumps 304 outlet is connect with the entrance of air-bathing gasifier 305;The outlet of air-bathing gasifier 305 is connect with gas cylinder;Liquid neon Dewar 303 helium outlet is connect by the first helium pipeline 313 with the entrance of helium compressor 301;The outlet of helium compressor 301 It is connect with the entrance of vacuum liquid nitrogen heat exchanger 39;The outlet of vacuum liquid nitrogen heat exchanger 39 is connect with the entrance of helium expanding machine 3021; The outlet of helium expanding machine 3021 is connect with the helium entrance of liquid neon Dewar 303;The first end of first valve R and the first N2 adsorption device The entrance connection of 33A;The second end of first valve R is connected with the first end of the second valve S, the second end of the second valve S and the The entrance connection of phenodiazine absorber 33B;The first end of third valve T is connect with the entrance of the first N2 adsorption device 33A;Third valve The second end of T is connected with the first end of the 4th valve U, and the second end of the 4th valve U and the entrance of the second N2 adsorption device 33B connect It connects;The second outlet of first gas-liquid separator 31 is connected to the first valve R and by ne-He mixture N2 adsorption device pipeline 309 Between two valve S;4th recycling gas output channel 320 is connected between third valve T and the 4th valve U;4th recycling gas is defeated The other end for going out pipeline 320 is connect with the entrance of vacuum pump 34;The outlet of vacuum pump 34 connects with third recycling gas output channel 308 It connects;The first end of 5th valve V is connect with the outlet of the first N2 adsorption device 33A;The second end of 5th valve V and the 6th valve X First end series connection, the second end of the 6th valve X connect with the outlet of the second N2 adsorption device 33B;With third gas-liquid separator 37 Entrance connection pure ne-He mixture discharge line 315 be connected between the 5th valve V and the 6th valve X;With the first gas-liquid The ne-He mixture N2 adsorption device pipeline 309 of the second outlet connection of separator 31, the entrance company with third gas-liquid separator 37 The pure ne-He mixture discharge line 315 connect, the crude Ne-He input channel being connect with the entrance of the first gas-liquid separator 31 310th, the dirty nitrogen output channel 311 that is connect with the second outlet of the second gas-liquid separator 32, the with third gas-liquid separator 37 The raw helium output channel 312 of one outlet connection is connected to the helium outlet of liquid neon Dewar 303 and the entrance of helium compressor 301 Between the first helium pipeline 313 and be connected to the outlet of helium compressor 301 and vacuum liquid nitrogen heat exchanger 39 entrance it Between the second helium pipeline 314 connect with the first plate-fin heat exchanger 35 and with the first plate-fin heat exchanger 35 formed exchange heat Relationship;The pure ne-He mixture discharge line 315 and third gas-liquid separator 37 being connect with the entrance of third gas-liquid separator 37 First outlet connection raw helium output channel 312, be connected to the helium outlet of liquid neon Dewar 303 with helium compressor 301 The first helium pipeline 313 between entrance and it is connected to the outlet of vacuum liquid nitrogen heat exchanger 39 and the entrance of helium expanding machine 3021 Between third helium pipeline 316 connect with the second plate-fin heat exchanger 36 and with the second plate-fin heat exchanger 36 formation change Hot relationship.
The first N2 adsorption device 33A and the second N2 adsorption device 33B is worked alternatively, when the first N2 adsorption device 33A works When, the second N2 adsorption device 33B is reversely depressured to vacuum to regenerate the second N2 adsorption device 33B by vacuum pump 34;By the first nitrogen The ne-He mixture for having removed nitrogen of the outlet discharge of absorber 33A is mixed by a 5th valve V parts into pure neon helium Gas discharge line 315 is closed, another part sucks the second N2 adsorption device 33B by the 6th valve X by vacuum pump 34, the second nitrogen is inhaled Adnexa 33B carries out pulse cleaning, is then recycled through the 4th valve U, the 4th recycling gas output channel 320, vacuum pump 34 by third Air bag is removed in the recycling of gas output channel 308;When the second N2 adsorption device 33B works, the first N2 adsorption device 33A is by vacuum pump 34 Vacuum is depressured to regenerate the first N2 adsorption device 33A;The neon for having removed nitrogen discharged by the outlet of the second N2 adsorption device 33B Helium gas mixture enters pure ne-He mixture discharge line 315 by a 6th valve X parts, and another part is passed through by vacuum pump 34 5th valve V sucks the first N2 adsorption device 33A, pulse cleaning is carried out to the first N2 adsorption device 33A, then through third valve T, the Four recycling gas output channels 320, vacuum pump 34 remove air bag by 308 recycling of third recycling gas output channel.
The first N2 adsorption device 33A and the second N2 adsorption device 33B by the lithium dimer sieve for being easy to adsorb nitrogen molecular and It is easy to adsorb the carbon molecular sieve composition of oxygen molecule, a small amount of nitrogen and minute quantity oxygen present in ne-He mixture are fallen in absorption respectively Gas.
The vacuum liquid nitrogen heat exchanger 39 is pumped to vacuum pressure 50mbar hereinafter, liquid in vacuum liquid nitrogen heat exchanger 39 The temperature of nitrogen is less than 65K.
Pipeline with helium entrance and helium the outlet connection of liquid neon Dewar 303 is vacuum heat-insulated pipe.
Included the following steps using device of the present invention by the method that ne-He mixture produces pure neon:
The crude Ne-He containing nitrogen that upstream pressure is 30 kilograms or so inputs ice chest through crude Ne-He input channel 310 30,65K or so is cooled to by the first plate-fin heat exchanger 35 first so that enter first after the nitrogen partial liquefaction wherein contained Gas-liquid separator 31, obtained ne-He mixture enter ne-He mixture nitrogen by the second outlet of the first gas-liquid separator 31 and inhale Adnexa pipeline 309, subsequently into after 35 re-heat of the first plate-fin heat exchanger enter the first N2 adsorption device 33A or the second N2 adsorption device 33B, the first N2 adsorption device 33A and the second N2 adsorption device 33B are by the lithium dimer sieve for being easy to adsorb nitrogen molecular and are easy to (or the first N2 adsorption device and the second N2 adsorption device are equipped with adsorption of nitrogen and oxygen to the carbon molecular sieve composition of absorption oxygen molecule Adsorbent, for adsorbing nitrogen present in ne-He mixture and oxygen), absorption respectively is fallen few present in ne-He mixture Measure nitrogen and minute quantity oxygen;The first N2 adsorption device 33A and the second N2 adsorption device 33B is worked alternatively, when the first nitrogen is inhaled When adnexa 33A works, the second N2 adsorption device 33B is reversely depressured to vacuum to regenerate the second N2 adsorption device by vacuum pump 34 33B;By the ne-He mixture for having removed nitrogen that the outlet of the first N2 adsorption device 33A is discharged by a 5th valve V parts Into pure ne-He mixture discharge line 315, another part sucks the second N2 adsorption device by vacuum pump 34 by the 6th valve X 33B carries out pulse cleaning to the second N2 adsorption device 33B, then through the 4th valve U, the 4th recycling gas output channel 320, vacuum Pump 34 removes air bag by 308 recycling of third recycling gas output channel;When the second N2 adsorption device 33B works, the first N2 adsorption Device 33A is depressured to vacuum to regenerate the first N2 adsorption device 33A by vacuum pump 34;It is discharged by the outlet of the second N2 adsorption device 33B The ne-He mixture for having removed nitrogen enters pure ne-He mixture discharge line 315, another portion by a 6th valve X parts Divide and the first N2 adsorption device 33A is sucked by the 5th valve V by vacuum pump 34, pulse cleaning is carried out to the first N2 adsorption device 33A, so Degassing is recycled by third recycling gas output channel 308 by third valve T, the 4th recycling gas output channel 320, vacuum pump 34 Capsule;
After the nitrogen-rich liquid obtained by the first gas-liquid separator 31 is throttled to 1.5 kilograms or so of pressure, pass through first The first outlet of gas-liquid separator 31 enters the second gas-liquid separator 32, and the obtained gas containing neon flashed off passes through The first outlet of second gas-liquid separator 32 enters the first recycling gas output channel 306, and air bag is removed in direct cooling box recycling;And it obtains To the liquid nitrogen fraction being further enriched with dirty nitrogen output channel 311 is then entered by the second outlet of the second gas-liquid separator 32, by It is directly vented as dirty nitrogen after first plate-fin heat exchanger, 35 re-heat;
It is mixed by the pure ne-He mixture of the first N2 adsorption device 33A or the second N2 adsorption device 33B after purification into pure neon helium Gas discharge line 315 cools down so that temperature drops to via the first plate-fin heat exchanger 35 and the second plate-fin heat exchanger 36 25K or so so that most neon component liquefaction therein, subsequently into third gas-liquid separator 37, obtaining the overwhelming majority is The raw helium gas of helium and the thick liquid neon rich in neon component, wherein raw helium gas are entered by the first outlet of third gas-liquid separator 37 Raw helium output channel 312 fills bottle via after 35 re-heat of the second plate-fin heat exchanger 36 and the first plate-fin heat exchanger by compressor Or enter lower purification procedures together;And thick liquid neon is then flowed out by the second outlet of third gas-liquid separator 37, into essence Tower 38 is evaporated, further rectifying obtains pure liquid neon and the neon containing part helium;Wherein the neon containing helium passes through rectifying column 38 first outlet enters the second recycling gas output channel 307, direct cooling box recycling;And pure liquid neon then passes through rectifying column 38 Second outlet flows out, and being sent into liquid neon Dewar 303 by vacuum heat-insulated pipe stores.
When needing to take out neon, then the liquid neon in liquid neon Dewar 303 is pressurized to 200 kilograms of pressure by liquid neon pump 304 Power is sent into gas cylinder after being sent into the gasification of air-bathing gasifier 305 in downstream, and packaging is taken out.
The cold of ice chest 30 is provided by the liquid nitrogen under vacuum and helium compression expansion cycles, and helium passes through the first helium pipeline 313 enter helium compressor 301, and 4 kilograms or so of pressure is compressed to via helium compressor 301, passes through the second helium pipeline 314 enter the first plate-fin heat exchangers 35, by the first plate-fin heat exchanger 35 by helium gas cooling to 80K or so, into having very The vacuum liquid nitrogen heat exchanger 39 of empty liquid nitrogen, vacuum liquid nitrogen heat exchanger 39 is pumped to vacuum pressure 50mbar hereinafter, vacuum liquid nitrogen changes Liquid nitrogen in hot device 39 is less than the low temperature liquid nitrogen of 65K for temperature, and the low temperature liquid nitrogen that the helium that temperature is 80K is 65K with temperature changes Heat obtains temperature close to the helium of 65K or so, enters the second plate-fin heat exchanger 36 further by third helium pipeline 316 Be cooled to 32K or so, into helium expanding machine 3021, be expanded into 1.5 kilograms or so of pressure so that the temperature of helium further under 23K or so is dropped to, enters liquid neon Dewar 303 via vacuum heat-insulated pipe, with the liquid neon evaporated in coolant neon Dewar 303, so Helium after exchanging heat afterwards exports outflow by the helium of liquid neon Dewar 203, ice chest 30 is returned to by vacuum heat-insulated pipe, into first Helium pipeline 313 via the second plate-fin heat exchanger 36 and 35 re-heat of the first plate-fin heat exchanger to room temperature, enters back into helium pressure Contracting machine 301, moves in circles, so as to achieve the purpose that refrigeration.
Compared with prior art, it is of the present invention that the devices and methods therefor of pure neon is produced with following by ne-He mixture Advantage:
By the way that N2 adsorption device is placed on except ice chest, the process of hot reactivation in the cold state is avoided, avoids ice chest In violent operating mode variation, so as to significantly improve the design of the thermal stress of ice chest, also avoid because the heating repeated again Raw and possible caused leakage;By the way that adsorption system is placed on outside ice chest, more easily adsorption system can be repaired, Plate-fin heat exchanger, rectifying column and gas-liquid separator are only left in ice chest, operating mode is easy to stablize, and is conducive to steadily run Whole device.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore, These modifications or improvements without departing from theon the basis of the spirit of the present invention belong to the scope of protection of present invention.

Claims (10)

1. a kind of device that pure neon is produced by ne-He mixture, which is characterized in that described device includes ice chest, the first N2 adsorption Device, the second N2 adsorption device, vacuum pump, helium compressor, helium expanding machine, helium expanding machine dog point, liquid neon Dewar, liquid neon pump and sky The first gas-liquid separator, the second gas-liquid separator, the first plate-fin heat exchanger, are provided in bathing gasifier, wherein ice chest Two plate-fin heat exchangers, third gas-liquid separator, rectifying column, helium expanding machine and vacuum liquid nitrogen heat exchanger;First N2 adsorption device, Phenodiazine absorber, vacuum pump, helium compressor, helium expanding machine dog point, liquid neon Dewar, liquid neon pump and air-bathing gasifier are all provided with It puts in the outside of ice chest;The entrance of first gas-liquid separator is connect with crude Ne-He input channel;First gas-liquid separation The first outlet of device is connect with the entrance of the second gas-liquid separator;The first outlet of second gas-liquid separator and the first recycling gas are defeated Go out pipeline connection;The second outlet of second gas-liquid separator is connect with dirty nitrogen output channel;The second of first gas-liquid separator goes out Mouth is connect with the entrance of the first N2 adsorption device and the entrance of the second N2 adsorption device;The outlet of first N2 adsorption device and the second nitrogen are inhaled Entrance of the outlet of adnexa with third gas-liquid separator is connect;The first outlet of third gas-liquid separator and raw helium output channel Connection;The second outlet of third gas-liquid separator and the entrance of rectifying column connect;The first outlet of rectifying column and the second recycling gas Output channel connects;The second outlet of rectifying column is connect with the pure neon entrance of liquid neon Dewar;The liquid neon outlet of liquid neon Dewar and liquid The entrance connection of neon pump;The outlet of liquid neon pump and the entrance of air-bathing gasifier connect;The outlet of air-bathing gasifier and gas cylinder Connection;The helium outlet of liquid neon Dewar is connected by the entrance of the first helium pipeline and helium compressor;Helium compressor goes out Mouth is connect with the entrance of vacuum liquid nitrogen heat exchanger;The outlet of vacuum liquid nitrogen heat exchanger is connect with the entrance of helium expanding machine;Helium expands The outlet of machine is connect with the helium entrance of liquid neon Dewar;The first end of first valve is connect with the entrance of the first N2 adsorption device;The The second end of one valve is connected with the first end of the second valve, and the second end of the second valve and the entrance of the second N2 adsorption device connect It connects;The first end of third valve is connect with the entrance of the first N2 adsorption device;The second end of third valve and the first of the 4th valve End series connection, the second end of the 4th valve are connect with the entrance of the second N2 adsorption device;The second outlet of first gas-liquid separator passes through Ne-He mixture N2 adsorption device pipeline is connected between the first valve and the second valve;4th recycling gas output channel is connected to the Between three valves and the 4th valve;The other end of 4th recycling gas output channel and the entrance of vacuum pump connect;Vacuum pump goes out Mouth is connect with third recycling gas output channel;The first end of 5th valve is connect with the outlet of the first N2 adsorption device;5th valve Second end connect with the first end of the 6th valve, the second end of the 6th valve is connect with the outlet of the second N2 adsorption device;With The pure ne-He mixture discharge line of the entrance connection of three gas-liquid separators is connected between the 5th valve and the 6th valve;With The ne-He mixture N2 adsorption device pipeline of the second outlet connection of one gas-liquid separator is connect with the entrance of third gas-liquid separator Pure ne-He mixture discharge line, connect with the entrance of the first gas-liquid separator crude Ne-He input channel, with the second gas The dirty nitrogen output channel of the second outlet connection of liquid/gas separator, the raw helium output being connect with the first outlet of third gas-liquid separator Pipeline, be connected to liquid neon Dewar helium outlet the entrance of helium compressor between the first helium pipeline and be connected to helium The second helium pipeline between the outlet of air compressor and the entrance of vacuum liquid nitrogen heat exchanger connects with the first plate-fin heat exchanger It connects and forms heat exchanging relation with the first plate-fin heat exchanger;The pure ne-He mixture being connect with the entrance of third gas-liquid separator Discharge line, the raw helium output channel being connect with the first outlet of third gas-liquid separator, the helium for being connected to liquid neon Dewar go out It the first helium pipeline mouthful between the entrance of helium compressor and is connected to the outlet of vacuum liquid nitrogen heat exchanger and is expanded with helium Third helium pipeline between the entrance of machine connect with the second plate-fin heat exchanger and is formed with the second plate-fin heat exchanger Heat exchanging relation.
2. device as described in claim 1, which is characterized in that the first N2 adsorption device and the second N2 adsorption device alternating work Make, when the first N2 adsorption device works, the second N2 adsorption device is reversely depressured to vacuum by vacuum pump to regenerate the suction of the second nitrogen Adnexa;The ne-He mixture for having removed nitrogen discharged by the outlet of the first N2 adsorption device enters by a 5th valve part Pure ne-He mixture discharge line, another part suck the second N2 adsorption device by the 6th valve by vacuum pump, the second nitrogen are inhaled Adnexa carries out pulse cleaning, then recycles gas output channel by third through the 4th valve, the 4th recycling gas output channel, vacuum pump Air bag is removed in recycling;When the second N2 adsorption device works, the first N2 adsorption device is depressured to vacuum to regenerate first by vacuum pump N2 adsorption device;By the ne-He mixture for having removed nitrogen that the outlet of the second N2 adsorption device is discharged by a 6th valve part Into pure ne-He mixture discharge line, another part sucks the first N2 adsorption device by vacuum pump by the 5th valve, to first N2 adsorption device carries out pulse cleaning, then through third valve, the 4th recycling gas output channel, vacuum pump by third recycling gas output Pipeline recycles degassing capsule.
3. device as described in claim 1, which is characterized in that the vacuum liquid nitrogen heat exchanger is extracted into vacuum pressure 50mbarA Hereinafter, vacuum liquid nitrogen heat exchanger, helium compressor and helium expanding machine composition recycle to provide the cold needed for device.
4. device as described in claim 1, which is characterized in that be equipped with the first gas-liquid separator and second in 63-70K warm areas Gas-liquid separator is equipped with the first N2 adsorption device and the second N2 adsorption device, for removing in thick ne-He mixture in room temperature warm area Nitrogen component;Helium expanding machine, third gas-liquid separator and rectifying column are installed in 20-35K warm areas to be used for pure ne-He mixture In neon separation.
5. device as described in claim 1, which is characterized in that the first N2 adsorption device and the second N2 adsorption device are used to inhale It is attached fall ne-He mixture present in nitrogen and oxygen.
6. device as described in claim 1, which is characterized in that the vacuum liquid nitrogen heat exchanger is pumped to vacuum pressure 50mbarA is hereinafter, the temperature of the liquid nitrogen in vacuum liquid nitrogen heat exchanger is less than 65K.
7. device as described in claim 1, which is characterized in that the pipe with helium entrance and helium the outlet connection of liquid neon Dewar Road is vacuum heat-insulated pipe.
8. the method for pure neon is produced by ne-He mixture using claim 1-7 any one of them device, which is characterized in that institute The method of stating includes the following steps:
Crude Ne-He containing nitrogen inputs ice chest through crude Ne-He input channel, is cooled down first by the first plate-fin heat exchanger, So that entering the first gas-liquid separator after the nitrogen partial liquefaction wherein contained, obtained ne-He mixture passes through the first gas-liquid point Second outlet from device enters ne-He mixture N2 adsorption device pipeline, subsequently into entering the after the first plate-fin heat exchanger re-heat One N2 adsorption device or the second N2 adsorption device, the first N2 adsorption device and the second N2 adsorption device are equipped with the absorption of adsorption of nitrogen and oxygen Agent, for adsorbing nitrogen present in ne-He mixture and oxygen;The first N2 adsorption device and the second N2 adsorption device are handed over Temporary substitute is made, and when the first N2 adsorption device works, the second N2 adsorption device is reversely depressured to vacuum by vacuum pump to regenerate second N2 adsorption device;By the ne-He mixture for having removed nitrogen that the outlet of the first N2 adsorption device is discharged by a 5th valve part Into pure ne-He mixture discharge line, another part sucks the second N2 adsorption device by vacuum pump by the 6th valve, to second N2 adsorption device carries out pulse cleaning, then through the 4th valve, the 4th recycling gas output channel, vacuum pump by third recycling gas output Pipeline recycles degassing capsule;When the second N2 adsorption device works, the first N2 adsorption device is depressured to vacuum to regenerate by vacuum pump First N2 adsorption device;The ne-He mixture for having removed nitrogen discharged by the outlet of the second N2 adsorption device passes through the 6th valve one Part enters pure ne-He mixture discharge line, and another part sucks the first N2 adsorption device by vacuum pump by the 5th valve, right First N2 adsorption device carries out pulse cleaning, then recycles gas by third through third valve, the 4th recycling gas output channel, vacuum pump Air bag is removed in output channel recycling;
After the nitrogen-rich liquid throttling obtained by the first gas-liquid separator, enter the by the first outlet of the first gas-liquid separator Two gas-liquid separators, the obtained gas containing neon flashed off enter the by the first outlet of the second gas-liquid separator Air bag is removed in one recycling gas output channel, direct cooling box recycling;Obtained from the liquid nitrogen fraction that is further enriched with then by the second gas The first outlet of liquid/gas separator enters dirty nitrogen output channel, by directly being put as dirty nitrogen after the first plate-fin heat exchanger re-heat It is empty;
Pure ne-He mixture discharge line is entered by the pure ne-He mixture of the first N2 adsorption device or the second N2 adsorption device after purification, It is cooled down via the first plate-fin heat exchanger and the second plate-fin heat exchanger so that its temperature declines, so that neon group therein Liquid separation subsequently into third gas-liquid separator, obtains raw helium gas and the thick liquid neon rich in neon component, and wherein raw helium gas passes through The first outlet of three gas-liquid separators enters raw helium output channel, via the second plate-fin heat exchanger and the first plate-fin heat exchanger Bottle is filled by compressor after re-heat or enters lower purification procedures together;And thick liquid neon then passes through the second of third gas-liquid separator Outlet outflow, into rectifying column, further rectifying obtains pure liquid neon and the neon containing part helium;The wherein neon containing helium Gas enters the second recycling gas output channel, direct cooling box recycling by the first outlet of rectifying column;And pure liquid neon then passes through essence The second outlet outflow of tower is evaporated, the storage of liquid neon Dewar is sent by vacuum heat-insulated pipe.
9. method as claimed in claim 8, which is characterized in that when needing to take out neon, then pumped by liquid neon by liquid neon Dewar In liquid neon be pressurized to 200 kilograms of pressure, be sent into gas cylinder after being sent into the air-bathing gasifier gasification in downstream, packaging is taken out.
10. method as claimed in claim 8, which is characterized in that the cold of ice chest is by being extracted into below vacuum pressure 50mbarA Liquid nitrogen of the temperature less than 65K and helium compression expansion cycles in vacuum liquid nitrogen heat exchanger provide, and helium passes through the first helium tube Road enters helium compressor, after being compressed via helium compressor, enters the first plate-fin heat exchanger by the second helium pipeline, by First plate-fin heat exchanger is by helium gas cooling, subsequently into the vacuum liquid nitrogen heat exchanger for having vacuum liquid nitrogen, the heat exchange of vacuum liquid nitrogen Device is pumped to vacuum pressure 50mbarA hereinafter, the liquid nitrogen in vacuum liquid nitrogen heat exchanger is less than the low temperature liquid nitrogen of 65K, helium for temperature Gas by third helium pipeline into the second plate-fin heat exchanger with after low temperature liquid nitrogen heat exchange cooling, further being cooled down, Ran Houjin Enter helium expander so that the temperature of helium further declines, and then enters liquid neon Dewar via vacuum heat-insulated pipe, with cold But the liquid neon evaporated in liquid neon Dewar, the helium after then exchanging heat exports outflow by the helium of liquid neon Dewar, by vacuum insulation Pipeline returns to ice chest, into the first helium pipeline, via the second plate-fin heat exchanger and the first plate-fin heat exchanger re-heat to often Temperature enters back into helium compressor.
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CN202522015U (en) * 2012-03-28 2012-11-07 上海启元空分技术发展股份有限公司 Neon and helium separation and purification device with refrigeration equipment
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