CN106052302A - Method for separating <22>Ne from neon - Google Patents
Method for separating <22>Ne from neon Download PDFInfo
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- CN106052302A CN106052302A CN201610627759.1A CN201610627759A CN106052302A CN 106052302 A CN106052302 A CN 106052302A CN 201610627759 A CN201610627759 A CN 201610627759A CN 106052302 A CN106052302 A CN 106052302A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
- F25J3/028—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/02—Processes or apparatus using separation by rectification in a single pressure main column system
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/04—Mixing or blending of fluids with the feed stream
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/32—Neon
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2220/00—Processes or apparatus involving steps for the removal of impurities
- F25J2220/90—Separating isotopes of a component, e.g. H2, O2
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/02—Recycle of a stream in general, e.g. a by-pass stream
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2270/00—Refrigeration techniques used
- F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
Abstract
The invention provides a method for separating <22>Ne from neon. The method is carried out through a low-temperature fractionation method. The method mainly comprises the following steps: combining high-purity Ne feed gas and circulating neon, and then compressing and cooling; then feeding into a separating device (2); sequentially cooling through a high-temperature section heat exchanger (3), a liquid nitrogen cooler (4) and a low-temperature section heat exchanger (6) to obtain low-temperature neon; dividing the low-temperature neon into two parts; treating one part by throttling and pressure reducing through an adjusting valve (7) and then feeding into a rectifying column (11) for rectifying; treating another part by throttling and pressure reducing through an adjusting valve (8) to obtain liquid Ne, and then conveying the liquid Ne into a condensing evaporator (9) to be used as a cold source, wherein mixed neon, mainly containing <20>Ne, generated at the evaporating side of the condensing evaporator and the top of the rectifying column is subjected to cold recovery after being combined and then exhausted; refrigerating circulating neon generated on the top part of the condensing evaporator is subjected to the cold recovery and then used for generating circulating neon; a <22>Ne liquid product is output from the bottom part of the rectifying column. With the adoption of the method, the purity and output of the <22>Ne are superior to those of prior art.
Description
Technical field
The present invention relates to a kind of isotopic process for separation and purification of Ne, be specifically related to a kind of cryogenic rectification method that passes through from neon
Middle separation22The method of Ne.
Background technology
Ne(neon) it is a kind of chemical element, its atomic number is 10, exists with simple substance, referred to as neon in nature,
It it is a kind of rare noble gas.Ne mainly has three kinds of isotopes:20Ne、21Ne and22Ne, wherein20Ne accounts for 90.48%,22Ne accounts for 9.25%, and21Ne the most only accounts for small part.
In prior art, " The Journal Of Chemical Physics " the 24th phase in 1956 reports Ke Laoxiu
This et al. prepared more than 99% with general Clusius-Dickel column22Ne and20Ne's and 13%21Ne, then makees auxiliary with deuterium methane
Gas is helped to incite somebody to action21Ne is further concentrated to 99.6%；And in 1940, the research team of Clausius was successfully extracted 99.8%
's20Ne's and 99.7%22Each 2.5 liters of Ne.
United States Atomic Energy Commission's Mound laboratory report in 1969, they use four post level Four Thermal Diffusion Column cascades point
From neon isotope, it is possible to obtain 99.95% with the yield of 4.2 liters/day20Ne, obtains 2.0% with the yield of 0.56 liter/day21Ne, obtains 99.8% with the yield of 0.22 liter/day22Ne.But, use the method to prepare abundant Ne isotope gas,
Often exist and yield poorly and the defect of production cycle length.
Additionally, Chinese patent CN1513587A discloses abundance in one22The isotopic process for separation and purification of Ne, the method
Mainly comprising the steps that and neon unstripped gas is passed through the cylindrical retention tower with chiller, described retention tower has 1 ~ 5 level
Connection, tower central authorities are provided with vertical heating wire, heat this heating wire,22Ne component diffuses up along this heating wire,22Ne component is along cold
Wall spreads downwards, collects22Ne component i.e. obtains the middle abundance separated22Ne gas；Gained22The abundance of Ne gas is 40-60%, produces
Amount is about 2.2L/ days.
At present, thermal diffusion method is method more ripe during Ne isotopic separation purifies, but thermal diffusion method yet suffers from producing
Measure low, the defect such as cycle length, it is also unsuitable for large-scale industrial production.
Therefore, a kind of separation being suitable to large-scale industrial production is developed22The method of Ne, becomes the research and development of current this area
One of study hotspot of personnel.
Summary of the invention
It is contemplated that overcome many disadvantages present in above-mentioned prior art, and one is provided to divide from neon efficiently
Separate out high-purity22The method of Ne.For reaching this purpose, inventor intends using cryogenic rectification method, high-purity to isolate on a large scale
Degree22Ne, and obtain the yield meeting demand.
Therefore, the invention provides a kind of separation from neon22The method of Ne, it uses cryogenic rectification method to implement, and wraps
Include following steps:
High-purity N e unstripped gas is merged with circulation neon, is conveyed into compressor 1 and is compressed to 7 ~ 9 MPa(g), the most cooled device enters
Row cooling, obtains the neon of compression cooling；Then, the neon of described compression cooling is conveyed into separation equipment 2；
In described separation equipment 2: the neon of described compression cooling is introduced into high-temperature section heat exchanger 3 and lowers the temperature, and subsequently enters
Liquid nitrogen cooler 4 cools down further, finally enters low-temperature zone heat exchanger 6 and cools down further, exports low temperature neon；Described low temperature neon
Gas splits into two strands, and wherein one is by regulation valve 7 expenditure and pressure to 0.1～0.2MPa(g) after, enter rectifying column 11 and carry out essence
Evaporate；Wherein another stock is by regulation valve 8 expenditure and pressure to 0.02MPa(g) after, generate liquid Ne, be conveyed into and be arranged on rectification
The condenser/evaporator 9 at tower 11 top and as low-temperature receiver；Wherein, described liquid nitrogen cooler 4, described low-temperature zone heat exchanger 6, described essence
Evaporate tower 11 and described condenser/evaporator 9 is all housed inside in the space that cold screen 5 surrounds, and described space keeps 1 × 10-6Pa to 1
×10-2The vacuum of Pa；Wherein, the internal logical liquid nitrogen of described cold screen 5, for maintaining the worst cold case in described space；
Wherein, described rectifying column 11 is internal is filled with structured packing, mainly contains in neon to be separated22Ne and20Ne component；Its
In,22Ne boiling point is of a relatively high, gathers the most in a liquid；20Ne boiling point is relatively low, therefore gathers in gas.
Described condenser/evaporator 9 has condenser/evaporator shell 10, and the bottom of described rectifying column 11 is provided with at the bottom of rectifying column
Electric heater 12, obtains rising gas to the heating of tower bottom liquid body by electric heater 12 at the bottom of this rectifying column；Described condenser/evaporator 9
Condensation side produces condensation Ne liquid, is back in described rectifying column 11, becomes the dropping liq in tower；Described condenser/evaporator 9
Evaporation side produces one respectively with described rectifying column 11 tower top and mainly contains20The mixing neon of Ne, exports from described rectifying column 11 again
Merge, reclaim cold through described low-temperature zone heat exchanger 6 and described high-temperature section heat exchanger 3 successively, afterwards from described separation equipment 2 row
Go out；The top of described condenser/evaporator 9 generates kind of refrigeration cycle neon, successively through described low-temperature zone heat exchanger 6 and described high temperature section
After heat exchanger 3 reclaims cold, generate described circulation neon；
Wherein, the evaporating pressure of condenser/evaporator 9 described in the pressure ratio in described rectifying column 11 is high, creates described condensation evaporation
The temperature difference of device 9 both sides, makes both sides heat to exchange；Condenser/evaporator 9 condensation side temperature is higher more than 1 DEG C than evaporation side temperature
Time, heat exchange can be carried out.
Wherein, along with the carrying out of rectification,22Ne liquid is constantly enriched with in the bottom of described rectifying column 11, until purity reaches
After 99.9%, as22Ne fluid product exports from the bottom of described rectifying column 11.
Preferably, in the above-mentioned methods, in described cooler is arranged on described compressor 1 or independent of described compressor
1 is arranged.
Preferably, in the above-mentioned methods, in described separation equipment 2, the neon of described compression cooling is introduced into high temperature section
Heat exchanger 3 is cooled to-140 DEG C ~-150 DEG C, subsequently enters liquid nitrogen cooler 4 and is cooled further to-188 DEG C ~-195 DEG C, finally
Enter low-temperature zone heat exchanger 6 and be cooled further to-218 DEG C ~-225 DEG C, export low temperature neon.
It is further preferred that in the above-mentioned methods, in described separation equipment 2, the neon of described compression cooling is introduced into
High-temperature section heat exchanger 3 is cooled to-145 DEG C, subsequently enters liquid nitrogen cooler 4 and is cooled further to-193 DEG C, finally enters low temperature
Section heat exchanger 6 is cooled further to-221 DEG C, exports low temperature neon.
Preferably, in the above-mentioned methods, the low-temperature receiver of described liquid nitrogen cooler 4 is that described separation equipment 2 outside separately provides
Liquid nitrogen or the liquid nitrogen that share internal with described cold screen 5.
Preferably, in the above-mentioned methods, described high-purity N e unstripped gas is 3:32 with the flow-rate ratio of described circulation neon.
Preferably, in the above-mentioned methods, in described separation equipment 2, by regulating one low temperature neon of valve 7 expenditure and pressure
Gas is 3:32 with the flow-rate ratio of another strand of low temperature neon by regulation valve 8 expenditure and pressure.
Compared with prior art, the invention have the advantages that
1. guarantee that the minimum operating temperature in described separation equipment 2 is 24.5K by evacuation and logical liquid nitrogen, and guarantee described cold
Working temperature in the space that screen 5 surrounds, less than 77K, is effectively prevented radiant heat transfer loss, it is achieved that main processes is exhausted
Heat；2. the cold rationally recycling described kind of refrigeration cycle neon and described mixing neon itself is used for cooling down high-purity N e raw material
Gas；3. utilizing regulation valve that described low temperature neon carries out expenditure and pressure, thus produce the low temperature cold of 27.7K, efficient implementation is low
Temperature rectification；4. from the output of the bottom of described rectifying column 1122The purity (abundance) of Ne fluid product up to 99.9%, additionally, yield
The highest.
Accompanying drawing explanation
Fig. 1 is separation from neon of the present invention22The process flow diagram of the method for Ne；
Wherein: 1-compressor, 2-separation equipment, 3-high-temperature section heat exchanger, 4-liquid nitrogen cooler, the cold screen of 5-, 6-low-temperature zone heat exchange
Device, 7-regulates valve, and 8-regulates valve, 9-condenser/evaporator, 10-condenser/evaporator shell, 11-rectifying column, and electricity at the bottom of 12-rectifying column adds
Hot device.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further elaborated, but the present invention is not limited to following embodiment party
Formula.
A kind of separation from neon22The method of Ne, it uses cryogenic rectification method to implement, and comprises the steps:
High-purity N e unstripped gas is merged with circulation neon, is conveyed into compressor 1 and is compressed to 7 ~ 9 MPa(g), the most cooled device enters
Row cooling, obtains the neon of compression cooling；Then, the neon of described compression cooling is conveyed into separation equipment 2；
In described separation equipment 2: the neon of described compression cooling is introduced into high-temperature section heat exchanger 3 and lowers the temperature, and subsequently enters
Liquid nitrogen cooler 4 cools down further, finally enters low-temperature zone heat exchanger 6 and cools down further, exports low temperature neon；Described low temperature neon
Gas splits into two strands, and wherein one is by regulation valve 7 expenditure and pressure to 0.1～0.2MPa(g) after, enter rectifying column 11 and carry out essence
Evaporate；Wherein another stock is by regulation valve 8 expenditure and pressure to 0.02MPa(g) after, generate liquid Ne, be conveyed into and be arranged on rectification
The condenser/evaporator 9 at tower 11 top and as low-temperature receiver；Wherein, described liquid nitrogen cooler 4, described low-temperature zone heat exchanger 6, described essence
Evaporate tower 11 and described condenser/evaporator 9 is all housed inside in the space that cold screen 5 surrounds, and described space keeps 1 × 10-6Pa to 1
×10-2The vacuum of Pa；Wherein, the internal logical liquid nitrogen of described cold screen 5, for maintaining the worst cold case in described space；
Described condenser/evaporator 9 has condenser/evaporator shell 10, and the bottom of described rectifying column 11 is provided with electricity at the bottom of rectifying column and adds
Hot device 12；The condensation side of described condenser/evaporator 9 produces condensation Ne liquid, is back in described rectifying column 11；Described condensation evaporation
The evaporation side of device 9 produces one respectively with described rectifying column 11 tower top and mainly contains20The mixing neon of Ne, defeated from described rectifying column 11
Go out to remerge, reclaim cold through described low-temperature zone heat exchanger 6 and described high-temperature section heat exchanger 3 successively, set from described separation afterwards
Standby 2 discharge；The top of described condenser/evaporator 9 generates kind of refrigeration cycle neon, successively through described low-temperature zone heat exchanger 6 and described height
After temperature section heat exchanger 3 reclaims cold, generate described circulation neon；
Wherein, along with the carrying out of rectification,22Ne liquid is constantly enriched with in the bottom of described rectifying column 11, until purity reaches
After 99.9%, as22Ne fluid product exports from the bottom of described rectifying column 11.
In a preferred embodiment, in described cooler is arranged on described compressor 1 or independent of described compressor 1
Arrange.
In a preferred embodiment, in described separation equipment 2, the neon of described compression cooling is introduced into high temperature section and changes
Hot device 3 is cooled to-140 DEG C ~-150 DEG C, subsequently enters liquid nitrogen cooler 4 and is cooled further to-188 DEG C ~-195 DEG C, the most laggard
Enter low-temperature zone heat exchanger 6 and be cooled further to-218 DEG C ~-225 DEG C, export low temperature neon.
In a further preferred embodiment, in described separation equipment 2, the neon of described compression cooling is introduced into
High-temperature section heat exchanger 3 is cooled to-145 DEG C, subsequently enters liquid nitrogen cooler 4 and is cooled further to-193 DEG C, finally enters low temperature
Section heat exchanger 6 is cooled further to-221 DEG C, exports low temperature neon.
In a preferred embodiment, the low-temperature receiver of described liquid nitrogen cooler 4 is that described separation equipment 2 outside separately provides
Liquid nitrogen or the liquid nitrogen that share internal with described cold screen 5.
In a preferred embodiment, described high-purity N e unstripped gas is 3:32 with the flow-rate ratio of described circulation neon.
In a preferred embodiment, in described separation equipment 2, by regulating one low temperature neon of valve 7 expenditure and pressure
Gas is 3:32 with the flow-rate ratio of another strand of low temperature neon by regulation valve 8 expenditure and pressure.
Embodiment 1
Technological process as shown in Figure 1 is used to isolate from neon22Ne fluid product:
3 Nm/h high-purity N e unstripped gas and 32 Nm/h circulation neon are merged, are conveyed into compressor 1 and are compressed to 7 MPa(g),
The most configured cooler in compressor 1 cools down, and obtains the neon of compression cooling；Then, by described compression cooling
Neon be conveyed into separation equipment 2；The neon of described compression cooling is introduced into high-temperature section heat exchanger 3 and is cooled to-150 DEG C, connect
Entrance liquid nitrogen cooler 4 and be cooled further to-190 DEG C, finally enter low-temperature zone heat exchanger 6 and be cooled further to-220 DEG C,
Output low temperature neon；Wherein, the low-temperature receiver of described liquid nitrogen cooler 4 is the outside liquid nitrogen separately provided of described separation equipment 2；
Then, described low temperature neon is split into two strands, wherein one with the flow of 3 Nm/h by regulation valve 7 expenditure and pressure
To 0.1～0.2MPa(g) after, enter rectifying column 11 and carry out rectification；Wherein another stock with the flow of 32 Nm/h by regulation valve 8
Expenditure and pressure is to 0.02MPa(g) after, generate liquid Ne, be conveyed into and be arranged on the condenser/evaporator 9 at rectifying column 11 top and make
For low-temperature receiver；
Wherein, described liquid nitrogen cooler 4, described low-temperature zone heat exchanger 6, described rectifying column 11 and described condenser/evaporator 9 all quilts
It is contained in the space that cold screen 5 surrounds, and described space keeps 1 × 10-4The vacuum of Pa；Wherein, the internal logical liquid of described cold screen 5
Nitrogen, for maintaining the worst cold case in described space；
Described condenser/evaporator 9 has condenser/evaporator shell 10, and the bottom of described rectifying column 11 is provided with electricity at the bottom of rectifying column and adds
Hot device 12, power is 100W；Obtain rising gas to the heating of tower bottom liquid body by electric heater 12 at the bottom of this rectifying column；Described condensation is steamed
The condensation side sending out device 9 produces condensation Ne liquid, is back in described rectifying column 11, becomes the dropping liq in tower；Described condensation is steamed
The evaporation side sending out device 9 produces one respectively with described rectifying column 11 tower top and mainly contains20The mixing neon of Ne, from described rectifying column 11
Output remerges, wherein containing 95.1%20Ne, flow is 2.767Nm/h, successively through described low-temperature zone heat exchanger 6 and described height
Temperature section heat exchanger 3 reclaims cold, discharges from described separation equipment 2 afterwards；The top of described condenser/evaporator 9 generates kind of refrigeration cycle
Neon, successively after described low-temperature zone heat exchanger 6 and described high-temperature section heat exchanger 3 reclaim cold, generates described circulation neon；
Along with the carrying out of rectification,22Ne liquid is constantly enriched with in the bottom of described rectifying column 11, until after purity reaches 99.9%,
Using the flow of 0.1387 Nm/h as22Ne fluid product exports from the bottom of described rectifying column 11.
Embodiment 2
Technological process as shown in Figure 1 is used to isolate from neon22Ne fluid product:
3 Nm/h high-purity N e unstripped gas and 32 Nm/h circulation neon are merged, are conveyed into compressor 1 and are compressed to 8 MPa(g),
Then the cooler through arranging independent of described compressor 1 cools down, and obtains the neon of compression cooling；Then, by described pressure
The neon of contracting cooling is conveyed into separation equipment 2；The neon of described compression cooling is introduced into high-temperature section heat exchanger 3 and is cooled to-145
DEG C, subsequently enter liquid nitrogen cooler 4 and be cooled further to-193 DEG C, finally enter low-temperature zone heat exchanger 6 be cooled further to-
221 DEG C, export low temperature neon；Wherein, the low-temperature receiver of described liquid nitrogen cooler 4 is the outside liquid separately provided of described separation equipment 2
Nitrogen；
Then, described low temperature neon is split into two strands, wherein one with the flow of 3 Nm/h by regulation valve 7 expenditure and pressure
To 0.1～0.2MPa(g) after, enter rectifying column 11 and carry out rectification；Wherein another stock with the flow of 32 Nm/h by regulation valve 8
Expenditure and pressure is to 0.02MPa(g) after, generate liquid Ne, be conveyed into and be arranged on the condenser/evaporator 9 at rectifying column 11 top and make
For low-temperature receiver；
Wherein, described liquid nitrogen cooler 4, described low-temperature zone heat exchanger 6, described rectifying column 11 and described condenser/evaporator 9 all quilts
It is contained in the space that cold screen 5 surrounds, and described space keeps 1 × 10-4The vacuum of Pa；Wherein, the internal logical liquid of described cold screen 5
Nitrogen, for maintaining the worst cold case in described space；
Described condenser/evaporator 9 has condenser/evaporator shell 10, and the bottom of described rectifying column 11 is provided with electricity at the bottom of rectifying column and adds
Hot device 12, power is 100W；Obtain rising gas to the heating of tower bottom liquid body by electric heater 12 at the bottom of this rectifying column；Described condensation is steamed
The condensation side sending out device 9 produces condensation Ne liquid, is back in described rectifying column 11, becomes the dropping liq in tower；Described condensation is steamed
The evaporation side sending out device 9 produces one respectively with described rectifying column 11 tower top and mainly contains20The mixing neon of Ne, from described rectifying column 11
Output remerges, wherein containing 95.4%20Ne, flow is 2.853Nm/h, successively through described low-temperature zone heat exchanger 6 and described height
Temperature section heat exchanger 3 reclaims cold, discharges from described separation equipment 2 afterwards；The top of described condenser/evaporator 9 generates kind of refrigeration cycle
Neon, successively after described low-temperature zone heat exchanger 6 and described high-temperature section heat exchanger 3 reclaim cold, generates described circulation neon；
Along with the carrying out of rectification,22Ne liquid is constantly enriched with in the bottom of described rectifying column 11, until after purity reaches 99.9%,
Using the flow of 0.1466 Nm/h as22Ne fluid product exports from the bottom of described rectifying column 11.
Embodiment 3
Technological process as shown in Figure 1 is used to isolate from neon22Ne fluid product:
3 Nm/h high-purity N e unstripped gas and 32 Nm/h circulation neon are merged, are conveyed into compressor 1 and are compressed to 9 MPa(g),
Then the cooler through arranging independent of described compressor 1 cools down, and obtains the neon of compression cooling；Then, by described pressure
The neon of contracting cooling is conveyed into separation equipment 2；The neon of described compression cooling is introduced into high-temperature section heat exchanger 3 and is cooled to-140
DEG C, subsequently enter liquid nitrogen cooler 4 and be cooled further to-189 DEG C, finally enter low-temperature zone heat exchanger 6 be cooled further to-
218 DEG C, export low temperature neon；Wherein, the low-temperature receiver of described liquid nitrogen cooler 4 is the liquid nitrogen that shares internal with described cold screen 5；
Then, described low temperature neon is split into two strands, wherein one with the flow of 3 Nm/h by regulation valve 7 expenditure and pressure
To 0.1～0.2MPa(g) after, enter rectifying column 11 and carry out rectification；Wherein another stock with the flow of 32 Nm/h by regulation valve 8
Expenditure and pressure is to 0.02MPa(g) after, generate liquid Ne, be conveyed into and be arranged on the condenser/evaporator 9 at rectifying column 11 top and make
For low-temperature receiver；
Wherein, described liquid nitrogen cooler 4, described low-temperature zone heat exchanger 6, described rectifying column 11 and described condenser/evaporator 9 all quilts
It is contained in the space that cold screen 5 surrounds, and described space keeps 1 × 10-4The vacuum of Pa；Wherein, the internal logical liquid of described cold screen 5
Nitrogen, for maintaining the worst cold case in described space；
Described condenser/evaporator 9 has condenser/evaporator shell 10, and the bottom of described rectifying column 11 is provided with electricity at the bottom of rectifying column and adds
Hot device 12, power is 100W；Obtain rising gas to the heating of tower bottom liquid body by electric heater 12 at the bottom of this rectifying column；Described condensation is steamed
The condensation side sending out device 9 produces condensation Ne liquid, is back in described rectifying column 11, becomes the dropping liq in tower；Described condensation is steamed
The evaporation side sending out device 9 produces one respectively with described rectifying column 11 tower top and mainly contains20The mixing neon of Ne, from described rectifying column 11
Output remerges, wherein containing 95.3%20Ne, flow is 2.844Nm/h, successively through described low-temperature zone heat exchanger 6 and described height
Temperature section heat exchanger 3 reclaims cold, discharges from described separation equipment 2 afterwards；The top of described condenser/evaporator 9 generates kind of refrigeration cycle
Neon, successively after described low-temperature zone heat exchanger 6 and described high-temperature section heat exchanger 3 reclaim cold, generates described circulation neon；
Along with the carrying out of rectification,22Ne liquid is constantly enriched with in the bottom of described rectifying column 11, until after purity reaches 99.9%,
Using the flow of 0.1438 Nm/h as22Ne fluid product exports from the bottom of described rectifying column 11.
Embodiment 4
Technological process as shown in Figure 1 is used to isolate from neon22Ne fluid product:
3 Nm/h high-purity N e unstripped gas and 32 Nm/h circulation neon are merged, are conveyed into compressor 1 and are compressed to 8 MPa(g),
Then the cooler through arranging independent of described compressor 1 cools down, and obtains the neon of compression cooling；Then, by described pressure
The neon of contracting cooling is conveyed into separation equipment 2；The neon of described compression cooling is introduced into high-temperature section heat exchanger 3 and is cooled to-148
DEG C, subsequently enter liquid nitrogen cooler 4 and be cooled further to-195 DEG C, finally enter low-temperature zone heat exchanger 6 be cooled further to-
224 DEG C, export low temperature neon；Wherein, the low-temperature receiver of described liquid nitrogen cooler 4 is the liquid nitrogen that shares internal with described cold screen 5；
Then, described low temperature neon is split into two strands, wherein one with the flow of 3 Nm/h by regulation valve 7 expenditure and pressure
To 0.1～0.2MPa(g) after, enter rectifying column 11 and carry out rectification；Wherein another stock with the flow of 32 Nm/h by regulation valve 8
Expenditure and pressure is to 0.02MPa(g) after, generate liquid Ne, be conveyed into and be arranged on the condenser/evaporator 9 at rectifying column 11 top and make
For low-temperature receiver；
Wherein, described liquid nitrogen cooler 4, described low-temperature zone heat exchanger 6, described rectifying column 11 and described condenser/evaporator 9 all quilts
It is contained in the space that cold screen 5 surrounds, and described space keeps 1 × 10-4The vacuum of Pa；Wherein, the internal logical liquid of described cold screen 5
Nitrogen, for maintaining the worst cold case in described space；
Described condenser/evaporator 9 has condenser/evaporator shell 10, and the bottom of described rectifying column 11 is provided with electricity at the bottom of rectifying column and adds
Hot device 12, power is 100W；Obtain rising gas to the heating of tower bottom liquid body by electric heater 12 at the bottom of this rectifying column；Described condensation is steamed
The condensation side sending out device 9 produces condensation Ne liquid, is back in described rectifying column 11, becomes the dropping liq in tower；Described condensation is steamed
The evaporation side sending out device 9 produces one respectively with described rectifying column 11 tower top and mainly contains20The mixing neon of Ne, from described rectifying column 11
Output remerges, wherein containing 94.9%20Ne, flow is 2.795Nm/h, successively through described low-temperature zone heat exchanger 6 and described height
Temperature section heat exchanger 3 reclaims cold, discharges from described separation equipment 2 afterwards；The top of described condenser/evaporator 9 generates kind of refrigeration cycle
Neon, successively after described low-temperature zone heat exchanger 6 and described high-temperature section heat exchanger 3 reclaim cold, generates described circulation neon；
Along with the carrying out of rectification,22Ne liquid is constantly enriched with in the bottom of described rectifying column 11, until after purity reaches 99.9%,
Using the flow of 0.1417 Nm/h as22Ne fluid product exports from the bottom of described rectifying column 11.
As can be seen here, the method for the invention is used to separate acquisition22The very high purity of Ne fluid product, its average output
Flow is about 1600 times of output flow described in Chinese patent CN1513587A 2.2L/ days.
Being described in detail the specific embodiment of the present invention above, but it is intended only as example, the present invention does not limit
It is formed on particular embodiments described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and
Substitute the most all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and
Amendment, all should contain within the scope of the invention.
Claims (7)
1. one kind separates from neon22The method of Ne, it uses cryogenic rectification method to implement, it is characterised in that comprise the steps:
High-purity N e unstripped gas is merged with circulation neon, is conveyed into compressor (1) and is compressed to 7 ~ 9 MPa(g), the most cooled device
Cool down, obtain the neon of compression cooling；Then, the neon of described compression cooling is conveyed into separation equipment (2)；
In described separation equipment (2): the neon of described compression cooling is introduced into high-temperature section heat exchanger (3) and lowers the temperature, then
Enter liquid nitrogen cooler (4) to cool down further, finally enter low-temperature zone heat exchanger (6) and cool down further, export low temperature neon；Institute
Stating low temperature neon and split into two strands, wherein one is by regulation valve (7) expenditure and pressure to 0.1～0.2MPa(g) after, enter rectification
Tower (11) carries out rectification；Wherein another stock is by regulation valve (8) expenditure and pressure to 0.02MPa(g) after, generate liquid Ne, defeated
Feeding is arranged on the condenser/evaporator (9) at rectifying column (11) top and as low-temperature receiver；Wherein, described liquid nitrogen cooler (4), described
Low-temperature zone heat exchanger (6), described rectifying column (11) and described condenser/evaporator (9) are all housed inside the space that cold screen (5) surrounds
In, and described space holding 1 × 10-6Pa to 1 × 10-2The vacuum of Pa；Wherein, the internal logical liquid nitrogen of described cold screen (5), it is used for
Maintain the worst cold case in described space；
Described condenser/evaporator (9) has condenser/evaporator shell (10), and the bottom of described rectifying column (11) is provided with rectifying column
End electric heater (12)；The condensation side of described condenser/evaporator (9) produces condensation Ne liquid, is back in described rectifying column (11)；
The evaporation side of described condenser/evaporator (9) produces one respectively with described rectifying column (11) tower top and mainly contains20The mixing neon of Ne,
Remerge from described rectifying column (11) output, reclaim through described low-temperature zone heat exchanger (6) and described high-temperature section heat exchanger (3) successively
Cold, discharges from described separation equipment (2) afterwards；The top of described condenser/evaporator (9) generates kind of refrigeration cycle neon, successively warp
After described low-temperature zone heat exchanger (6) and described high-temperature section heat exchanger (3) reclaim cold, generate described circulation neon；
Wherein, along with the carrying out of rectification,22Ne liquid is constantly enriched with in the bottom of described rectifying column (11), until purity reaches
After 99.9%, as22Ne fluid product exports from the bottom of described rectifying column (11).
Method the most according to claim 1, it is characterised in that described cooler be arranged in described compressor (1) or
Arrange independent of described compressor (1).
Method the most according to claim 1, it is characterised in that in described separation equipment (2), the neon of described compression cooling
Gas is introduced into high-temperature section heat exchanger (3) and is cooled to-140 DEG C ~-150 DEG C, subsequently enter liquid nitrogen cooler (4) be cooled further to-
188 DEG C ~-195 DEG C, finally enter low-temperature zone heat exchanger (6) and be cooled further to-218 DEG C ~-225 DEG C, export low temperature neon.
Method the most according to claim 3, it is characterised in that in described separation equipment (2), the neon of described compression cooling
Gas is introduced into high-temperature section heat exchanger (3) and is cooled to-145 DEG C, subsequently enters liquid nitrogen cooler (4) and is cooled further to-193 DEG C,
Finally enter low-temperature zone heat exchanger (6) and be cooled further to-221 DEG C, export low temperature neon.
Method the most according to claim 1, it is characterised in that the low-temperature receiver of described liquid nitrogen cooler (4) is that described separation sets
Standby (2) outside liquid nitrogen separately provided or the liquid nitrogen that share internal with described cold screen (5).
Method the most according to claim 1, it is characterised in that described high-purity N e unstripped gas and the flow of described circulation neon
Ratio is 3:32.
Method the most according to claim 1, it is characterised in that in described separation equipment (2), is saved by regulation valve (7)
One low temperature neon of stream decompression is 3:32 with the flow-rate ratio of another strand of low temperature neon by regulation valve (8) expenditure and pressure.
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