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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- Prior art keywords
- neon
- low
- temperature
- heat exchanger
- rectifying tower
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- 229910052754 neon Inorganic materials 0.000 title claims abstract description 122
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 238000000034 method Methods 0.000 title claims abstract description 37
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 90
- 239000007788 liquid Substances 0.000 claims abstract description 82
- 239000007789 gas Substances 0.000 claims abstract description 57
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 45
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 239000012263 liquid product Substances 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 10
- 238000009833 condensation Methods 0.000 claims description 50
- 230000005494 condensation Effects 0.000 claims description 48
- 238000000926 separation method Methods 0.000 claims description 41
- 239000000203 mixture Substances 0.000 claims description 14
- 230000001105 regulatory effect Effects 0.000 claims description 11
- 230000008020 evaporation Effects 0.000 claims description 7
- 238000011084 recovery Methods 0.000 abstract 2
- -1 containing <20>Ne Chemical compound 0.000 abstract 1
- 238000005194 fractionation Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 238000009792 diffusion process Methods 0.000 description 6
- 230000001174 ascending effect Effects 0.000 description 5
- 238000007599 discharging Methods 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 238000009835 boiling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910052805 deuterium Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005372 isotope separation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
The invention 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 invention relates to a separation and purification method of Ne isotope, in particular to a method for separating neon gas by low-temperature rectification22Ne.
Background
Ne (neon) is a chemical element having an atomic number of 10, which exists as a simple substance in nature, called neon, and is a rare inert gas. Ne has mainly three isotopes:20Ne、21ne and22ne of, wherein20Ne is about 90.48%,22ne is about 9.25%, and21ne then only occupies a small fraction.
In The prior art, it was reported in 1956 that more than 99% Of The total Of Clausius et al prepared by a general thermal diffusion column in The 24 th phase Of The Journal Of Chemical Physics22Ne and20ne and 13%21Ne, then using deuterium methane as an auxiliary gas21Ne was further concentrated to 99.6%; in 1940, the Clausius research team successfully extracted 99.8% of the total20Ne and 99.7% of22Ne 2.5 liters each.
1969, Mound's laboratory report by the American atomic energy Commission, who used a four-column, four-stage thermal diffusion column cascade to separate neon isotopes, and was able to obtain 99.95% of neon isotopes with a yield of 4.2 liters/day20Ne, in a yield of 0.56 l/day, to obtain 2.0%21Ne, yield of 99.8% in 0.22 l/day22Ne. However, the method for preparing high abundance Ne isotope gas often has the defects of low yield and long production period.
In addition, Chinese patent CN1513587A discloses a medium abundance22A method for separating and purifying Ne isotopes, which mainly comprises the following steps: introducing neon raw material gas into a cylindrical diffusion tower with a cooling device, wherein 1-5 diffusion towers are cascaded, a vertical heating wire is arranged in the center of the tower to heat the heating wire,22group NeThe component is diffused upward along the heating wire,22the Ne component diffuses downward along the cold wall and is collected22The Ne component is separated to obtain medium abundance22Ne gas; obtained by22The abundance of Ne gas was 40-60%, and the yield was about 2.2L/day.
At present, the thermal diffusion method is a mature method in Ne isotope separation and purification, but the thermal diffusion method still has the defects of low yield, long period and the like, and is not suitable for large-scale industrial production.
Therefore, a separation suitable for large-scale industrial production was developed22Ne is one of the research focuses of researchers in this field.
Disclosure of Invention
The present invention is directed to overcoming the various deficiencies in the prior art as set forth above and providing a process for efficiently separating neon gas to a high degree of purity22Ne. To achieve this, the inventors propose to use cryogenic rectification to separate high purity on a large scale22Ne, and yield satisfying the demand is obtained.
Accordingly, the present invention provides a process for the separation of neon22A method of Ne, carried out by cryogenic rectification, comprising the steps of:
combining the high-purity Ne feed gas and the circulating neon gas, conveying the mixture into a compressor 1 to be compressed to 7-9 MPa (g), and then cooling the mixture by a cooler to obtain compressed and cooled neon gas; the compressed and cooled neon is then fed into a separation device 2;
within the separation device 2: the compressed and cooled neon enters a high-temperature section heat exchanger 3 for cooling, then enters a liquid nitrogen cooler 4 for further cooling, finally enters a low-temperature section heat exchanger 6 for further cooling, and low-temperature neon is output; the low-temperature neon is divided into two streams, wherein one stream is throttled and decompressed to 0.1-0.2 MPa (g) by an adjusting valve 7 and then enters a rectifying tower 11 for rectification; the other branch is throttled and reduced by the regulating valve 8After the pressure is increased to 0.02MPa (g), liquid Ne is generated and is conveyed into a condensation evaporator 9 arranged at the top of a rectifying tower 11 to be used as a cold source, wherein the liquid nitrogen cooler 4, the low-temperature section heat exchanger 6, the rectifying tower 11 and the condensation evaporator 9 are all accommodated in a space surrounded by a cold screen 5, and the space keeps 1 × 10-6Pa to 1 × 10-2Vacuum degree of Pa; liquid nitrogen is introduced into the cold shield 5 and is used for maintaining the low-temperature working condition in the space;
wherein, the rectifying tower 11 is filled with regular packing, and the neon gas to be separated mainly contains22Ne and20a Ne component; wherein,22ne has a relatively high boiling point and therefore accumulates in the liquid;20ne has a relatively low boiling point and therefore accumulates in the gas.
The condensation evaporator 9 is provided with a condensation evaporator shell 10, the bottom of the rectifying tower 11 is provided with a rectifying tower bottom electric heater 12, and the rectifying tower bottom electric heater 12 heats the tower bottom liquid to obtain the ascending gas; a condensed Ne liquid is generated on the condensation side of the condensation evaporator 9 and refluxed into the rectifying column 11 to become a descending liquid in the column; the evaporation side of the condensation evaporator 9 and the top of the rectifying tower 11 respectively generate a stream of the main component20Ne mixed neon is output from the rectifying tower 11 and then combined, and is sequentially recycled through the low-temperature section heat exchanger 6 and the high-temperature section heat exchanger 3 to recover cold energy, and then is discharged from the separation equipment 2; refrigerating cycle neon is generated at the top of the condensation evaporator 9, and the cycle neon is generated after cold energy is recovered by the low-temperature section heat exchanger 6 and the high-temperature section heat exchanger 3 in sequence;
wherein, the pressure in the rectifying tower 11 is higher than the evaporating pressure of the condensing evaporator 9, so as to generate the temperature difference between two sides of the condensing evaporator 9, and the heat of the two sides can be exchanged; when the temperature of the condensing side of the condensing evaporator 9 is higher than the temperature of the evaporating side by 1 ℃ or more, heat exchange can be performed.
Wherein, as the rectification is carried out,22ne liquid is continuously enriched at the bottom of the rectifying tower 11 until the purity reaches 99.9 percent, and then the Ne liquid is used as22Ne liquid product is output from the bottom of the rectifying column 11.
Preferably, in the above method, the cooler is provided within the compressor 1 or separately from the compressor 1.
Preferably, in the method, in the separation equipment 2, the compressed and cooled neon enters a high-temperature heat exchanger 3 to be cooled to-140 ℃ to-150 ℃, then enters a liquid nitrogen cooler 4 to be further cooled to-188 ℃ to-195 ℃, finally enters a low-temperature heat exchanger 6 to be further cooled to-218 ℃ to-225 ℃, and low-temperature neon is output.
Further preferably, in the above method, in the separation device 2, the compressed and cooled neon enters the high-temperature section heat exchanger 3 to be cooled to-145 ℃, then enters the liquid nitrogen cooler 4 to be further cooled to-193 ℃, and finally enters the low-temperature section heat exchanger 6 to be further cooled to-221 ℃, so as to output low-temperature neon.
Preferably, in the above method, the cold source of the liquid nitrogen cooler 4 is liquid nitrogen independently provided outside the separation device 2 or liquid nitrogen shared with the inside of the cold shield 5.
Preferably, in the above method, the flow ratio of the high purity Ne raw material gas to the recycled neon gas is 3: 32.
Preferably, in the above process, the flow ratio of one stream of low-temperature neon throttled for pressure reduction by regulating valve 7 to the other stream of low-temperature neon throttled for pressure reduction by regulating valve 8 in said separation apparatus 2 is 3: 32.
Compared with the prior art, the invention has the following advantages:
①, ensuring the lowest working temperature in the separation equipment 2 to be 24.5K by vacuumizing and introducing liquid nitrogen, ensuring the working condition temperature in the space surrounded by the cold screen 5 to be lower than 77K, effectively preventing radiation heat transfer loss, realizing the heat insulation of the main process, reasonably recycling the cold energy of the refrigeration cycle neon and the mixed neon for cooling the high-purity Ne feed gas ②;③ the low-temperature neon gas is throttled and decompressed by a regulating valve, thereby generating low-temperature cold of 27.7K and efficiently implementing cryogenic rectification, ④ the low-temperature neon gas is output from the bottom of the rectifying tower 1122The purity (abundance) of Ne liquid product is as high as 99.9%, and besides, the yield is also high.
Drawings
FIG. 1 is a diagram illustrating the separation of neon according to the present invention22A process flow schematic of the method of Ne;
wherein: 1-compressor, 2-separation equipment, 3-high temperature section heat exchanger, 4-liquid nitrogen cooler, 5-cold shield, 6-low temperature section heat exchanger, 7-regulating valve, 8-regulating valve, 9-condensation evaporator, 10-condensation evaporator shell, 11-rectifying tower and 12-rectifying tower bottom electric heater.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the following embodiments.
Separation from neon22A method of Ne, carried out by cryogenic rectification, comprising the steps of:
combining the high-purity Ne feed gas and the circulating neon gas, conveying the mixture into a compressor 1 to be compressed to 7-9 MPa (g), and then cooling the mixture by a cooler to obtain compressed and cooled neon gas; the compressed and cooled neon is then fed into a separation device 2;
within the separation device 2: the compressed and cooled neon enters a high-temperature section heat exchanger 3 for cooling, then enters a liquid nitrogen cooler 4 for further cooling, finally enters a low-temperature section heat exchanger 6 for further cooling, and low-temperature neon is output; the low-temperature neon is divided into two streams, wherein one stream is throttled and decompressed to 0.1-0.2 MPa (g) by an adjusting valve 7 and then enters a rectifying tower 11 for rectification; the other branch is throttled and decompressed by a regulating valve 8After reaching 0.02MPa (g), the generated liquid Ne is conveyed into a condensation evaporator 9 arranged at the top of a rectifying tower 11 to be used as a cold source, wherein the liquid nitrogen cooler 4, the low-temperature section heat exchanger 6, the rectifying tower 11 and the condensation evaporator 9 are all accommodated in a space surrounded by a cold screen 5, and the space keeps 1 × 10-6Pa to 1 × 10-2Vacuum degree of Pa; liquid nitrogen is introduced into the cold shield 5 and is used for maintaining the low-temperature working condition in the space;
the condensation evaporator 9 is provided with a condensation evaporator shell 10, and the bottom of the rectifying tower 11 is provided with a rectifying tower bottom electric heater 12; a condensed Ne liquid is produced on the condensation side of the condensation evaporator 9 and refluxed into the rectifying tower 11; the evaporation side of the condensation evaporator 9 and the top of the rectifying tower 11 respectively generate a stream of the main component20Ne mixed neon is output from the rectifying tower 11 and then combined, and is sequentially recycled through the low-temperature section heat exchanger 6 and the high-temperature section heat exchanger 3 to recover cold energy, and then is discharged from the separation equipment 2; refrigerating cycle neon is generated at the top of the condensation evaporator 9, and the cycle neon is generated after cold energy is recovered by the low-temperature section heat exchanger 6 and the high-temperature section heat exchanger 3 in sequence;
wherein, as the rectification is carried out,22ne liquid is continuously enriched at the bottom of the rectifying tower 11 until the purity reaches 99.9 percent, and then the Ne liquid is used as22Ne liquid product is output from the bottom of the rectifying column 11.
In a preferred embodiment, the cooler is arranged within the compressor 1 or separately from the compressor 1.
In a preferred embodiment, in the separation equipment 2, the compressed and cooled neon enters a high-temperature heat exchanger 3 to be cooled to-140 ℃ to-150 ℃, then enters a liquid nitrogen cooler 4 to be further cooled to-188 ℃ to-195 ℃, finally enters a low-temperature heat exchanger 6 to be further cooled to-218 ℃ to-225 ℃, and low-temperature neon is output.
In a further preferred embodiment, in the separation device 2, the compressed and cooled neon enters the high-temperature section heat exchanger 3 to be cooled to-145 ℃, then enters the liquid nitrogen cooler 4 to be further cooled to-193 ℃, and finally enters the low-temperature section heat exchanger 6 to be further cooled to-221 ℃, so as to output low-temperature neon.
In a preferred embodiment, the cold source of the liquid nitrogen cooler 4 is liquid nitrogen provided separately outside the separation device 2 or shared with the inside of the cold screen 5.
In a preferred embodiment, the flow ratio of the high purity Ne feed gas to the recycled neon gas is 3: 32.
In a preferred embodiment, the flow ratio of one stream of low temperature neon throttled for pressure reduction by regulating valve 7 to the other stream of low temperature neon throttled for pressure reduction by regulating valve 8 in said separation apparatus 2 is 3: 32.
Example 1
The process flow shown in figure 1 is adopted to separate neon gas22Ne liquid product:
carrying out dry distillation on the Ne raw material gas with high purity 3 Nm/h and the neon gas with high purity 32 Nm/h, combining the Ne raw material gas and the neon gas with high purity, conveying the mixture into a compressor 1 to be compressed to 7 MPa (g), and then cooling the mixture by a cooler arranged in the compressor 1 to obtain the compressed and cooled neon gas; the compressed and cooled neon is then fed into a separation device 2; the compressed and cooled neon enters a high-temperature section heat exchanger 3 to be cooled to-150 ℃, then enters a liquid nitrogen cooler 4 to be further cooled to-190 ℃, and finally enters a low-temperature section heat exchanger 6 to be further cooled to-220 ℃, and low-temperature neon is output; wherein the cold source of the liquid nitrogen cooler 4 is liquid nitrogen independently provided outside the separation equipment 2;
then, dividing the low-temperature neon into two strands, throttling and decompressing one strand of low-temperature neon through an adjusting valve 7 at the flow rate of 3 Nm/h to 0.1-0.2 MPa (g), and then rectifying in a rectifying tower 11; wherein the other part is throttled and decompressed to 0.02MPa (g) at a flow rate of 32 Nm/h by an adjusting valve 8, and then the produced liquid Ne is conveyed into a condensation evaporator 9 arranged at the top of a rectifying tower 11 to be used as a cold source;
wherein the liquid nitrogen cooler 4, the low-temperature section heat exchanger 6, the rectifying tower 11 and the condensing evaporator 9 are all accommodated in a space surrounded by a cold screen 5, and the space keeps 1 × 10-4Vacuum degree of Pa; liquid nitrogen is introduced into the cold shield 5 and is used for maintaining the low-temperature working condition in the space;
the condensation evaporator 9 is provided with a condensation evaporator shell 10, the bottom of the rectifying tower 11 is provided with a rectifying tower bottom electric heater 12, and the power is 100W; heating the liquid at the bottom of the tower by the electric heater 12 at the bottom of the rectifying tower to obtain ascending gas; a condensed Ne liquid is generated on the condensation side of the condensation evaporator 9 and refluxed into the rectifying column 11 to become a descending liquid in the column; the evaporation side of the condensation evaporator 9 and the top of the rectifying tower 11 respectively generate a stream of the main component20Ne mixed neon gas containing 95.1% of Ne is discharged from the rectifying tower 11 and recombined20Ne with the flow rate of 2.767 Nm/h, sequentially passing through the low-temperature-stage heat exchanger 6 and the high-temperature-stage heat exchanger 3 to recover cold energy, and then discharging the cold energy from the separation equipment 2; refrigerating cycle neon is generated at the top of the condensation evaporator 9, and the cycle neon is generated after cold energy is recovered by the low-temperature section heat exchanger 6 and the high-temperature section heat exchanger 3 in sequence;
as the distillation is carried out,22ne liquid is continuously enriched at the bottom of the rectification column 11 until the purity reaches 99.9%, and the flow rate of 0.1387 Nm/h is taken as22Ne liquid product is output from the bottom of the rectifying column 11.
Example 2
The process flow shown in figure 1 is adopted to separate neon gas22Ne liquid product:
carrying out labor-intensive cultivation on 3 Nm/h high-purity Ne raw material gas and 32 Nm/h circulating neon gas together, conveying the mixture into a compressor 1 to be compressed to 8 MPa (g), and then cooling the mixture by a cooler which is independent of the compressor 1 to obtain compressed and cooled neon gas; the compressed and cooled neon is then fed into a separation device 2; the compressed and cooled neon enters a high-temperature section heat exchanger 3 to be cooled to-145 ℃, then enters a liquid nitrogen cooler 4 to be further cooled to-193 ℃, and finally enters a low-temperature section heat exchanger 6 to be further cooled to-221 ℃, and low-temperature neon is output; wherein the cold source of the liquid nitrogen cooler 4 is liquid nitrogen independently provided outside the separation equipment 2;
then, dividing the low-temperature neon into two strands, throttling and decompressing one strand of low-temperature neon through an adjusting valve 7 at the flow rate of 3 Nm/h to 0.1-0.2 MPa (g), and then rectifying in a rectifying tower 11; wherein the other part is throttled and decompressed to 0.02MPa (g) at a flow rate of 32 Nm/h by an adjusting valve 8, and then the produced liquid Ne is conveyed into a condensation evaporator 9 arranged at the top of a rectifying tower 11 to be used as a cold source;
wherein the liquid nitrogen cooler 4, the low-temperature section heat exchanger 6, the rectifying tower 11 and the condensing evaporator 9 are all accommodated in a space surrounded by a cold screen 5, and the space keeps 1 × 10-4Vacuum degree of Pa; liquid nitrogen is introduced into the cold shield 5 and is used for maintaining the low-temperature working condition in the space;
the condensation evaporator 9 is provided with a condensation evaporator shell 10, the bottom of the rectifying tower 11 is provided with a rectifying tower bottom electric heater 12, and the power is 100W; heating the liquid at the bottom of the tower by the electric heater 12 at the bottom of the rectifying tower to obtain ascending gas; a condensed Ne liquid is generated on the condensation side of the condensation evaporator 9 and refluxed into the rectifying column 11 to become a descending liquid in the column; the evaporation side of the condensation evaporator 9 and the top of the rectifying tower 11 respectively generate a stream of the main component20Ne mixed neon gas containing 95.4% of Ne and recombined at the output of the rectifying tower 1120Ne with the flow rate of 2.853 Nm/h, sequentially passing through the low-temperature-stage heat exchanger 6 and the high-temperature-stage heat exchanger 3 to recover cold energy, and then discharging the cold energy from the separation equipment 2; refrigerating cycle neon is generated at the top of the condensation evaporator 9, and the cycle neon is generated after cold energy is recovered by the low-temperature section heat exchanger 6 and the high-temperature section heat exchanger 3 in sequence;
as the distillation is carried out,22ne liquid is continuously enriched at the bottom of the rectification column 11 until the purity reaches 99.9%, and the flow rate of 0.1466 Nm/h is taken as22Ne liquid product is output from the bottom of the rectifying column 11.
Example 3
The process flow shown in figure 1 is adopted to separate neon gas22Ne liquid product:
carrying out labor-intensive cultivation on 3 Nm/h high-purity Ne raw material gas and 32 Nm/h circulating neon gas together, conveying the mixture into a compressor 1 to be compressed to 9 MPa (g), and then cooling the mixture by a cooler which is independent of the compressor 1 to obtain compressed and cooled neon gas; the compressed and cooled neon is then fed into a separation device 2; the compressed and cooled neon enters a high-temperature section heat exchanger 3 to be cooled to-140 ℃, then enters a liquid nitrogen cooler 4 to be further cooled to-189 ℃, and finally enters a low-temperature section heat exchanger 6 to be further cooled to-218 ℃, and low-temperature neon is output; wherein the cold source of the liquid nitrogen cooler 4 is liquid nitrogen shared with the interior of the cold screen 5;
then, dividing the low-temperature neon into two strands, throttling and decompressing one strand of low-temperature neon through an adjusting valve 7 at the flow rate of 3 Nm/h to 0.1-0.2 MPa (g), and then rectifying in a rectifying tower 11; wherein the other part is throttled and decompressed to 0.02MPa (g) at a flow rate of 32 Nm/h by an adjusting valve 8, and then the produced liquid Ne is conveyed into a condensation evaporator 9 arranged at the top of a rectifying tower 11 to be used as a cold source;
wherein the liquid nitrogen cooler 4, the low-temperature section heat exchanger 6, the rectifying tower 11 and the condensing evaporator 9 are all accommodated in a space surrounded by a cold screen 5, and the space keeps 1 × 10-4Vacuum degree of Pa; liquid nitrogen is introduced into the cold shield 5 and is used for maintaining the low-temperature working condition in the space;
the condensation evaporator 9 is provided with a condensation evaporator shell 10, and the bottom of the rectifying tower 11 is provided with a rectifying towerA tower bottom electric heater 12 with the power of 100W; heating the liquid at the bottom of the tower by the electric heater 12 at the bottom of the rectifying tower to obtain ascending gas; a condensed Ne liquid is generated on the condensation side of the condensation evaporator 9 and refluxed into the rectifying column 11 to become a descending liquid in the column; the evaporation side of the condensation evaporator 9 and the top of the rectifying tower 11 respectively generate a stream of the main component20Ne mixed neon gas containing 95.3% of Ne and recombined at the output of the rectifying tower 1120Ne with a flow rate of 2.844 Nm/h, sequentially passing through the low-temperature-stage heat exchanger 6 and the high-temperature-stage heat exchanger 3 to recover cold energy, and then discharging the cold energy from the separation equipment 2; refrigerating cycle neon is generated at the top of the condensation evaporator 9, and the cycle neon is generated after cold energy is recovered by the low-temperature section heat exchanger 6 and the high-temperature section heat exchanger 3 in sequence;
as the distillation is carried out,22ne liquid is continuously enriched at the bottom of the rectification column 11 until the purity reaches 99.9%, and the flow rate of 0.1438 Nm/h is taken as22Ne liquid product is output from the bottom of the rectifying column 11.
Example 4
The process flow shown in figure 1 is adopted to separate neon gas22Ne liquid product:
carrying out labor-intensive cultivation on 3 Nm/h high-purity Ne raw material gas and 32 Nm/h circulating neon gas together, conveying the mixture into a compressor 1 to be compressed to 8 MPa (g), and then cooling the mixture by a cooler which is independent of the compressor 1 to obtain compressed and cooled neon gas; the compressed and cooled neon is then fed into a separation device 2; the compressed and cooled neon enters a high-temperature section heat exchanger 3 to be cooled to minus 148 ℃, then enters a liquid nitrogen cooler 4 to be further cooled to minus 195 ℃, and finally enters a low-temperature section heat exchanger 6 to be further cooled to minus 224 ℃, and low-temperature neon is output; wherein the cold source of the liquid nitrogen cooler 4 is liquid nitrogen shared with the interior of the cold screen 5;
then, dividing the low-temperature neon into two strands, throttling and decompressing one strand of low-temperature neon through an adjusting valve 7 at the flow rate of 3 Nm/h to 0.1-0.2 MPa (g), and then rectifying in a rectifying tower 11; wherein the other part is throttled and decompressed to 0.02MPa (g) at a flow rate of 32 Nm/h by an adjusting valve 8, and then the produced liquid Ne is conveyed into a condensation evaporator 9 arranged at the top of a rectifying tower 11 to be used as a cold source;
wherein the liquid nitrogen cooler 4, the low-temperature section heat exchanger 6, the rectifying tower 11 and the condensing evaporator 9 are all accommodated in a space surrounded by a cold screen 5, and the space keeps 1 × 10-4Vacuum degree of Pa; liquid nitrogen is introduced into the cold shield 5 and is used for maintaining the low-temperature working condition in the space;
the condensation evaporator 9 is provided with a condensation evaporator shell 10, the bottom of the rectifying tower 11 is provided with a rectifying tower bottom electric heater 12, and the power is 100W; heating the liquid at the bottom of the tower by the electric heater 12 at the bottom of the rectifying tower to obtain ascending gas; a condensed Ne liquid is generated on the condensation side of the condensation evaporator 9 and refluxed into the rectifying column 11 to become a descending liquid in the column; the evaporation side of the condensation evaporator 9 and the top of the rectifying tower 11 respectively generate a stream of the main component20Ne mixed neon gas containing 94.9% of neon gas and recombined from the rectifying tower 1120Ne with the flow rate of 2.795 Nm/h, sequentially passing through the low-temperature-stage heat exchanger 6 and the high-temperature-stage heat exchanger 3 to recover cold energy, and then discharging the cold energy from the separation equipment 2; refrigerating cycle neon is generated at the top of the condensation evaporator 9, and the cycle neon is generated after cold energy is recovered by the low-temperature section heat exchanger 6 and the high-temperature section heat exchanger 3 in sequence;
as the distillation is carried out,22ne liquid is continuously enriched at the bottom of the rectification column 11 until the purity reaches 99.9%, and the flow rate of 0.1417 Nm/h is taken as22Ne liquid product is output from the bottom of the rectifying column 11.
It can be seen that the product obtained by separation according to the process of the invention22The purity of Ne liquid product is extremely high, and the average output flow rate is about 1600 times of the 2.2L/day output flow rate described in Chinese patent CN 1513587A.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (7)
1. Separation from neon22A method for Ne, performed by cryogenic rectification, comprising the steps of:
combining the high-purity Ne feed gas and the circulating neon gas, conveying the mixture into a compressor (1) to be compressed to 7-9 MPa (g), and then cooling the mixture by a cooler to obtain compressed and cooled neon gas; then, feeding said compressed and cooled neon to a separation device (2);
within the separation device (2): the compressed and cooled neon enters a high-temperature section heat exchanger (3) for cooling, and then enters the high-temperature section heat exchangerThe low-temperature neon gas is divided into two streams, wherein one stream is throttled and decompressed to 0.1-0.2 MPa (g) by a regulating valve (7) and then enters a rectifying tower (11) for rectification, the other stream is throttled and decompressed to 0.02MPa (g) by a regulating valve (8) and then generates liquid Ne which is conveyed into a condensing evaporator (9) arranged at the top of the rectifying tower (11) to serve as a cold source, the liquid nitrogen cooler (4), the low-temperature section heat exchanger (6), the rectifying tower (11) and the condensing evaporator (9) are all accommodated in a space surrounded by a cold screen (5), and the space keeps 1 × 10-6Pa to 1 × 10-2Vacuum degree of Pa; liquid nitrogen is introduced into the cold shield (5) and is used for maintaining the low-temperature working condition in the space;
the condensation evaporator (9) is provided with a condensation evaporator shell (10), and the bottom of the rectifying tower (11) is provided with a rectifying tower bottom electric heater (12); a condensed Ne liquid is generated on the condensing side of the condensing evaporator (9) and flows back to the rectifying tower (11); the evaporation side of the condensation evaporator (9) and the top of the rectifying tower (11) respectively generate a strand of the main component20Ne mixed neon gas is output from the rectifying tower (11) and then is combined, and the Ne mixed neon gas is sequentially recycled through the low-temperature section heat exchanger (6) and the high-temperature section heat exchanger (3) and then is discharged from the separation equipment (2); refrigerating cycle neon is generated at the top of the condensation evaporator (9), and the refrigerating cycle neon is generated after cold energy is recycled by the low-temperature section heat exchanger (6) and the high-temperature section heat exchanger (3) in sequence;
wherein, as the rectification is carried out,22ne liquid is continuously enriched at the bottom of the rectifying tower (11) until the purity reaches 99.9 percent, and then the Ne liquid is used as22Ne liquid product is output from the bottom of the rectification column (11).
2. Method according to claim 1, characterized in that the cooler is arranged in the compressor (1) or independently of the compressor (1).
3. The method according to claim 1, characterized in that in the separation equipment (2), the compressed and cooled neon enters a high-temperature heat exchanger (3) to be cooled to-140 ℃ to-150 ℃, then enters a liquid nitrogen cooler (4) to be further cooled to-188 ℃ to-195 ℃, and finally enters a low-temperature heat exchanger (6) to be further cooled to-218 ℃ to-225 ℃ to output low-temperature neon.
4. The method of claim 3 wherein said compressed and cooled neon is passed into said separation apparatus (2) to cool said neon to-145 ℃ in a high temperature section heat exchanger (3), then to a liquid nitrogen cooler (4) to further cool said neon to-193 ℃, and finally to a low temperature section heat exchanger (6) to further cool said neon to-221 ℃, and to output said neon at a low temperature.
5. Method according to claim 1, characterized in that the cold source of the liquid nitrogen cooler (4) is liquid nitrogen provided separately outside the separation device (2) or liquid nitrogen shared with the inside of the cold screen (5).
6. The method of claim 1, wherein the flow ratio of said high purity Ne feed gas to said recycled neon is 3: 32.
7. The process according to claim 1, characterized in that, in said separation device (2), the flow ratio of one stream of low-temperature neon throttled for pressure reduction by means of the regulating valve (7) to the other stream of low-temperature neon throttled for pressure reduction by means of the regulating valve (8) is 3: 32.
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