CN1085188C - Method for extracting high-purity krypton, xenon from mixed gas containing oxygen, krypton, xenon. - Google Patents
Method for extracting high-purity krypton, xenon from mixed gas containing oxygen, krypton, xenon. Download PDFInfo
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- CN1085188C CN1085188C CN97103252A CN97103252A CN1085188C CN 1085188 C CN1085188 C CN 1085188C CN 97103252 A CN97103252 A CN 97103252A CN 97103252 A CN97103252 A CN 97103252A CN 1085188 C CN1085188 C CN 1085188C
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- xenon
- krypton
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- 1ppm
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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
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04642—Recovering noble gases from air
- F25J3/04745—Krypton and/or Xenon
- F25J3/04751—Producing pure krypton and/or xenon recovered from a crude krypton/xenon mixture
- F25J3/04757—Producing pure krypton and/or xenon recovered from a crude krypton/xenon mixture using a hybrid system, e.g. using adsorption, permeation or catalytic reaction
-
- 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
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/60—Processes 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
-
- 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
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/82—Processes or apparatus using other separation and/or other processing means using a reactor with combustion or catalytic reaction
-
- 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
- F25J2215/34—Krypton
-
- 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
- F25J2215/36—Xenon
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
The present invention relates to a method for extracting a krypton gas product and a xenon gas product in a gas mixture of oxygen, krypton and xenon. Raw gas is generated into CO2 and H2O by a methane removing furnace, the CH4 is removed, and the CH4 concentration reaches less than 1 ppm; a molecular sieve is used for absorbing the CO2 and the H2O, and the concentrations of the CO2 and the H2O respectively reach less than 1 ppm; a O2-Kr-Xr gas mixture enters a cryogenic rectification tower, and O2, Kr and Xe are respectively separated out; when the O2 concentration in the Kr is less than 1000 ppm, the O2 concentration is caused to be less than 1 ppm by an oxygen removing furnace, and the obtained krypton product of high purity is filled into a product bottle; when the Xe contains less than 3% of the krypton or other impurities, the Kr, the O2, the N2, the CH4, N2O, and the like are removed, and the obtained xenon product is filled into the product bottle. The present invention has the advantages of production technological flow simplification, convenient operation, product quality reliability improvement and product extraction rate improvement.
Description
The present invention relates to a kind of double rectification column low ternperature separation process and catalytic purification method, specifically from the gas mixture of oxygen, krypton, xenon, extract the method for krypton-85 gas product, xenon-133 gas product.
Normally adopt sieve-board type tower or blade membrane type tower and general Raschig ring packing tower for from oxygen, krypton, xenon mixed gas, extracting krypton, xenon at the low temperature fractionation tower section; Active copper and general dehydrogenation catalyst are partly adopted in the deoxygenation of krypton fraction; Xenon fraction purification part adopts
Add absorption and remove CO
2And H
2O removes H with rectifying again
2, N
2, Kr or remove Kr, H with absorption method
2, N
2And xenon purifier and absorption method; The control of the second rectifying tower top condenser temperature adopts ethanol to add dry ice or liquid nitrogen is made heat-eliminating medium, all adds with manual type.The shortcoming of above-mentioned part is respectively that separation efficiency is lower, and the viscous flow amount increases starting time greatly, and the permission bound amplitude of upstream amount is little, troublesome poeration; It is few that used deoxygenation stove removes oxygen capacity, handles 15m at every turn
3The krypton fraction in behind the oxygen, need carry out the hydrogenating reduction activation, and retaining of hydrogen needs replace with a large amount of high pure nitrogens, the pollution of hydrogen still can occur, make in the krypton product hydrogen richness up to 2～3ppm; The treatment capacity of absorption method is low, and flow process is numerous and diverse, operation inconvenience, and the xenon extraction yield is low especially; This artificial cooling mode, operator's intensity is big, and temperature is wayward.
The objective of the invention is shortcoming, provide a kind of krypton, xenon extraction yield height, the method for easy handling at above-mentioned existence.
Technical essential of the present invention is: will contain Kr-Xe component concentration at the gas mixture more than 18%, and as raw material of the present invention, extract 99.995% or more highly purified krypton product and xenon product.Contain in the oxygen in the krypton xenon gas mixture of 18% above concentration, also contain CH
4, N
2, CO, CO
2And N
2Impurity such as O according to the different properties of these impurity components, are formed the whole production technical process, as shown in Figure 1.Unstripped gas is with 10～15m
3/ h flow is dosed to 50m
3The time till, do periodical operation production, at first with CH in the unstripped gas
4Remove by removing methane stove (1) CH
4Add O
2Decompose and generate CO
2And H
2O makes CH
4Reduce to below the 1ppm, and CO
2And H
2O removes freshwater mussel with molecular sieve adsorber (2) absorption and reduces to below the 1ppm.Gas mixture is sent in first low-temperature fractionating tower (3), operate under 0.3～0.5MPa pressure, overhead condenser adopts liquid oxygen to make heat-eliminating medium, with the Mixed Gas Condensation that enters, and from cat head discharge oxygen fraction, till finishing to charging, then carry out total reflux operation, the tower still is made thermal source with electric heater or heated nitrogen, make material rising steam flow amount reach steady state operation, continue to discharge the oxygen fraction then, when krypton component content is increased to more than 0.1% to 99.9% the time, as O
2-Kr fraction is delivered in the basin (4).Krypton more than 99.9% is the krypton fraction, sends in the deoxygenation stove (5) to reach below the 1ppm except that oxygen impurities, goes to fill the production of promptly having finished the krypton product in the product bottle as krypton product pneumatic transmission.When contain in the krypton fraction of cat head discharge xenon concentration be more than the 20ppm to 97% the time, deliver in the basin (6) as the Kr-Xe fraction, make the raw material of operation next time, and stop the operation that discharge is finished first rectifying tower, column hold-up is the xenon fraction and delivers to storage metering in the basin (12), contain impurity in the xenon fraction and be about Kr, O
2, N
2, CH
4, CO
2And N
2O etc. feed in the front end xenon purifier (7) O
2, N
2, CH
4, CO
2And N
2O removes and reaches product defined content, and enter and give in cold second low-temperature fractionating tower (8), with total reflux operation and keep tower to be pressed in 0.2～0.3MPa condition, overhead condenser adds liquid nitrogen with ethanol and makes heat-eliminating medium and form automatic temperature control system (10), the tower still heats with nitrogen and reaches steady state operation, impurity such as cat head krypton are done to be interrupted discharge, deliver in the basin (9) and deposit, when krypton component in the cat head discharge to 100ppm or according to requiring when lower, stop discharge and operation and in the tower material be the xenon product, charge into respectively in the product bottle again after delivering to basin (11), finished the production of xenon product.In short, the present invention be with contain Kr-Xe component concentration at the gas mixture more than 18% as raw material, it is characterized in that unstripped gas passes through to remove methane stove (1) and generates CO
2And H
2O removes CH
4Reach below the 1ppm, utilize molecular sieve adsorber (2) CO absorption
2And H
2O makes it respectively to reach below the 1ppm O
2-Kr-Xe mixed gas enters first low-temperature fractionating tower (3), with O
2, Kr and Xe separate respectively, contain O in Kr
2When 1000ppm is following, make below 1ppm by deoxygenation stove (5), get the high purity krypton product and charge in the product bottle, in Xe, contain 3% following krypton and other impurity, by xenon purifier (7) and second low-temperature fractionating tower (8) and tower top temperature automatic control system (10), with Kr, O
2, N
2, CH
4And N
2O etc. remove to such an extent that high purity xenon product charges in the product bottle.
The present invention compared with prior art, the high efficiency separation that adopts is used Stainless Steel Cloth corrugated regular filler and Dixon ring filler by comparison, under identical tower height degree condition, has separation efficiency height significantly, oxygen level can reach 10～20ppm in the krypton fraction, and its retention amount I shortens starting time simultaneously, and the permission bound amplitude of upstream amount is big, easy handling, thus product extraction rate improved.Adopt large vol deoxygenation stove (selecting for use Dalian Inst of Chemicophysics, Chinese Academy of Sciences to produce and sell the DE1 type in 1993), can handle 300m
3Above krypton fraction gas, carry out the hydrogen reduction activation then, thereby simplified operation, save a large amount of high-purity nitrogens, more importantly avoided hydrogen contamination, guaranteed the quality of krypton product the krypton product, the deficiencies in the prior art have been solved with xenon purifier and cryogenic rectification method, can handle the xenon fraction in a large number, and krypton component content is had the permission of broad, reach higher extraction yield.Adding liquid nitrogen with ethanol is heat-eliminating medium, adopt a cover constant temperature automatic control system, with the temperature sensor of cat head, make the requirement of operation between-76～-82 ℃, provide the specified temperature signal, deliver to liquid nitrogen automatic discharge valve, control its switch degree and provide different amount of liquid nitrogen, reach the constant temperature of regulation, thereby realized automatization, improved operation, also reduce or avoid causing and freeze tower accident (because of xenon boiling point and zero pour differ 3 ℃), improved extraction yield simultaneously.
The present invention has simplified the technological process of production, has made things convenient for operation, has improved the reliability and the product extraction rate of quality product.Accompanying drawing is a process flow sheet of the present invention.
Said double rectification column all adopts the packed tower of efficient separation; Removing of oxygen impurities is the large capacity deoxygenation stove that adopts deoxidation catalyst (Dalian Inst of Chemicophysics, Chinese Academy of Sciences produces and sells, the AE2 type) in the krypton fraction, and deoxygenation reaches below the 1ppm; The purifying of impurity in the xenon fraction has adopted xenon purifier and rectifying column, its impurity is all removed reach the regulation requirement; The constant temperature of the second low-temperature fractionating tower overhead condenser, adopting ethanol and liquid nitrogen is cooling medium, forms automatic temperature control system with condenser temperature sensor liquid nitrogen container and liquid nitrogen automatic regulating valve.
Embodiment 1
Unstripped gas is formed: O
2～64.6%, Kr～34%; Xe～1.38%, foreign matter content: CH
4＜100ppm; N
2～50ppm; CO
2～5ppm; N
2O～10ppm;
Inlet amount is 25M
3, by removing CH behind the methane stove
4＜1ppm is by CO behind the adsorber
2＜1ppm, H
2O＜1ppm, it is from containing O that first rectifying tower top is discharged the krypton fraction
2Till～10000ppm begins to increase to 20ppm to Xe content, by O behind the deoxygenation stove
2＜1ppm, the krypton group of products becomes down:
Kr 〉=99.995% foreign matter content ppm
| Xe | O 2 | N 2 | CH 4 | CO 2 | H 2 | H 2O |
| 17 | 3 | 5 | 1 | 1 | 1 | 3 |
The krypton product volume is 7.148m
3
Xenon fractional composition: K
1～2%, N
2O～100ppm, O
2～3ppm,
N
2～5ppm，CH
4～1ppm，CO
2～1ppm
Inlet amount is 346L, and by entering second rectifying tower behind the front end xenon purifier, cat head is interrupted discharge till krypton component content is 60ppm, and the xenon product is composed as follows:
Xe 〉=99.995% foreign matter content ppm
| Kr | O 2 | N 2 | CH 4 | CO 2 | N 2O | H 2 | H 2O |
| 17 | 3 | 5 | 1 | 1 | 0.2 | 1 | 3 |
The xenon product volume is 300.2L
Krypton product extraction yield is about 87.27%; Xenon product extraction yield is about 86.76%.
Unstripped gas is formed: O
2～71.45%, Kr～26.8%, Xe～1.75%;
Foreign matter content: CH
4＜100ppm; N
2～30ppm; CO
2～4ppm; N
2O～6ppm;
Inlet amount is 47.5M
3, by removing CH behind the methane stove
4～3ppm is by CO behind the adsorber
2＜1ppm, H
2O＜1ppm, it is from containing O that first rectifying tower top is discharged the krypton fraction
2Till～1000ppm begins to increase to 5ppm to Xe content, CH wherein
4＜1ppm is by the O behind the deoxygenation stove
2＜1ppm, the krypton group of products becomes down:
Kr 〉=99.998% foreign matter content ppm
| Xe | O 2 | N 2 | CH 4 | CO 2 | H 2 | H 2O |
| 5 | 1 | 5 | 1 | 1 | 1 | 3 |
The krypton product volume is 11.46m
3
Xenon fractional composition: Kr～1%, N
2O～40ppm, O
2～3ppm,
N
2～7ppm，CH
4～1ppm，CO
2～1ppm
Inlet amount is 829.3L, and by entering second rectifying tower behind the front end xenon purifier, cat head is interrupted discharge till krypton component content is 20ppm, and the xenon product is composed as follows:
Xe 〉=99.998% foreign matter content ppm
| Kr | O 2 | N 2 | CH 4 | CO 2 | N 2O | H 2 | H 2O |
| 5 | 1 | 3 | 1 | 1 | 0.2 | 1 | 3 |
The xenon product volume is 746.3L
Krypton product extraction yield is about 90%; Xenon product extraction yield is about 90%.
Claims (5)
1. extract the method for high purity krypton, xenon in an oxygen, krypton, the xenon gas mixture, it be with contain Kr-Xe component concentration at the gas mixture more than 18% as raw material, it is characterized in that unstripped gas passes through to remove methane stove (1) and generates CO
2And H
2O removes CH
4Reach below the 1ppm, utilize molecular sieve adsorber (2) CO absorption
2And H
2O makes it respectively to reach below the 1ppm O
2-Kr-Xe mixed gas enters first low-temperature fractionating tower (3), with O
2, Kr and Xe separate respectively, contain O in Kr
2When 1000ppm is following, make below 1ppm by deoxygenation stove (5), get the high purity krypton product and charge in the product bottle, in Xe, contain 3% following krypton and other impurity, by xenon purifier (7) and second low-temperature fractionating tower (8) and tower top temperature automatic control system (10), with Kr, O
2, N
2, CH
4And N
2O removes to such an extent that high purity xenon product charges in the product bottle.
2. method according to claim 1 is characterized in that double rectification column all adopts packing tower.
3. method according to claim 1 is characterized in that removing of oxygen impurities is the large vol deoxygenation stove that adopts deoxidation catalyst in the krypton fraction, and deoxygenation reaches below the 1ppm.
4. method according to claim 1 is characterized in that the purifying of impurity in the xenon fraction having adopted xenon purifier and rectifying tower, its impurity is all removed reach specified requirement.
5. method according to claim 1 is characterized in that the constant temperature of the second low-temperature fractionating tower overhead condenser, and adopting ethanol and liquid nitrogen is heat-eliminating medium, and with condenser temperature sensor, liquid nitrogen container and liquid nitrogen automatic regulating valve are formed automatic temperature control system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97103252A CN1085188C (en) | 1997-04-17 | 1997-04-17 | Method for extracting high-purity krypton, xenon from mixed gas containing oxygen, krypton, xenon. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97103252A CN1085188C (en) | 1997-04-17 | 1997-04-17 | Method for extracting high-purity krypton, xenon from mixed gas containing oxygen, krypton, xenon. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1196331A CN1196331A (en) | 1998-10-21 |
| CN1085188C true CN1085188C (en) | 2002-05-22 |
Family
ID=5166606
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97103252A Expired - Fee Related CN1085188C (en) | 1997-04-17 | 1997-04-17 | Method for extracting high-purity krypton, xenon from mixed gas containing oxygen, krypton, xenon. |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1085188C (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE60208641T2 (en) * | 2001-11-19 | 2006-11-09 | Air Products And Chemicals, Inc. | Process for the recovery of krypton and xenon from a gas or liquid stream |
| FR2899320B1 (en) * | 2006-04-03 | 2008-05-16 | Air Liquide | DEVICE AND METHOD FOR PACKAGING CARBON SNOW IN A PLASTIC FILM |
| FR2911391A1 (en) * | 2007-01-16 | 2008-07-18 | Air Liquide | Cryogenic separation method for gas, involves using distillation columns and absorption column with heat and/or material exchange section between descending liquid and mounting gas, where section has specific parameter |
| CN102389683B (en) * | 2011-08-15 | 2014-05-28 | 西北核技术研究所 | Method and device for separating krypton from xenon by using active carbon |
| CN104310325B (en) * | 2014-10-24 | 2016-06-29 | 武汉钢铁(集团)公司 | Krypton, xenon-133 gas purification method and device |
| CN108609591A (en) * | 2018-04-27 | 2018-10-02 | 南京特种气体厂股份有限公司 | The removing means and removal methods of trace methane in a kind of krypton xenon gaseous mixture |
| CN111874881B (en) * | 2019-06-27 | 2022-10-25 | 南京工业大学 | Method for purifying xenon by using DD3R molecular sieve membrane |
| CN112557157B (en) * | 2021-02-28 | 2021-05-04 | 中国工程物理研究院核物理与化学研究所 | Method for separating, purifying and collecting xenon in air sample based on specific device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87101534A (en) * | 1987-04-13 | 1988-10-26 | 中国科学院大连化学物理研究所 | Xenon purification process and equipment |
| JPH05296653A (en) * | 1992-04-15 | 1993-11-09 | Nippon Sanso Kk | Method for refining krypton and xenon |
| JPH0970067A (en) * | 1995-08-31 | 1997-03-11 | Nippon Telegr & Teleph Corp <Ntt> | Contract information cache method for mobile terminal equipment |
-
1997
- 1997-04-17 CN CN97103252A patent/CN1085188C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87101534A (en) * | 1987-04-13 | 1988-10-26 | 中国科学院大连化学物理研究所 | Xenon purification process and equipment |
| JPH05296653A (en) * | 1992-04-15 | 1993-11-09 | Nippon Sanso Kk | Method for refining krypton and xenon |
| JPH0970067A (en) * | 1995-08-31 | 1997-03-11 | Nippon Telegr & Teleph Corp <Ntt> | Contract information cache method for mobile terminal equipment |
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| Publication number | Publication date |
|---|---|
| CN1196331A (en) | 1998-10-21 |
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