CN101941684A - Helium purifying method - Google Patents
Helium purifying method Download PDFInfo
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- CN101941684A CN101941684A CN2009101521310A CN200910152131A CN101941684A CN 101941684 A CN101941684 A CN 101941684A CN 2009101521310 A CN2009101521310 A CN 2009101521310A CN 200910152131 A CN200910152131 A CN 200910152131A CN 101941684 A CN101941684 A CN 101941684A
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- activated carbon
- carbon fiber
- helium
- helium flow
- fiber bed
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
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Abstract
The invention discloses a method and a system for purifying helium. The method comprises the following step of: enabling helium containing impurities to pass through an oil/fat filter, a multilayered molecule screen/silica gel device, an active carbon/active carbon fiber bed, a metal getter and a particulate filter. Therefore, in the invention, the helium purity up to 99.999 percent is achieved.
Description
Technical field
The present invention relates to prepare the method and system of high purity helium.Described device adopts the activated carbon/active carbon fibre column of operation at low temperatures, with the trace chemistry impurity in the helium, is reduced to the level of 10ppm-100ppm from 0.1%-3%.Employing with further reduction trace chemistry impurity, is reduced to 1ppm-10ppm to prepare highly purified helium at about 400-600 ℃ air-breathing post.
Background technology
The helium resource-constrained usually is present in the underground gas aggradation layer, separates during the preparation of Sweet natural gas.Sweet natural gas contains the helium of the 0.3%-0.7% that has an appointment.Helium has the character of many uniquenesses, for example lower boiling, low density, low solubility, high thermal conductivity and inertia, and can liquefy.Its coagulation temperature is minimum in all known substances.The application of helium comprises: fill balloon and dirigible, autogenous welding, the cooling of superconducting magnet in medical scanners and the research, the gas under pressure in the rocket liquid propellant, Breathing device for gas, the working fluid in the nuclear reactor and as the chemico-analytic carrier gas of gas-chromatography.These application in many scientific researches all require the purity of helium greater than 99.999%.
From the effusive helium of Magnetic resonance imaging (MRI) system owing to air leaks has 98.5% minimum purity to system.After helium contracted with pump pressure, gaseous impurities comprised: grease, carbonic acid gas, moisture, oxygen and nitrogen.These gaseous impuritiess are usually removed by the following method: make gas by one or more activated carbon/activated carbon fibers cold bed or by freezing come out in heat exchanger.To surpass 99.999% purity in order reaching, to consume a large amount of liquid nitrogen to keep the low temperature of microscler activated carbon/activated carbon fiber adsorption bed.Yet,, the invention provides the method that low-purity helium is purified to the lower cost of high purity helium because the expense of this method of problem of material and energy cost is huge.
Because the importance of high purity helium and reach the required cost problem of high purity, needing can be with the method and system of economized form purifying helium.
Summary of the invention
The invention provides a kind of helium purification process, this method may further comprise the steps: (a) impure helium flow is delivered to filter, to remove the oil/grease in the helium flow; (b) this helium flow is delivered to multilayer molecular sieve/silica gel device, to remove moisture and the carbonic acid gas that exists in the helium flow; (c) this helium flow is delivered to activated carbon/activated carbon fiber bed, to remove carbonic acid gas, moisture and the oil/grease of nitrogen, oxygen and trace in the helium flow; (d) this helium flow is delivered to metal getter; (e) helium flow is delivered to filter, to remove the nanocarbon/metal particulate.
The present invention also provides a kind of helium purification system, and this system comprises: (a) purolator; (b) multilayer molecular sieve/silica gel device; (c) activated carbon/activated carbon fiber bed; (d) metal getter; (e) particulate filter.
The helium source comprises various industry, research and science application, for example Magnetic resonance imaging (MRI).Usually, the purity of the helium in these sources is about 97-99.9%, can be purified to 99.999% helium.
Purolator can be removed oil/grease in the helium flow by the wire cloth filter, and oil/grease is reduced to less than 10ppm; If the oil/fat content in the helium flow is higher than 10ppm, this step can not be left in the basket.
Design multilayer molecular sieve/silica gel device is reduced to less than 5ppm respectively to remove moisture and the carbonic acid gas in the helium flow.If moisture in the helium flow or carbon dioxide content are higher than 5ppm, this step can not be left in the basket.Molecular sieve can comprise the sorbing material that can remove these pollutents.Can adopt zeolite adsorption material such as 3A in the molecular sieve device, 4A, 5A, 13X or their mixture.These multilayer molecular sieve/silica gel devices use at ambient temperature.Can regenerate by electrically heated, vacuum purge and pure helium; When operate continuously, adopt two beds.
Activated carbon/active carbon fiber fixed bed carbonic acid gas, moisture and the oil/grease of removing oxygen, nitrogen and trace in the helium flow.These comprise activated carbon or the activated carbon powder or the activated carbon fiber of pellets; Activated carbon fiber can be made into many forms, for example band shape, sheet or pectination.Preferred two beds are worked together, and one of them bed is regenerated for another bed of absorption mode.Usually by electric heater activated carbon/activated carbon fiber bed is heated to 120 ℃, carries out vacuum purge simultaneously, regenerate with rare gas element such as nitrogen and high purity helium purge then; But for the activated carbon fiber bed, because activated carbon fiber is a good conductor, can be by electricity, nitrogen and pure helium purge and regenerates then.Activated carbon/activated carbon fiber bed is immersed in the liquid nitrogen of cryogenic tank of vacuum insulation to keep activated carbon/activated carbon fiber bed tempertaure in liquid nitrogen temperature.
The service temperature of metal getter is about 400-800 ℃, more preferably 400-600 ℃, is used for further removing the oxygen and the nitrogen of trace.Activation usually occurs in 600 ℃ to 800 ℃ scope.The metal getter agent material is selected from down group: transition metal more specifically is copper, nickel, cobalt, iron, manganese and zirconium-aluminium alloy or their mixture.
At last, the employing particulate filter is removed the particulate in activated carbon/activated carbon fiber bed and the metal getter.
Brief Description Of Drawings
Accompanying drawing is the synoptic diagram of helium purge process of the present invention.
Embodiment
Shown the helium purge process in the accompanying drawings.The helium flow 1 of pressure 50-250 crust is delivered to filter 10, and filter 10 will be removed the oil/grease in the helium flow, and it is reduced to less than 10ppm.Helium flow leaves filter 10, is transported to multilayer molecular sieve/silica gel device 11 by pipeline 10A; Described multilayer molecular sieve/silica gel device 11 can be two beds of TSA round-robin.Adopt zeolite adsorption material such as 3A, 4A, 5A, 13X or their mixture in the molecular sieve device; Silica gel is used for the high humidity situation.Multilayer molecular sieve/silica gel device 11 comprises electric heater 4, by vacuum purge then the purifying helium purge make described bed regeneration.Multilayer molecular sieve/silica gel device 11 is operation at ambient temperature usually.Multilayer molecular sieve/silica gel device 11 can separate moisture and carbonic acid gas from helium flow mixture 1, and the moisture of helium flow mixture 1 and carbonic acid gas are reduced to less than 5ppm.
Helium flow leaves multilayer molecular sieve/silica gel device, is transported to No. three heat exchangers by pipeline 11A, in heat exchanger helium is carried out precooling.The helium of precooling is transported to activated carbon/activated carbon fiber bed 12 by pipeline 11A and valve V1 (V2 closes), cools off in the liquid nitrogen of the cryogenic tank 16 of activated carbon/activated carbon fiber bed 12 by being immersed in vacuum insulation.Activated carbon/activated carbon fiber bed 12 will adsorb carbonic acid gas, moisture and the oil/grease of nitrogen, oxygen and trace in the helium flow.Activated carbon beds comprises the activated carbon of pellets, activated carbon powder or activated carbon fiber; And activated carbon fiber can be many forms, for example band shape, sheet or pectination.Activated carbon/activated carbon fiber bed 12 is by well heater/galvanic couple 6, simultaneously through pipeline 12A and valve V7 (V8 closes) vacuum purge, purges with the helium of nitrogen and purifying respectively then and regenerates.
The helium flow that purity reaches the purifying of 99.99%-99.999% flows out to metal getter 14 from activated carbon/activated carbon fiber bed 12 through pipeline 12B and valve V5 (V7 and V6 close), and metal getter 14 will further reduce the level of foreign matter content to 1-10ppm.Metal getter is by electric heater 9 regeneration.Foreign matter content is that the helium flow of the purifying of 1-10ppm leaves metal getter 14,, stores or utilizes through pipeline 2 by removing after the metal particle in the carbon particulate or 14 12 from particulate filter 15.
The helium flow of purifying from 12 be directed to by valve V5 and through pipeline 12B be transported to No. three heat exchangers 5 with adverse current cooling from 11 logistics.Another road is the nitrogen by V3 (V4 closes), is the nitrogen from the liquid nitrogen vaporization of vacuum insulation cryogenic tank 16.Liquid nitrogen is carried by V9 (V10 closes) through pipeline 7.After the heat exchange, nitrogen blows downwards by 11C or recirculation and is used as sweeping gas.
In the present invention, also there is second activated carbon/activated carbon fiber bed 13.Be similar to activated carbon/activated carbon fiber bed 12, bed 13 can adsorb water, carbonic acid gas and the oil/grease of nitrogen, oxygen and trace in the helium flow that needs purifying.Two activated carbon/activated carbon fiber beds 12 and 13 synergies, when a bed just during the impurity in the separation of helium air-flow, another bed is regenerated.Be similar to bed 12, bed 13 is by electrically heated 6 regeneration, by cooling off in the liquid nitrogen that is immersed in the vacuum insulation cryogenic tank.
Embodiment: use the getter cryogenic absorption
To be stored in the tubular type trailer (tube trailer) about 250 crust of pressure from about 99.5% helium of the purity of MRI system.Impurity mainly is about 1000ppm oxygen, moisture, grease and the carbonic acid gas of about 4000ppm nitrogen and the trace of content between 1 to 100ppm.The diameter of active carbon column is 0.55 meter, long 1.2 meters.Powdered activated carbon is from coconut husk, and the BET specific surface area is 1230 meters
2/ gram.The bed voidage is about 0.7.
Adsorption time depends on the purity and the helium flow velocity of working pressure, import helium.When the helium flow velocity be 150 standard cubic meter/hour, during purity 99.5%, working pressure 250 crust, (oxygen＞20ppm) is 4 hours to run through the time (breakthrough time).Output logistics from activated carbon beds continues to pass through 650 ℃ getter device, is filled with not evaporable getter zirconium-aluminium alloy in the getter device.The lowest purity of getter ingress helium flow is about 99.99%.The helium purity in getter device exit reaches 99.999%.
The regenerative process of activated carbon comprises in the cryogenic tank that at first liquid nitrogen is discharged into another vacuum insulation.Set then and extremely about 125 crust of another Regenerative beds equilibrated countercurrent pressure.Then, when bed is heated to 120 ℃, contact, carry out the adverse current step-down, be reduced to 1 crust from 125 crust with reclaiming the chamber.Carry out the adverse current vacuum purge, then the nitrogen countercurrent purge.Then, carry out the adverse current vacuum purge, carry out clockwise pressurization equilibration to 125 crust with another exhausted bed then.With clockwise pressurization equilibration to 250 crust of purifying helium.Then liquid nitrogen is discharged and switched feeding helium feedstream from the cryogenic tank of another vacuum insulation and begin next circulation.
The whole recovery time is the 4 hours time with the coupling adsorption step.Getter is 800 ℃ of activation.
Embodiment: cryogenic absorption only
To be stored in the tubular type trailer about 250 crust of pressure from the helium of the purity of MRI system about 99.5%.Impurity mainly is about 1000ppm oxygen, moisture, grease and the carbonic acid gas of about 4000ppm nitrogen and the trace of content between 1 to 100ppm.The diameter of active carbon column is 0.55 meter, long 1.2 meters.Powdered activated carbon is from coconut husk, 1230 meters of its BET specific surface areas
2/ gram.The bed voidage is about 0.7.
Adsorption time depends on the purity and the helium flow velocity of working pressure, import helium.The helium flow velocity be 150 standard cubic meter/hour, purity 99.5%, working pressure 250 crust.The output logistics of activated carbon beds 12 continues by another new activated carbon beds, and running through the time (oxygen＞2ppm, helium purity＞99.999%) is 0.5 hour.
The recovery time of required 4 beds of preparation is about 4 hours continuously, in each step, and two bed series connection.
Though described the present invention with reference to embodiment, obviously many other forms of the present invention and improved form are that those skilled in the art understand.Appended claims of the present invention generally should be interpreted as covering all these tangible form and improved forms, and these forms are included in true spirit of the present invention and the scope.
Claims (27)
1. the method for a helium purifying said method comprising the steps of:
(a) impure helium flow is delivered to filter;
(b) will be delivered to multilayer molecular sieve/silica gel device from the described helium flow of described filter;
(c) will be delivered to activated carbon/activated carbon fiber bed from the described helium flow of described multilayer molecular sieve/silica gel device;
(d) will be delivered to metal getter from the described helium flow of described activated carbon/activated carbon fiber bed; With
(e) will be delivered to particulate filter from the described helium flow of described metal getter.
2. the method for claim 1 is characterized in that, described impure helium is the helium of the about 97-99.9% of purity.
3. the method for claim 1 is characterized in that, the described helium flow that reclaims from step (e) is that purity is the helium of 99.99-99.999%.
4. the method for claim 1 is characterized in that, described filter is removed oil/grease and the particulate in the described helium flow.
5. the method for claim 1 is characterized in that, described molecular sieve device contains the zeolite that is selected from down group: 3A, 4A, 5A, 13X and their mixture.
6. the method for claim 1 is characterized in that, described multilayer molecular sieve/silica gel device is removed moisture, carbonic acid gas and the oil/grease in the described helium flow.
7. the method for claim 1 is characterized in that, described activated carbon/activated carbon fiber bed is removed moisture, carbonic acid gas and the oil/grease of oxygen in the described helium flow, nitrogen, trace.
8. the method for claim 1 is characterized in that, described activated carbon beds is two or more activated carbon beds.
9. the method for claim 1, it is characterized in that, described activated carbon beds contains the activated carbon that is selected from down group: the activated carbon of pellets, activated carbon powder and activated carbon fiber, described activated carbon fiber bed contains the activated carbon fiber that is selected from down the group form: band shape, sheet and pectination.
10. method as claimed in claim 8 is characterized in that, in described activated carbon/activated carbon fiber bed one is in absorption mode and another is in regeneration mode.
11. the method for claim 1 is characterized in that, described activated carbon/activated carbon fiber bed maintains the temperature of liquid nitrogen.
12. the method for claim 1 is characterized in that, heats in the time of with vacuum purge and rare gas element or more than one inert gas purge and makes the regeneration of described activated carbon beds.
13. the method for claim 1 is characterized in that, the temperature of described metal getter is 400-800 ℃ of scope.
14. the method for claim 1 is characterized in that, described metal getter contains the metal that is selected from down group: transition metal, copper, nickel, iron, manganese, zirconium-aluminium alloy and their mixture.
15. a system that is used for impure helium flow purifying, described system comprises: (a) filter; (b) molecular sieve device; (c) activated carbon beds; (d) metal getter; (e) particulate filter.
16. system as claimed in claim 15 is characterized in that, described filter is removed the particulate in the described helium flow.
17. system as claimed in claim 15 is characterized in that, described molecular sieve device contains the zeolite that is selected from down group: 3A, 4A, 5A, 13X and their mixture.
18. system as claimed in claim 15 is characterized in that, described molecular sieve device is removed moisture, carbonic acid gas and the oil/grease in the described helium flow.
19. system as claimed in claim 15 is characterized in that, described activated carbon/activated carbon fiber bed is removed oxygen and the nitrogen in the described helium flow.
20. system as claimed in claim 15 is characterized in that, described activated carbon/activated carbon fiber bed is two or more activated carbon beds.
21. system as claimed in claim 15, it is characterized in that, described activated carbon beds contains the activated carbon that is selected from down group: the activated carbon of pellets, activated carbon powder and activated carbon fiber, described activated carbon fiber bed contains the activated carbon fiber that is selected from down the group form: band shape, sheet and pectination.
22. system as claimed in claim 21 is characterized in that, in described activated carbon/activated carbon fiber bed one is in absorption mode and another is in regeneration mode.
23. system as claimed in claim 15 is characterized in that, described activated carbon/activated carbon fiber bed maintains the temperature of liquid nitrogen.
24. system as claimed in claim 15 is characterized in that, heats in the time of with vacuum purge and rare gas element or more than one inert gas purge and makes the regeneration of described activated carbon/activated carbon fiber bed.
25. system as claimed in claim 15 is characterized in that, the temperature of described metal getter is 400-800 ℃ of scope.
26. system as claimed in claim 15 is characterized in that, described metal getter contains the metal that is selected from down group: transition metal, copper, nickel, iron, manganese, zirconium-aluminium alloy and their mixture.
27. system as claimed in claim 15 is characterized in that, described particulate filter is selected from down group: wire cloth filter and agglomerating metal filter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2009101521310A CN101941684A (en) | 2009-07-10 | 2009-07-10 | Helium purifying method |
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| CN2009101521310A CN101941684A (en) | 2009-07-10 | 2009-07-10 | Helium purifying method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103159192A (en) * | 2011-12-13 | 2013-06-19 | 住友精化株式会社 | Purifying method and purifying device of helium |
| CN103626142A (en) * | 2013-11-28 | 2014-03-12 | 华南农业大学 | Helium low-pressure recycling, purification and storage device and application method thereof |
| CN104128071A (en) * | 2014-08-15 | 2014-11-05 | 苏州市兴鲁空分设备科技发展有限公司 | Helium purifying device |
| CN105139904A (en) * | 2015-08-25 | 2015-12-09 | 天鼎联创密封技术（北京）有限公司 | Molecular sieve device |
| CN108097036A (en) * | 2012-02-10 | 2018-06-01 | 恩特格里斯公司 | Gas purifier |
| CN108394878A (en) * | 2018-04-09 | 2018-08-14 | 西安保埃罗环保科技有限公司 | A kind of hydrogeneous helium tail gas purification Helium process |
| CN110302631A (en) * | 2019-07-18 | 2019-10-08 | 大连中鼎化学有限公司 | The purification devices and its technique of a kind of argon gas that can replace adsorption column online, helium and hydrogen |
| CN111977622A (en) * | 2019-05-23 | 2020-11-24 | 香港城市大学深圳研究院 | Helium purification method and device |
| CN113144821A (en) * | 2021-04-27 | 2021-07-23 | 大连理工大学 | Multi-technology integrated separation process for producing high-purity helium gas from helium-rich natural gas liquefaction tail gas |
-
2009
- 2009-07-10 CN CN2009101521310A patent/CN101941684A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103159192A (en) * | 2011-12-13 | 2013-06-19 | 住友精化株式会社 | Purifying method and purifying device of helium |
| CN108097036A (en) * | 2012-02-10 | 2018-06-01 | 恩特格里斯公司 | Gas purifier |
| CN103626142A (en) * | 2013-11-28 | 2014-03-12 | 华南农业大学 | Helium low-pressure recycling, purification and storage device and application method thereof |
| CN103626142B (en) * | 2013-11-28 | 2015-07-29 | 华南农业大学 | A kind of helium low pressure recovery, purifying and storage facilities and using method thereof |
| CN104128071A (en) * | 2014-08-15 | 2014-11-05 | 苏州市兴鲁空分设备科技发展有限公司 | Helium purifying device |
| CN105139904A (en) * | 2015-08-25 | 2015-12-09 | 天鼎联创密封技术（北京）有限公司 | Molecular sieve device |
| CN108394878A (en) * | 2018-04-09 | 2018-08-14 | 西安保埃罗环保科技有限公司 | A kind of hydrogeneous helium tail gas purification Helium process |
| CN108394878B (en) * | 2018-04-09 | 2019-03-05 | 西安保埃罗环保科技有限公司 | A kind of hydrogeneous helium tail gas purification Helium process |
| CN111977622A (en) * | 2019-05-23 | 2020-11-24 | 香港城市大学深圳研究院 | Helium purification method and device |
| CN110302631A (en) * | 2019-07-18 | 2019-10-08 | 大连中鼎化学有限公司 | The purification devices and its technique of a kind of argon gas that can replace adsorption column online, helium and hydrogen |
| CN113144821A (en) * | 2021-04-27 | 2021-07-23 | 大连理工大学 | Multi-technology integrated separation process for producing high-purity helium gas from helium-rich natural gas liquefaction tail gas |
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Application publication date: 20110112 |