CN104383784B - The system and method for separation and Extraction inert gas from environmental gas - Google Patents
The system and method for separation and Extraction inert gas from environmental gas Download PDFInfo
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- CN104383784B CN104383784B CN201410705017.7A CN201410705017A CN104383784B CN 104383784 B CN104383784 B CN 104383784B CN 201410705017 A CN201410705017 A CN 201410705017A CN 104383784 B CN104383784 B CN 104383784B
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Abstract
The disclosure relates to a kind of system of separation and Extraction inert gas from environmental gas, and described system comprises: except moisture device; Low-temperature fractionation device; Titanium sponge chemisorption apparatus; Gas-chromatography separator; Inert gas gathering-device; And vacuum plant.The disclosure also relates to a kind of method of separation and Extraction inert gas from environmental gas, and described method comprises: dewater step by step; Low-temperature fractionation step; Titanium sponge chemisorption step; Gas-chromatography separating step; Step is collected with inert gas.The disclosure also relates to the purposes that above system and method extracts for the separated in synchronization of microlitre magnitude Krypton and hundred milliliters of magnitude argon gas.
Description
Technical field
The disclosure relates to gaseous sample and is separated and inert gas extractive technique field, particularly relates to a kind of system and method for efficient separation and Extraction micro-inert gas wherein from a small amount of environmental gas.
Background technology
From a small amount of environmental gas (as solution gas air, underground water and ice core etc.), the system and method for efficient separation and Extraction inert gas is the technology that the methods such as a kind of novel comprehensive utilization low-temperature fractionation, chemisorbed and gas-chromatography are separated extract inert gas (argon gas and Krypton) wherein.The argon gas extracted by the method and Krypton sample, be can be used for the application such as isotope and tracer analysis of environmental sample, such as, carry out radio isotope
39ar and
81kr,
85kr surveys year etc.Be specially: for environmental gas sample (its Main Ingredients and Appearance is nitrogen, oxygen, methane etc.), first moisture and carbon dioxide is removed, then being separated argon gas and Krypton is realized by low-temperature fractionation method, titanium sponge is at high temperature utilized to carry out chemisorbed again, the nitrogen, oxygen, methane etc. of the removing overwhelming majority, realize the priority enrichment to argon gas and Krypton, finally utilize chromatographic process to be separated the Krypton after enrichment, finally realize the high efficiency extraction of argon gas and Krypton.
Because Krypton and the argon gas volume fraction in environmental gas sample is generally respectively a few millionths and 1% level, the while of needs in application, from an environmental gas sample, efficient separation and Extraction volume content differs two kinds of rare gas difficulty of four magnitudes very greatly, and especially sample total amount at hundreds of milliliter to tens of premium on currency at ordinary times.Separation and Extraction Krypton mainly single in the world or argon gas at present, normally used method is: for Krypton, and Krypton enrichment is carried out in the pure low temperature compression fractionation of general employing, then uses gas-chromatography to be separated Krypton ([1] Yokochi, R.; Heraty, L.J.; Sturchio, N.C.:MethodforPurificationofKryptonfromEnvironmentalSamp lesforAnalysisofRadiokryptonIsotopes.AnalyicalChemistry8 0 (2008), No.22,8688-8693).The maximum shortcoming of this method is exactly that the loss of Krypton is larger in pure low temperature compression fractionation stage, makes the separative efficiency of Krypton not high.For argon gas, the heavy dose of gas-chromatography separation method of general employing, directly obtains argon gas ([2] Riedmann, R.A.:SeparationofArgonfromatmosphericairandMeasurementso f by gaseous sample chromatographic isolation
37arforCTBTpurposes, UniversityofBern, Dissertation, 2011).Although this kind of method is direct, to chromatogram column filling and temperature control requirement high, and separative efficiency and product purity unsatisfactory.
Above-mentioned two kinds of methods can only realize the separation of Krypton to single or argon gas, process more complicated, and efficiency is not high, create very large restriction to application.
Summary of the invention
In embodiments more of the present disclosure, relate to a kind of system of separation and Extraction inert gas from environmental gas, described system comprises:
Except moisture device, described except moisture device is for removing moisture in environmental gas sample and carbon dioxide;
Low-temperature fractionation device, described low-temperature fractionation device is for loading from the described environmental gas sample except moisture device, and low-temperature fractionation is carried out to described environmental gas sample, produce and comprise the fractionation gas of most of argon gas and comprise the fractionation residual gas of a small amount of argon gas and most of Krypton;
Titanium sponge chemisorption apparatus, described titanium sponge chemisorption apparatus carries out chemisorbed under being used for high temperature, successively remove nitrogen, oxygen and the methane in the fractionation gas and fractionation residual gas that described low-temperature fractionation device produces, retain argon gas and Krypton, successively obtain argon gas and the rich krypton-85 gas comprising a small amount of argon gas and most of Krypton;
Gas-chromatography separator, described gas-chromatography separator adopts helium carrier gas to carry out chromatographic isolation to the rich krypton-85 gas obtained after described titanium sponge chemisorption apparatus chemisorbed;
Inert gas gathering-device, described inert gas gathering-device is for collecting inert gas, and the argon gas that the argon gas obtain described titanium sponge chemisorption apparatus adsorptive fractionation gas and described gas-chromatography separator obtain merges, and collects together; Further, described gas-chromatography separator is separated and obtains Krypton and be also admitted to inert gas gathering-device and collect; With
Vacuum plant, described vacuum plant is for generation of the vacuum condition needed for whole system.
In embodiments more of the present disclosure, described low-temperature fractionation device comprises:
Active carbon cylinder, described active carbon cylinder is equipped with active carbon, for physical absorption under liquid nitrogen temperature from the described environmental gas sample sent into except moisture device; And/or
Mass-flow gas meter, described mass-flow gas meter enters the speed of described titanium sponge chemisorption apparatus for controlling fractionation gas and fractionation residual gas in low-temperature fractionation process, and record enters the gas flow of described titanium sponge chemisorption apparatus respectively.
In embodiments more of the present disclosure, described titanium sponge chemisorption apparatus comprises:
Titanium sponge, described titanium sponge is used for carrying out chemisorbed under high temperature, successively removes nitrogen, oxygen, methane in the fractionation gas and fractionation residual gas that described low-temperature fractionation device sends into; And/or
Pyroreaction pipe, the effective container doing to react between described titanium sponge and gas of described pyroreaction; And/or
Pressure gauge, described pressure gauge, for monitoring the air pressure in titanium sponge adsorbent equipment, to judge the process of chemisorbed between described titanium sponge and fractionation gas, between described titanium sponge and fractionation residual gas, judges the deadline of chemisorbed.
In embodiments more of the present disclosure, described inert gas gathering-device comprises:
Argon gas collecting pipe, described argon gas collecting pipe is equipped with active carbon, for collecting the argon gas that obtains through described titanium sponge chemisorption apparatus chemisorbed fractionation gas under liquid nitrogen temperature and being separated the argon gas that obtains through described gas-chromatography separator to store; And/or
Krypton collecting pipe, described Krypton collecting pipe is equipped with active carbon, is separated the Krypton that obtains to store for collecting under liquid nitrogen temperature through described gas-chromatography separator.
In embodiments more of the present disclosure, described environmental gas is selected from solution gas in air, geothermal gas, Groundwater solution, surface water solution gas, ocean water solution gas and ice core.
In embodiments more of the present disclosure, relate to a kind of method of separation and Extraction inert gas from environmental gas, described method comprises:
Dewater step by step, wherein with the moisture removed except moisture device in environmental gas sample and carbon dioxide;
Low-temperature fractionation step, wherein with active carbon cylinder under liquid nitrogen temperature physical absorption by the described environmental gas sample sent into except moisture device, and low-temperature fractionation is carried out to environmental gas sample, produce and comprise the fractionation gas of most of argon gas and comprise the fractionation residual gas of a small amount of argon gas and most of Krypton;
Titanium sponge chemisorption step, wherein under manometric supervision, in pyroreaction pipe, high temeperature chemistry absorption is carried out with titanium sponge, remove described low-temperature fractionation device produce fractionation gas and fractionation residual gas in nitrogen, oxygen, methane, retain argon gas and Krypton, successively obtain argon gas and the rich krypton-85 gas comprising a small amount of argon gas and most of Krypton;
Gas-chromatography separating step, the rich krypton-85 gas obtained after described titanium sponge chemisorption apparatus chemisorbed is wherein loaded with injection annulus, the rich krypton-85 gas that helium carrier gas purges in injection annulus enters chromatographic column, argon gas in rich krypton-85 gas, nitrogen are separated through chromatographic column with Krypton, then are purged successively to enter in described inert gas gathering-device by helium carrier gas and collect;
Inert gas collects step, wherein the argon gas obtained through titanium sponge high temeperature chemistry adsorptive fractionation gas is separated with gas-chromatography the argon gas obtained to merge, send in argon gas collecting pipe together and collect, and gas-chromatography is separated in the Krypton feeding Krypton collecting pipe obtained and collects.
In embodiments more of the present disclosure, in described low-temperature fractionation step, under liquid nitrogen temperature, described in physical absorption, remove the environmental gas sample of moisture device feeding with the active carbon be equipped with in the active carbon cylinder in described low-temperature fractionation device; And/or
In described titanium sponge chemisorption step, control fractionation gas and fractionation residual gas in low-temperature fractionation process with the mass-flow gas meter in described low-temperature fractionation device and enter the speed of described titanium sponge chemisorption apparatus, and record enters the gas flow of described titanium sponge chemisorption apparatus respectively; And/or
In described titanium sponge chemisorption step, at high temperature carry out chemisorbed with the titanium sponge in described titanium sponge chemisorption apparatus, successively remove described low-temperature fractionation device send into fractionation gas and fractionation residual gas in nitrogen, oxygen, methane; And/or
In described titanium sponge chemisorption step, with the pyroreaction pipe in described titanium sponge chemisorption apparatus as the container reacted between titanium sponge and gas.
In embodiments more of the present disclosure, to be effectively separated and enrichment volume fraction respectively differs argon gas and the Krypton of four orders of magnitude.
In embodiments more of the present disclosure, described environmental gas is selected from solution gas in air, geothermal gas, Groundwater solution, surface water solution gas, ocean water solution gas and ice core.
In embodiments more of the present disclosure, relate to the purposes that system in the disclosure or method are extracted for the separated in synchronization of microlitre magnitude Krypton and hundred milliliters of magnitude argon gas.
Accompanying drawing explanation
In order to be illustrated more clearly in disclosure embodiment or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, the accompanying drawing that the following describes is only some embodiments recorded in the disclosure, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is a kind of structural representation of the disclosed a kind of system of efficient separation and Extraction inert gas from a small amount of environmental gas (as solution gas air, underground water and ice core etc.) of disclosure embodiment;
Detailed description of the invention
In view of this, specific embodiments more of the present disclosure relate to a kind of system and method for efficient separation and Extraction inert gas from a small amount of environmental gas (as solution gas air, underground water and ice core etc.), to improve separation and Extraction efficiency.Technical scheme is as follows:
Specific embodiments more of the present disclosure relate to a kind of system of efficient separation and Extraction inert gas from a small amount of environmental gas (as solution gas air, underground water and ice core etc.), comprise: vacuum plant, except moisture device, low-temperature fractionation device, titanium sponge chemisorption apparatus, gas-chromatography separator, inert gas gathering-device, wherein:
Described except moisture device is for removing moisture in environmental gas sample (its Main Ingredients and Appearance is nitrogen, oxygen, methane etc.) and carbon dioxide, environmental gas sample is admitted to described low-temperature fractionation device subsequently;
Described low-temperature fractionation device is for loading environmental gas sample, and low-temperature fractionation is carried out to environmental gas sample, produce fractionation gas (comprising main argon gas) and fractionation residual gas (comprising a small amount of argon gas and main Krypton), realize being separated argon gas and Krypton;
Described titanium sponge chemisorption apparatus carries out chemisorbed under being used for high temperature, successively remove the nitrogen, oxygen, methane etc. in the fractionation gas and fractionation residual gas that described low-temperature fractionation device produces, argon gas and Krypton are retained, successively obtain argon gas and rich krypton-85 gas (comprising a small amount of argon gas and main Krypton), realize the enrichment to argon gas and Krypton;
Described gas-chromatography separator comprises chromatographic column, injection annulus and helium carrier gas, described injection annulus loads the rich krypton-85 gas obtained after described titanium sponge chemisorption apparatus chemisorbed, the rich krypton-85 gas that described helium carrier gas purges in injection annulus enters in described chromatographic column, argon gas in rich krypton-85 gas, nitrogen are separated through chromatographic column with Krypton, purged successively to enter in described inert gas gathering-device by helium carrier gas again and collect, thus realize the separation of Krypton;
Described inert gas gathering-device is for collecting inert gas, the argon gas that the argon gas obtain described titanium sponge chemisorption apparatus adsorptive fractionation gas and described gas-chromatography separator obtain merges, send into inert gas gathering-device together to collect, finally store; Similarly, described gas-chromatography separator is separated and obtains Krypton and be also admitted to inert gas gathering-device and collect;
Described vacuum plant comprises stainless-steel vacuum pipeline, vacuum valve, vacuum seal and vacuum pump system, for generation of the vacuum condition needed for experiment.
In specific embodiments more of the present disclosure, described low-temperature fractionation device also comprises:
Active carbon cylinder;
Described active carbon cylinder, is equipped with active carbon, for the environmental gas sample that de-watering apparatus described in physical absorption under liquid nitrogen temperature is sent into.
In specific embodiments more of the present disclosure, described low-temperature fractionation device also comprises:
Mass-flow gas meter;
Described mass-flow gas meter, enters the speed of described titanium sponge chemisorption apparatus for controlling fractionation gas and fractionation residual gas in low-temperature fractionation process, and record enters the gas flow of described titanium sponge chemisorption apparatus respectively.
In specific embodiments more of the present disclosure, described titanium sponge chemisorption apparatus comprises:
Titanium sponge;
Described titanium sponge, for carrying out chemisorbed under high temperature, successively remove described low-temperature fractionation device send into fractionation gas and fractionation residual gas in nitrogen, oxygen, methane etc.
In specific embodiments more of the present disclosure, described titanium sponge chemisorption apparatus also comprises:
Pyroreaction pipe;
Described pyroreaction pipe, for the container reacted between described titanium sponge and gas.
In specific embodiments more of the present disclosure, described titanium sponge chemisorption apparatus also comprises:
Pressure gauge;
Described pressure gauge, for monitoring the air pressure in titanium sponge adsorbent equipment, for judging the process of chemisorbed between described titanium sponge and fractionation gas, between described titanium sponge and fractionation residual gas, judges the deadline of chemisorbed.
In specific embodiments more of the present disclosure, described inert gas gathering-device comprises:
Argon gas collecting pipe;
Described argon gas collecting pipe, is equipped with active carbon, for collecting the argon gas that obtains through described titanium sponge chemisorption apparatus chemisorbed fractionation gas under liquid nitrogen temperature and being separated the argon gas obtained through described gas-chromatography separator, finally stores.
In specific embodiments more of the present disclosure, described inert gas gathering-device also comprises:
Krypton collecting pipe;
Described Krypton collecting pipe, is equipped with active carbon, being separated the Krypton obtained, finally storing for collecting under liquid nitrogen temperature through described gas-chromatography separator.
In specific embodiments more of the present disclosure, also relate to a kind of method of efficient separation and Extraction inert gas from a small amount of environmental gas (as solution gas air, underground water and ice core etc.), comprising:
Except moisture, except the moisture in moisture device removing environmental gas sample (its Main Ingredients and Appearance is nitrogen, oxygen, methane etc.) and carbon dioxide, environmental gas sample is admitted to described low-temperature fractionation device subsequently;
Low-temperature fractionation, the environmental gas sample that moisture device is sent into is removed described in physical absorption under active carbon cylinder liquid nitrogen temperature, and low-temperature fractionation is carried out to environmental gas sample, produce fractionation gas (comprising main argon gas) and fractionation residual gas (comprising a small amount of argon gas and main Krypton), realize being separated argon gas and Krypton;
Titanium sponge chemisorbed, under manometric supervision, titanium sponge carries out high temeperature chemistry absorption in pyroreaction pipe, remove described low-temperature fractionation device produce fractionation gas and fractionation residual gas in nitrogen, oxygen, methane etc., argon gas and Krypton are retained, successively obtain argon gas and rich krypton-85 gas (comprising a small amount of argon gas and main Krypton), realize the enrichment to argon gas and Krypton;
Gas-chromatography is separated, injection annulus loads the rich krypton-85 gas obtained after described titanium sponge chemisorption apparatus chemisorbed, the rich krypton-85 gas that helium carrier gas purges in injection annulus enters chromatographic column, the compositions such as the argon gas in rich krypton-85 gas, nitrogen and Krypton are separated through chromatographic column, purged successively to enter in described inert gas gathering-device by helium carrier gas again and collect, thus realize the separation of Krypton;
Inert gas is collected, and the argon gas obtained is separated with gas-chromatography the argon gas obtained merges through titanium sponge high temeperature chemistry adsorptive fractionation gas, sends in argon gas collecting pipe together and collects, finally store; Gas-chromatography is separated in the Krypton feeding Krypton collecting pipe obtained and collects, finally store.
In specific embodiments more of the present disclosure, also comprise:
Active carbon cylinder in described low-temperature fractionation device, is equipped with active carbon, for the environmental gas sample that de-watering apparatus described in physical absorption under liquid nitrogen temperature is sent into.
In specific embodiments more of the present disclosure, also comprise:
Mass-flow gas meter in described low-temperature fractionation device, enters the speed of described titanium sponge chemisorption apparatus for controlling fractionation gas and fractionation residual gas in low-temperature fractionation process, and record enters the gas flow of described titanium sponge chemisorption apparatus respectively.
In specific embodiments more of the present disclosure, also comprise:
Titanium sponge in described titanium sponge chemisorption apparatus, for carrying out chemisorbed under high temperature, successively remove described low-temperature fractionation device send into fractionation gas and fractionation residual gas in nitrogen, oxygen, methane etc.
In specific embodiments more of the present disclosure, also comprise:
Pyroreaction pipe in described titanium sponge chemisorption apparatus, for the container reacted between titanium sponge and gas.
For enabling above-mentioned purpose of the present disclosure, feature and advantage become apparent more, are described in further detail the disclosure below in conjunction with the drawings and specific embodiments.
Embodiment
Refer to Fig. 1, Fig. 1 is the system of the open a kind of efficient separation and Extraction inert gas from a small amount of environmental gas (as solution gas air, underground water and ice core etc.) of disclosure embodiment, comprise: except moisture device 102, low-temperature fractionation device 110, titanium sponge chemisorption apparatus 120, gas-chromatography separator 103, inert gas gathering-device 130 and vacuum plant 101, wherein:
Whole device vacuumizes by vacuum plant 101, is passed into by environmental gas sample (its Main Ingredients and Appearance is nitrogen, oxygen, methane etc.) except moisture device 102 removes moisture wherein and carbon dioxide.
Under liquid nitrogen temperature, environmental gas sample is sent in the active carbon cylinder 1101 in low-temperature fractionation device 110, under the control of mass-flow gas meter 1102, fractionation gas in active carbon cylinder 1101 and fractionation residual gas are successively passed in titanium sponge chemisorption apparatus 120, realize being separated of argon gas and Krypton.
Titanium sponge 1201 in titanium sponge chemisorption apparatus 120, under the supervision of pressure gauge 1203, high temeperature chemistry absorption is carried out in pyroreaction pipe 1202, argon gas and Krypton are retained, successively obtain argon gas and rich krypton-85 gas (comprising a small amount of argon gas and main Krypton), realize the enrichment of argon gas and Krypton.
The rich krypton-85 gas produced by titanium sponge 1201 high temperature adsorption is sent in gas-chromatography separator 103, realizes the separation of Krypton.
The argon gas obtain titanium sponge 1201 high temperature adsorption and gas-chromatography separator 103 are separated the argon gas obtained and merge, and together send in the argon gas collecting pipe 1301 of inert gas gathering-device 130 and collect, finally store; The Krypton obtained after being separated by gas-chromatography separator 103 is sent in the Krypton collecting pipe 1302 of inert gas gathering-device 130 and is collected, and finally stores.
It is very high that inventor sums up one separative efficiency of the system of efficient separation and Extraction inert gas from a small amount of environmental gas (as air, underground water and ice core solution gas etc.) disclosed in disclosure embodiment through many experiments, can quickly and easily from a small amount of environmental gas simultaneously expeditiously separation and Extraction go out microlitre Krypton and hundred milliliters of argon gas, there is great using value and prospect.
Claims (10)
1. the system of separation and Extraction inert gas from environmental gas, described system comprises:
Except moisture device, described except moisture device is for removing moisture in environmental gas sample and carbon dioxide;
Low-temperature fractionation device, described low-temperature fractionation device is for loading from the described environmental gas sample except moisture device, and low-temperature fractionation is carried out to described environmental gas sample, produce the fractionation residual gas comprising the fractionation gas of most of argon gas and generation and comprise a small amount of argon gas and most of Krypton;
Titanium sponge chemisorption apparatus, described titanium sponge chemisorption apparatus carries out chemisorbed under being used for high temperature, first remove nitrogen, oxygen and the methane in the fractionation gas of described low-temperature fractionation device generation, nitrogen, oxygen and methane in rear removing fractionation residual gas, retain argon gas and Krypton, first obtain argon gas, after obtain the rich krypton-85 gas comprising a small amount of argon gas and most of Krypton;
Gas-chromatography separator, described gas-chromatography separator adopts helium carrier gas to carry out chromatographic isolation to the rich krypton-85 gas obtained after described titanium sponge chemisorption apparatus chemisorbed;
Inert gas gathering-device, described inert gas gathering-device is for collecting inert gas, and the argon gas that the argon gas obtain described titanium sponge chemisorption apparatus adsorptive fractionation gas and described gas-chromatography separator obtain merges, and collects together; Further, described gas-chromatography separator is separated the Krypton obtained and is also admitted to inert gas gathering-device and collects; With
Vacuum plant, described vacuum plant is for generation of the vacuum condition needed for whole system.
2. the system of separation and Extraction inert gas from environmental gas according to claim 1, wherein said low-temperature fractionation device comprises:
Active carbon cylinder, described active carbon cylinder is equipped with active carbon, for physical absorption under liquid nitrogen temperature from the described environmental gas sample sent into except moisture device; And/or
Mass-flow gas meter, described mass-flow gas meter enters the speed of described titanium sponge chemisorption apparatus for controlling fractionation gas and fractionation residual gas in low-temperature fractionation process, and record enters the gas flow of described titanium sponge chemisorption apparatus respectively.
3. the system of separation and Extraction inert gas from environmental gas according to claim 1, wherein said titanium sponge chemisorption apparatus comprises:
Titanium sponge, described titanium sponge carries out chemisorbed under being used for high temperature, first removes nitrogen, oxygen, methane in the fractionation gas of described low-temperature fractionation device feeding, nitrogen, oxygen, methane in rear removing fractionation residual gas; And/or
Pyroreaction pipe, the effective container doing to react between described titanium sponge and gas of described pyroreaction; And/or
Pressure gauge, described pressure gauge, for monitoring the air pressure in titanium sponge chemisorption apparatus, to judge the process of chemisorbed between described titanium sponge and fractionation gas, between described titanium sponge and fractionation residual gas, judges the deadline of chemisorbed.
4. the system of separation and Extraction inert gas from environmental gas according to claim 1, wherein said inert gas gathering-device comprises:
Argon gas collecting pipe, described argon gas collecting pipe is equipped with active carbon, for collecting the argon gas that obtains through described titanium sponge chemisorption apparatus chemisorbed fractionation gas under liquid nitrogen temperature and being separated the argon gas that obtains through described gas-chromatography separator to store; And/or
Krypton collecting pipe, described Krypton collecting pipe is equipped with active carbon, is separated the Krypton that obtains to store for collecting under liquid nitrogen temperature through described gas-chromatography separator.
5. the system of separation and Extraction inert gas from environmental gas described in any one in claim 1-4, wherein said environmental gas is selected from solution gas in air, geothermal gas, Groundwater solution, surface water solution gas, ocean water solution gas and ice core.
6. the method for separation and Extraction inert gas from environmental gas, described method comprises:
Dewater step by step, wherein with the moisture removed except moisture device in environmental gas sample and carbon dioxide;
Low-temperature fractionation step, wherein with active carbon cylinder under liquid nitrogen temperature physical absorption by the described environmental gas sample sent into except moisture device, and low-temperature fractionation is carried out to environmental gas sample, produce the fractionation gas comprising most of argon gas, and produce the fractionation residual gas comprising a small amount of argon gas and most of Krypton;
Titanium sponge chemisorption step, wherein under manometric supervision, in pyroreaction pipe, high temeperature chemistry absorption is carried out with titanium sponge, first remove nitrogen, oxygen, the methane in the fractionation gas of low-temperature fractionation device generation, nitrogen, oxygen, methane in rear removing fractionation residual gas, retain argon gas and Krypton, first obtain argon gas, after obtain the rich krypton-85 gas comprising a small amount of argon gas and most of Krypton;
Gas-chromatography separating step, the rich krypton-85 gas obtained after titanium sponge chemisorption apparatus chemisorbed is wherein loaded with injection annulus, the rich krypton-85 gas that helium carrier gas purges in injection annulus enters chromatographic column, argon gas in rich krypton-85 gas, nitrogen are separated through chromatographic column with Krypton, then are purged successively to enter in inert gas gathering-device by helium carrier gas and collect;
Inert gas collects step, wherein the argon gas obtained through titanium sponge high temeperature chemistry adsorptive fractionation gas is separated with gas-chromatography the argon gas obtained to merge, send in argon gas collecting pipe together and collect, and gas-chromatography is separated in the Krypton feeding Krypton collecting pipe obtained and collects.
7. the method for separation and Extraction inert gas from environmental gas according to claim 6, wherein:
In described low-temperature fractionation step, under liquid nitrogen temperature, described in physical absorption, remove the environmental gas sample of moisture device feeding with the active carbon be equipped with in the active carbon cylinder in low-temperature fractionation device; And/or
In described titanium sponge chemisorption step, control fractionation gas and fractionation residual gas in low-temperature fractionation process with the mass-flow gas meter in described low-temperature fractionation device and enter the speed of titanium sponge chemisorption apparatus, and record enters the gas flow of described titanium sponge chemisorption apparatus respectively; And/or
In described titanium sponge chemisorption step, at high temperature chemisorbed is carried out with the titanium sponge in described titanium sponge chemisorption apparatus, first remove nitrogen, oxygen, the methane in the fractionation gas of described low-temperature fractionation device feeding, nitrogen, oxygen, methane in rear removing fractionation residual gas; And/or
In described titanium sponge chemisorption step, with the pyroreaction pipe in described titanium sponge chemisorption apparatus as the container reacted between titanium sponge and gas.
8. the method for separation and Extraction inert gas from environmental gas according to claim 6, is wherein effectively separated and enrichment volume fraction respectively differs argon gas and the Krypton of four orders of magnitude.
9. the method for separation and Extraction inert gas from environmental gas described in any one in claim 6-8, wherein said environmental gas is selected from solution gas in air, geothermal gas, Groundwater solution, surface water solution gas, ocean water solution gas and ice core.
10. the purposes that the separated in synchronization that the system described in any one in claim 1-5 or the method described in any one in claim 6-9 are used for microlitre magnitude Krypton and hundred milliliters of magnitude argon gas is extracted.
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| CN106512702A (en) * | 2016-12-08 | 2017-03-22 | 天津工业大学 | Online purification method for inert gases based on titanium metallic chemical properties |
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| CN109323909B (en) * | 2018-10-22 | 2020-10-27 | 中国科学技术大学 | Gas automatic separation system for inertness in small-gas-volume environment sample |
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| CN1498851A (en) * | 2002-11-01 | 2004-05-26 | 日本派欧尼株式会社 | Refining method of inert gas |
| CN102282100A (en) * | 2009-01-14 | 2011-12-14 | 赖卡有限公司 | Method and device for separating argon from a gas mixture |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1241985A (en) * | 1996-12-24 | 2000-01-19 | 液体空气乔治洛德方法利用和研究有限公司 | Method for purifying a cryogenic fluid by filtration and adsorption |
| CN1420079A (en) * | 2001-11-19 | 2003-05-28 | 气体产品与化学公司 | Method and adsorbent for recovering kryptsn and xenon from gas stream or liquid stream |
| CN1498851A (en) * | 2002-11-01 | 2004-05-26 | 日本派欧尼株式会社 | Refining method of inert gas |
| CN102282100A (en) * | 2009-01-14 | 2011-12-14 | 赖卡有限公司 | Method and device for separating argon from a gas mixture |
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