CN109879259A - A kind of ultra-pure xenon, krypton purification system and purification process - Google Patents
A kind of ultra-pure xenon, krypton purification system and purification process Download PDFInfo
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- CN109879259A CN109879259A CN201910296960.XA CN201910296960A CN109879259A CN 109879259 A CN109879259 A CN 109879259A CN 201910296960 A CN201910296960 A CN 201910296960A CN 109879259 A CN109879259 A CN 109879259A
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- 238000000746 purification Methods 0.000 title claims abstract description 31
- 229910052724 xenon Inorganic materials 0.000 title claims abstract description 28
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052743 krypton Inorganic materials 0.000 title claims abstract description 26
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 33
- 239000003054 catalyst Substances 0.000 claims abstract description 31
- 238000001179 sorption measurement Methods 0.000 claims abstract description 29
- 230000006698 induction Effects 0.000 claims abstract description 27
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 17
- 238000005192 partition Methods 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 239000003463 adsorbent Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 230000003647 oxidation Effects 0.000 claims abstract description 9
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 9
- 238000010521 absorption reaction Methods 0.000 claims abstract description 8
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 7
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 59
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001569 carbon dioxide Substances 0.000 claims description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000002808 molecular sieve Substances 0.000 claims description 8
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910001868 water Inorganic materials 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 7
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 7
- 239000000956 alloy Substances 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- -1 methane hydrocarbon Chemical class 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 claims description 4
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 claims description 3
- 150000002222 fluorine compounds Chemical class 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 3
- DNNSSWSSYDEUBZ-OUBTZVSYSA-N krypton-85 Chemical compound [85Kr] DNNSSWSSYDEUBZ-OUBTZVSYSA-N 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- PZZOEXPDTYIBPI-UHFFFAOYSA-N 2-[[2-(4-hydroxyphenyl)ethylamino]methyl]-3,4-dihydro-2H-naphthalen-1-one Chemical compound C1=CC(O)=CC=C1CCNCC1C(=O)C2=CC=CC=C2CC1 PZZOEXPDTYIBPI-UHFFFAOYSA-N 0.000 description 1
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- WMIYKQLTONQJES-UHFFFAOYSA-N hexafluoroethane Chemical compound FC(F)(F)C(F)(F)F WMIYKQLTONQJES-UHFFFAOYSA-N 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000003434 inspiratory effect Effects 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Landscapes
- Separation By Low-Temperature Treatments (AREA)
Abstract
The invention belongs to high-purity gas purification arts, more particularly, to a kind of ultra-pure xenon, krypton purification system and purification process.It include raw material gas cylinder using purification system, unstripped gas is stored in raw material gas cylinder, raw material gas cylinder connection heating room, heating is outdoor to be equipped with insulating layer, insulating layer is externally provided with heating layer, it heats room and connects catalyst chamber bottom, there is catalyst in catalyst chamber, catalyst chamber connects adsorption chamber, partition is equipped in adsorption chamber, adsorption chamber is divided into labyrinth-like channel, adsorbent is equipped in adsorption chamber, adsorption chamber connects induction chamber, metal getter room is equipped in induction chamber, partition is equipped in induction chamber, induction chamber is divided into labyrinth-like channel, induction chamber linking parsing instrument, by being connected with valvular airflow pipeline between each component, present invention combination catalysis oxidation, chemical reaction, three kinds of principles of physical absorption, depth purified feed stock gas, remove xenon, C5 or more hydrocarbon component and fluoride in krypton-85 gas, reach ultra-pure rank, meet electric propulsion With the technical requirements of xenon, krypton.
Description
Technical field
The invention belongs to high-purity gas purification arts, more particularly, to a kind of ultra-pure xenon, krypton purification system and purifying side
Method.
Background technique
Electric propulsion is widely used in space propultion as one of space electric propulsion technology, as Spacecraft Attitude Control,
Position holding, orbit maneuver and space flight etc..The propellant that electric propulsion system uses is generally the indifferent gas such as xenon, Krypton
Body, the purity of gas are thrust, specific impulse, efficiency and the key problem in technology in service life for guaranteeing electric propulsion.Water impurity, oxygen in xenon, krypton
The exceeded cathode oxidation for be easy to causeing electric propulsion system of content causes its service life impaired;The objectionable impurities such as carbide, fluoride are easy
Deposition is covered in emitter surface, will directly affect thrust, specific impulse and the efficiency of electric propulsion.Impurity in xenon and Krypton is main
There are nitrogen, oxygen, hydrogen, carbon monoxide, carbon dioxide, methane, perfluoroethane, carbon tetrafluoride etc..At present in purification xenon and Krypton
In method, mainly have using Activated carbon separation, step by step enriching and purifying, and the side of concentration, heat exchange vaporization, reaction after-purification absorption
Formula.Aspect is removed for the purifying of the low content impurity gas in ultra-pure xenon, Krypton, then mature technique is not reported.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of ultra-pure xenon, krypton purification system and purification process.
The complete technical solution of the present invention includes:
A kind of ultra-pure xenon, krypton purification system, which includes raw material gas cylinder, heats room, catalyst chamber, and adsorption chamber is inhaled
Gas chamber, analyzer, above-mentioned each component pass sequentially through the connection of the airflow pipeline with valve;
Wherein, heating is outdoor is equipped with insulating layer, and insulating layer is externally provided with heating layer;There is catalyst in catalyst chamber, in adsorption chamber
Equipped with adsorbent, metal getter is equipped in induction chamber.
Preferably, it heats in outdoor heating layer and is provided with resistance heating wire;
Preferably, heating room connects catalyst chamber bottom;
Preferably, it is equipped with partition in adsorption chamber, adsorption chamber is divided into labyrinth-like channel;
Preferably, it is equipped with partition in induction chamber, entire induction chamber is divided into labyrinth-like channel.
According to above system, inventor has invented a kind of ultra-pure xenon, krypton purification process, specifically comprises the following steps:
Open valve, unstripped gas enter heating room from raw material gas cylinder, open the resistance heating wire in heating layer and start to add
Heating room temperature is heated to 380~420 DEG C, enters catalyst chamber from bottom through pipeline after, control the unstrpped gas of entrance by heat
Pressure is 0.1-0.4MPa, blows the indoor catalyst of catalysis, makes it in boiling-like, plays the catalysis reaction effect of similar fluidized bed
Fruit makes hydrogen, carbon monoxide, methane and non-methane hydrocarbon in gas in the presence of having micro amount of oxygen, high
By quickly becoming carbon dioxide and water under the intense contact with catalyst under temperature;Later on valve, makes through catalysis oxidation
Gas enters adsorption chamber, and gas is flowed in adsorption chamber along labyrinth passage, by adsorbent of molecular sieve, by the dioxy in gas
Change carbon, water carries out selective absorption;Gas through catalysis oxidation enters induction chamber, and metal getter, gas are placed in induction chamber
Body is flowed in induction chamber along the labyrinth passage that partition is divided into, by metal getter, by carbon tetrafluoride, the hexafluoro in gas
Change fluorides and remaining micro amount of oxygen, hydrogen, carbon monoxide, methane or the non-methane hydrocarbon Adsorptions such as carbon,
Gas after air-breathing finally enters analyzer and carries out purity analysis, obtains ultra-pure gases.
Wherein, the catalyst in catalyst chamber is Pd75Pt25Alloy, partial size 10-30nm.Raw material gas flow is 2-4m3/
min。
Adsorbent of molecular sieve is a kind of silicate compound with cubic lattice, and it is more to common are A type, X-type, Y type etc.
Kind model, the present invention mainly use 4A type or 5A type adsorbent of molecular sieve, partial size 0.3-0.5cm, aperture 10-30nm;
The indoor metal getter of air-breathing is NiZrTi alloy, partial size 0.1-0.2cm.
The present invention compared with the existing technology the advantages of be: present invention combination catalysis oxidation, chemical reaction, physical absorption three
Kind principle, depth purified feed stock gas remove xenon, the hydrogen in krypton-85 gas, carbon monoxide, carbon dioxide, nitrogen, oxygen, water, hydro carbons
Component and fluoride reach ultra-pure rank, meet the technical requirements of electric propulsion xenon, krypton.It can be used in catalysis similar
Fluidized bed type working method, greatly improves purification efficiency.Adsorption chamber and induction chamber use maze-type structure, make gas wherein
Path extension is flowed through, absorption and inspiratory effects are improved.
Detailed description of the invention
Fig. 1 is ultra-pure xenon disclosed by the invention, krypton purification system structural schematic diagram.
In figure: 1- raw material gas cylinder, 2- heat room, 3- insulating layer, 4- heating layer, 5- catalyst chamber, 6- catalyst, 7- absorption
Room, 8- partition, 9- adsorbent, 10- induction chamber, 11- metal getter, 12- partition, 13- analyzer, 14- airflow pipeline, 15-
Valve.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and detailed description.
As shown in Figure 1, a kind of ultra-pure xenon disclosed by the invention, krypton purification system, including sample gas cylinder 1, unstripped gas
Unstripped gas is stored in steel cylinder, raw material gas cylinder connection heating room 2, heating is outdoor to be equipped with insulating layer 3, and insulating layer is externally provided with heating
Layer 4, heating room connect 5 bottom of catalyst chamber, there is catalyst in catalyst chamber, and catalyst chamber 5 connects adsorption chamber 7, be equipped in adsorption chamber 7 every
Adsorption chamber 7 is divided into labyrinth-like channel by plate 8, is equipped with adsorbent 9 in adsorption chamber 7, and adsorption chamber connects induction chamber 10, in induction chamber
Equipped with metal getter 11, it is equipped with partition 12 in induction chamber, induction chamber 10 is divided into labyrinth-like channel, 10 linking parsing of induction chamber
Instrument 13 passes through the airflow pipeline 14 with valve 15 between each component and connects.
Ultra-pure xenon disclosed by the invention, krypton purification process, specifically comprise the following steps:
Opening valve 15, unstripped gas enter heating room from raw material gas cylinder, open the resistance heating wire in heating layer and start to add
Heat, heating layer and heating room between be equipped with thermal insulation material, will heating room temperature be heated to (380~420) DEG C, after through pipeline from
Bottom enters catalyst chamber, and the feedstock gas pressures for controlling entrance are 0.25MPa, blows the indoor catalyst of catalysis, makes it in boiling
Shape is risen, the catalysis reaction effect of similar fluidized bed is played, keeps hydrogen in gas, carbon monoxide, methane and non-methane class hydrocarbon
Compound in the presence of having micro amount of oxygen, under high temperature by under the intense contact with catalyst quickly become carbon dioxide and
Water can suitably increase the indoor oxygen content of catalysis, enable the hydrocarbon substance fully reacting in gas, specific increased oxygen
Content can be by detecting the carbohydrate content in unstripped gas before being catalyzed.Catalyst used is Pd75Pt25Alloy, partial size
For 10-30nm.Raw material gas flow is 2-4m3/ min is blasted by experimental verification using the gas under 380~420 DEG C of high temperature
Mode, the micro amount of oxygen in unstripped gas can be made to be combined under the action of catalyst with carbon hydrogen element in 30-60s, it is raw
Cheng Shui and carbon dioxide, and if temperature is at 160-200 DEG C or so, catalytic effect significantly reduces, 5-10min is generally required,
Since whole process of purification is streamlined operation, present invention employs the catalysis reactions under high temperature, make purification efficiency significantly
It improves.
Later on valve makes the gas through catalysis oxidation enter adsorption chamber, is equipped with partition in adsorption chamber, will entirely adsorb
Room is divided into maze-type structure, and adsorbent of molecular sieve, partial size 0.3-0.5cm, aperture 10-30nm, gas are placed between partition
Body can be flowed in adsorption chamber along labyrinth passage that partition is divided into, by adsorbent of molecular sieve, by gas carbon dioxide,
Water carries out selective absorption.
So that the gas through catalysis oxidation is entered induction chamber, is equipped with partition in induction chamber, entire induction chamber is divided into labyrinth type
Structure, is placed with metal getter between partition, and metal getter is NiZrTi alloy, partial size 0.1-0.2cm, and gas is being inhaled
Gas chamber is flowed along the labyrinth passage that partition is divided into, by metal getter, by carbon tetrafluoride, the carbon hexa fluoride etc. in gas
The Adsorption of fluoride.
Gas after air-breathing finally enters analyzer and carries out purity analysis, and detection is qualified, obtains ultra-pure gases.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification to the above embodiments, change and equivalent structural changes, still fall within skill of the present invention
In the protection scope of art scheme.
Claims (9)
1. a kind of ultra-pure xenon, krypton purification system, which is characterized in that the system includes raw material gas cylinder (1), heats room (2), urges
Change room (5), adsorption chamber (7), induction chamber (10), analyzer (13), above-mentioned each component passes sequentially through the gas flow tube with valve (15)
Road (14) connection;
Wherein, heating room (2) is externally provided with insulating layer (3), and insulating layer (3) is externally provided with heating layer (4);There is catalysis in catalyst chamber (5)
Agent (6), adsorption chamber (7) is interior to be equipped with adsorbent (9), is equipped with metal getter (11) in induction chamber (10).
2. a kind of ultra-pure xenon according to claim 1, krypton purification system, which is characterized in that the heating of heating room (2) outside
Resistance heating wire is provided in layer (4).
3. a kind of ultra-pure xenon, krypton purification system, which is characterized in that heating room (2) connects catalyst chamber (5) bottom.
4. a kind of ultra-pure xenon, krypton purification system, which is characterized in that be equipped with partition (8) in adsorption chamber (7), by adsorption chamber (7) every
At labyrinth-like channel.
5. a kind of ultra-pure xenon, krypton purification system, which is characterized in that partition (12) are equipped in induction chamber (10), by entire air-breathing
Room (10) is divided into labyrinth-like channel.
6. a kind of ultra-pure xenon using system described in claim 1, krypton purification process, which is characterized in that specifically include as follows
Step:
Open valve, unstripped gas enter heating room from raw material gas cylinder, and the resistance heating wire opened in heating layer begins to warm up, will
Heating room temperature is heated to 380~420 DEG C, enters catalyst chamber from bottom through pipeline after, controls the feedstock gas pressures of entrance
For 0.1-0.4MPa, blow the indoor catalyst of catalysis, make it in boiling-like, make hydrogen in gas, carbon monoxide, methane and
Non-methane hydrocarbon is in the presence of having micro amount of oxygen, by fast rapid-result under the intense contact with catalyst under high temperature
For carbon dioxide and water;Later on valve makes the gas through catalysis oxidation enter adsorption chamber, and gas is in adsorption chamber along labyrinth
Carbon dioxide, water in gas is carried out selective absorption by adsorbent of molecular sieve by the flowing of formula channel;Through catalysis oxidation
Gas enters induction chamber, and metal getter, the labyrinth passage that gas is divided into induction chamber along partition are placed in induction chamber
Flowing, by metal getter, by the fluorides such as carbon tetrafluoride, carbon hexa fluoride in gas and remaining micro amount of oxygen, hydrogen,
Carbon monoxide, methane or non-methane hydrocarbon Adsorption, the gas after air-breathing finally enter analyzer progress
Purity analysis obtains ultra-pure gases.
7. ultra-pure xenon according to claim 6, krypton purification process, which is characterized in that the catalyst in catalyst chamber is
Pd75Pt25Alloy, partial size 10-30nm.
8. ultra-pure xenon according to claim 6, krypton purification process, which is characterized in that adsorbent of molecular sieve uses 4A type
Or 5A type adsorbent of molecular sieve, partial size 0.3-0.5cm, aperture 10-30nm.
9. ultra-pure xenon according to claim 6, krypton purification process, which is characterized in that the indoor metal getter of air-breathing
For NiZrTi alloy, partial size 0.1-0.2cm.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110467164A (en) * | 2019-08-20 | 2019-11-19 | 中国科学院合肥物质科学研究院 | A kind of inert gas high temperature purification system |
CN112250050A (en) * | 2020-10-27 | 2021-01-22 | 深圳市博纯半导体材料有限公司 | Xenon production and preparation device and method |
CN113702585A (en) * | 2021-08-26 | 2021-11-26 | 山东非金属材料研究所 | Automatic capturing and digesting device for trace metal elements in high-purity gas |
CN114377542A (en) * | 2021-12-22 | 2022-04-22 | 常州大学 | CO removing device and method mounted at outlet of high-purity oxygen steel cylinder |
CN116812885A (en) * | 2023-08-03 | 2023-09-29 | 衢州杭氧特种气体有限公司 | Xenon purification system and purification method thereof |
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JPH04149010A (en) * | 1990-10-15 | 1992-05-22 | Japan Pionics Co Ltd | Method for refining noble gas |
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CN113702585A (en) * | 2021-08-26 | 2021-11-26 | 山东非金属材料研究所 | Automatic capturing and digesting device for trace metal elements in high-purity gas |
CN114377542A (en) * | 2021-12-22 | 2022-04-22 | 常州大学 | CO removing device and method mounted at outlet of high-purity oxygen steel cylinder |
CN116812885A (en) * | 2023-08-03 | 2023-09-29 | 衢州杭氧特种气体有限公司 | Xenon purification system and purification method thereof |
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Application publication date: 20190614 |