FR2557810A1 - Noncontaminating process for removing the traces of impurities present in rare gases heated to a high temperature - Google Patents
Noncontaminating process for removing the traces of impurities present in rare gases heated to a high temperature Download PDFInfo
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- FR2557810A1 FR2557810A1 FR8400096A FR8400096A FR2557810A1 FR 2557810 A1 FR2557810 A1 FR 2557810A1 FR 8400096 A FR8400096 A FR 8400096A FR 8400096 A FR8400096 A FR 8400096A FR 2557810 A1 FR2557810 A1 FR 2557810A1
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- active element
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B23/00—Noble gases; Compounds thereof
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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
- Y02C20/20—Capture or disposal of greenhouse gases of methane
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Abstract
Description
ta présente Invention se rapporte à un procédé industriel pour éliminer les traces d impureté G2,N2,CH4,CO, C02, H2, H20. dans les gaz rares tels que Argon Xenon. Krypton. Hélium ou autre afin d'obtenir un gaz de pureté meilleur que 99.9999 % par l'emploi d'un dispositif adapté. The present invention relates to an industrial process for eliminating traces of impurity G2, N2, CH4, CO, C02, H2, H20. in rare gases such as Argon Xenon. Krypton. Helium or other in order to obtain a gas of purity better than 99.9999% by using a suitable device.
Sous forme de traces. on entend des impuretés dont la teneur corresau maximum à 50 PPMV. In the form of traces. impurities means a content corresponding to a maximum of 50 PPMV.
On sait épurer des gaz par des moyens reversible ou irréversible, chimique. catalyse. absortion. adsortion. sur des produits qui forment un composé chimique avec I impureté à éliminer ou qui la retiennent dans sa structure. Voir Brevets n0 1023498. 1128064. 1117002. We know how to purify gases by reversible or irreversible, chemical means. catalysis. absortion. adsorption. on products which form a chemical compound with impurity to be removed or which retain it in its structure. See Patents No. 1023498. 1128064. 1117002.
Ces procédés ont en général plusieurs défauts. Ils sont souvent selec tifs( exemple pour 02. H O Ils n éliminent pas l'azote et très difficile
2 ment les hydrocarbures. particulièrement le méthane. Ils nécessitent souvent 1 appoint d un gaz réducteur ou oxydant pour favoriser la catalyse.These methods generally have several shortcomings. They are often selective (example for 02. HO They do not remove nitrogen and very difficult
2 ment hydrocarbons. especially methane. They often require the addition of a reducing or oxidizing gas to promote catalysis.
le gaz épuré contient alors une quantité importante du gaz qui a servi à cette catalyse . Certains de ces procédés travaillent à haute température.the purified gas then contains a significant amount of the gas which was used for this catalysis. Some of these processes work at high temperatures.
L enveloppe comoortant le produit est aussi à haute. température, il est évident que d'une part l'air extérieur peut réagir avec cette envéloppe, ce qui en diminue sa durée de vie, d'autre part celle-ci devient poreuse et ì air ambiant diffuse dans le gaz à épurer et le polue. D'une manière générale, les contraintes i#mposées par l'utilisation de la haute température (isolement thermique. transfert de calorie. dilatation) ainsi que les risques de diffusion d impureté de l'atmosphère extérieur à travers les enveloppe portées à haute température contenant le produit actif font que de tels procédés sont difficiliment exploitable industriellement (Brevet 7635803). The envelope containing the product is also high. temperature, it is obvious that on the one hand the outside air can react with this envelope, which shortens its lifespan, on the other hand it becomes porous and the ambient air diffuses in the gas to be purified and the polite. In general, the constraints imposed by the use of high temperature (thermal insulation, calorie transfer, expansion) as well as the risks of impurity spreading from the outside atmosphere through the envelopes brought to high temperature. containing the active product make such processes difficult to use industrially (Patent 7635803).
Le procédé selon la présente invention ne pr4sente pas ces inconvénients. L élimination de 1'02. H20, N2, CO, C02, H2 CH4, C1 à C4. est simultanée. Il ne polue pas car il ne nécessite pas de gaz d'appointpour favoriser la réaction. Il est insensible à l'air extérieur (02. N2, H2 ) par l;emploi d'une technologie adaptée. Le rendement thermique est très bon.Le procédé est caractérisé par le fait que l'on fait passer le gaz à épurer dans un tube de titane, d alliage de titane ou d'inox contenant un mélange de Zirconium et de titane pastillé dont la composition est environ 65 % de Zirconium pour 35 O/G de titane et porté à une température comprise entre 400 à 8500c. Le tube de titane. d'alliage de titane ou d'inox joue aussi un rôle d!élément épurant. The method according to the present invention does not have these drawbacks. The elimination of 1'02. H20, N2, CO, C02, H2 CH4, C1 to C4. is simultaneous. It does not pollute because it does not require make-up gas to promote the reaction. It is insensitive to outside air (02. N2, H2) by the use of suitable technology. The thermal efficiency is very good. The process is characterized by the fact that the gas to be purified is passed through a tube of titanium, titanium alloy or stainless steel containing a mixture of zirconium and pelletized titanium, the composition of which is approximately 65% of Zirconium for 35 O / G of titanium and brought to a temperature between 400 to 8500c. The titanium tube. titanium alloy or stainless steel also plays a role!
Les figures ci-jointes donnent à titre d'exemple non limitatif deux possibilités de réalisation du procédé.The attached figures give by way of nonlimiting example two possibilities of carrying out the process.
La figure 1 représente un mode de réalisation où le gaz est préchauffé a ! extérieur dé l'enceinte. Il se compose d'un tube de titane 1 compor
ant le produit actif 11 et fermé par 2 frittés en inox 9 maintenus mécaniquement par deux manchons élastique 10. L'enceinte hermétique comporte deux tubulures 6 et 7 par lesquelles l'on peut soit faire passer un gaz autour du tube de titane, soit faire le vide. Deux traversées isolantes 3 dont 1 étanchéité sur l'enceinte 2 est obtenue à l'aide du joint torique 4 comportant deux passages electriques 3a et 3b. Le tube du titane est porté a haute température (environ 8000c) par passage d'un courant electrique intense dans son épaisseur.L'arrivée de ce courant se fait par l'intermédiaire de deux soudures 51 une bride de cuivre ou d'aluminium peut être utilisée, de cette manière le transfert de calorie entre le tube de titane et le produit actif sur lequel passe le gaz à épurer est optimum. Nous maintenons sous vide l'enceinte8/ la pompant en permanence aux environs de 10-4 Bar. Ce Procédé permet d'obtenir un très bon isolement thermique et d éviter toute pollution du gaz épuré par diffusion dans le tube cie;ti- tane.Figure 1 shows an embodiment where the gas is preheated a! outside the enclosure. It consists of a 1 compor titanium tube
ant the active product 11 and closed by 2 stainless steel frits 9 held mechanically by two elastic sleeves 10. The hermetic enclosure has two pipes 6 and 7 through which one can either pass a gas around the titanium tube, or make the void. Two insulating bushings 3 including 1 seal on the enclosure 2 is obtained using the O-ring 4 comprising two electrical passages 3a and 3b. The titanium tube is brought to high temperature (around 8000c) by the passage of an intense electric current in its thickness. The arrival of this current is done by means of two welds 51 a copper or aluminum flange can be used, in this way the transfer of calories between the titanium tube and the active product over which the gas to be purified passes is optimum. We keep the enclosure 8 vacuum / permanently pumping it around 10-4 Bar. This process makes it possible to obtain very good thermal insulation and to avoid any pollution of the purified gas by diffusion in the cie; titanium tube.
Un essai a été réalisé en faisant passer dans l'enceinte 8 le gaz non épuré. l'isolement thermique est moins bon. il depend de sa conductibilité thermique. mais le gaz sortant n'est pas polué. le gaz non épuré diffuse dans le tube 1 dans sa partie portée à haute température. tant de même nature que le gaz dans le tube 1 et ne comportant que des traces d'impuretes (quelques PPMV) il joue un rôle de séparateur entre l'air ambiant et le tube 1 évitant ainsi sa contamination. La pression du gaz à l'intérieur du tube 1 est sensiblement la même que dans l'enceinte 8. de cette manière
l'épaisseur du tube 1 est réduite au minimum même dans7fonctionnement à haute pression, de ce fait nous pouvons utiliser un tube à paroi mince ce qui est interessant pour son chauffage (resistance ohmique du tube plus resistance thermique longitudinale plus élevée donc moins de pertes de calories par les extrémités).A test was carried out by passing uncleaned gas through enclosure 8. the thermal insulation is less good. it depends on its thermal conductivity. but the outgoing gas is not polluted. the unpurified gas diffuses into the tube 1 in its part brought to high temperature. both of the same nature as the gas in tube 1 and comprising only traces of impurities (some PPMV) it plays a role of separator between the ambient air and the tube 1 thus avoiding its contamination. The pressure of the gas inside the tube 1 is substantially the same as in the enclosure 8. in this way
the thickness of the tube 1 is reduced to a minimum even in high pressure operation, therefore we can use a thin walled tube which is interesting for its heating (ohmic resistance of the tube plus higher longitudinal thermal resistance therefore less losses of calories from the extremities).
La figure 2 montre la mise en oeuvre de l'épurateur 13 précedement décrit. L'élément 12 est un serpentin de réchauffage dont la fonction est d'obtenir un gaz suffisament chaud à l'entrée de l'élément actif. Si ce serpentin n'existait pas le gaz entrant devrait se réchauffer le long de l épurateur 13. Il éxisterait un gradiant de température
entre l'entrée et la sortie. Le gaz entrant froid aux environs de 20
à 250c devrait se réchauffer le long de ce tube, celui-ci devrait donc
être plus long. Une partie de l'élément actif ne serait plus à sa température optimum de réaction, c'est-à-dire aux environs de 800- c. Le volume de produit actif de part le surdimensionement du tube serait plus grand. le coût de l'appareil serait Dlus élevé. Figure 2 shows the implementation of the purifier 13 previously described. The element 12 is a heating coil whose function is to obtain a sufficiently hot gas at the inlet of the active element. If this coil did not exist the incoming gas should heat up along the purifier 13. There would be a temperature gradient
between entry and exit. Gas entering cold around 20
to 250c should heat up along this tube, so this one should
be longer. Part of the active element would no longer be at its optimum reaction temperature, that is to say around 800 ° C. The volume of active product due to the oversizing of the tube would be greater. the cost of the device would be higher.
L élément 14 est un serpentin de refroidissement afin d'obtenir une
température de gaz sortant inférieur à 500c.Element 14 is a cooling coil in order to obtain a
leaving gas temperature below 500c.
La figure 3 représente un autre mode de réalisation : il utilise un tuS3 de titane ou d alliage de titane 17 fermé à une extrémité par laquel
le arrive le courant de chauffage du tube 17 par l'intermédiaire de la traversée de la cloison 22 et de son conducteur 22a. Le tube 17 contient
le produit actif qui est maintenu à l'aide du disque frité 19 et du manchon élastique 18, le tube 17 est soudé sur la bride 21 par laquelle arrive ì autre conducteur electrique pour le chauffage du tube.FIG. 3 represents another embodiment: it uses a tuS3 of titanium or of titanium alloy 17 closed at one end by which
the heating current from the tube 17 arrives via the passage through the partition 22 and its conductor 22a. Tube 17 contains
the active product which is maintained by means of the fried disc 19 and the elastic sleeve 18, the tube 17 is welded to the flange 21 through which arrives another electrical conductor for heating the tube.
Un serpentin 16 est enroulé sur le tube 17. Ce tuoe est porté à haute température par un courant electrique circulant dans son épaisseur envi ron 850cc. il cnauffe è la fois le produit actif par l'intérieur et le serpentin par I extérieur} le gaz est ainsi préchauffé, l'appareil est plus compact et son rendement est amélioré; comme dans le cas précédent I enceint~ hermétique 21a peut être balayée ou mise sous vide par l'inter médiaire destubulures 15. A coil 16 is wound on the tube 17. This tuoe is brought to high temperature by an electric current circulating in its thickness around 850cc. it cnauffe both active product from the inside and the coil from I outside} the gas is thus preheated, the device is more compact and its performance is improved; as in the previous case I pregnant ~ hermetic 21a can be scanned or put under vacuum by the intermediary of tubes 15.
L'extrémité du tube de titane 17 est libre e oui lui nermet de se dilater sans contraintes Des tubes de grande longueur peuvent ainsi être utilisé~
L ensemble serpentin, tube de titane, produit actif peut être démonté de l enceinte 21a en enlevant la bride 21. L étanchéité est obtenue à
aide de joint torique 23. cette bride sert de schunt thermique ce qui permet d avoir une température acceptable à l'extérieur de l'appareil
(environ 2000c). L-arrivée du gaz à épurer se fait par la canalisation 20.The end of the titanium tube 17 is free e yes it nermet to expand without constraints Long tubes can thus be used ~
The coil assembly, titanium tube, active product can be removed from the enclosure 21a by removing the flange 21. The seal is obtained at
using O-ring 23. this flange serves as a thermal schunt which allows to have an acceptable temperature outside the device
(around 2000c). The gas to be purified arrives via line 20.
Nos essais ont porté sur un gaz tel que l Argon comportant 30 ppm V d impuretés tel que 02. N2. Cq CO. CO2. H20. H2. La teneur de sortie du az épuré est inférieure à 1 ppm u pour la somme des concentrations 02 +
N2 +CH4 + CO + C02 + H20 + H2.Our tests focused on a gas such as Argon comprising 30 ppm V of impurities such as 02. N2. Cq CO. CO2. H20. H2. The output content of the purified az is less than 1 ppm u for the sum of the concentrations 02 +
N2 + CH4 + CO + C02 + H20 + H2.
Un tube de titane de diamètre 100 mm et de longueur 1000 mm rempli d un alliage ZR - TI permet d'épurer au minimum 3000 m3 de gaz. A titanium tube with a diameter of 100 mm and a length of 1000 mm filled with a ZR - TI alloy makes it possible to purify at least 3000 m3 of gas.
Claims (13)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR8400096A FR2557810A1 (en) | 1984-01-05 | 1984-01-05 | Noncontaminating process for removing the traces of impurities present in rare gases heated to a high temperature |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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FR8400096A FR2557810A1 (en) | 1984-01-05 | 1984-01-05 | Noncontaminating process for removing the traces of impurities present in rare gases heated to a high temperature |
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FR2557810A1 true FR2557810A1 (en) | 1985-07-12 |
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FR8400096A Withdrawn FR2557810A1 (en) | 1984-01-05 | 1984-01-05 | Noncontaminating process for removing the traces of impurities present in rare gases heated to a high temperature |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2584063A1 (en) * | 1985-06-28 | 1987-01-02 | Taiyo Sanso Co Ltd | SUPER PURIFIER FOR ARGON GAS AND PROCESS FOR THE PURIFICATION OF ARGON. |
US4983194A (en) * | 1990-02-02 | 1991-01-08 | Air Products And Chemicals, Inc. | Production of high purity argon |
US5489327A (en) * | 1994-03-04 | 1996-02-06 | Japan Pionics Co., Ltd. | Process for purifying hydrogen gas |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB805516A (en) * | 1957-02-08 | 1958-12-10 | Standard Telephones Cables Ltd | Improvements in or relating to the purification of gases |
FR1539693A (en) * | 1966-06-07 | 1968-09-20 | Japan Pure Hydrogen Company Lt | Process for removing impurities from noble gases |
FR2161347A5 (en) * | 1971-11-23 | 1973-07-06 | Ugine Kuhlmann | Gas purification - using zirconium - titanium alloy sintered without compression |
-
1984
- 1984-01-05 FR FR8400096A patent/FR2557810A1/en not_active Withdrawn
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB805516A (en) * | 1957-02-08 | 1958-12-10 | Standard Telephones Cables Ltd | Improvements in or relating to the purification of gases |
FR1539693A (en) * | 1966-06-07 | 1968-09-20 | Japan Pure Hydrogen Company Lt | Process for removing impurities from noble gases |
FR2161347A5 (en) * | 1971-11-23 | 1973-07-06 | Ugine Kuhlmann | Gas purification - using zirconium - titanium alloy sintered without compression |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2584063A1 (en) * | 1985-06-28 | 1987-01-02 | Taiyo Sanso Co Ltd | SUPER PURIFIER FOR ARGON GAS AND PROCESS FOR THE PURIFICATION OF ARGON. |
US4983194A (en) * | 1990-02-02 | 1991-01-08 | Air Products And Chemicals, Inc. | Production of high purity argon |
US5489327A (en) * | 1994-03-04 | 1996-02-06 | Japan Pionics Co., Ltd. | Process for purifying hydrogen gas |
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