EP0082061A2 - Verfahren und Vorrichtung zur Aufarbeitung von tritiumoxydhaltigen Lösungen, dafür verwendbare Elektrode und ihr Herstellungsverfahren - Google Patents

Verfahren und Vorrichtung zur Aufarbeitung von tritiumoxydhaltigen Lösungen, dafür verwendbare Elektrode und ihr Herstellungsverfahren Download PDF

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Publication number
EP0082061A2
EP0082061A2 EP82402226A EP82402226A EP0082061A2 EP 0082061 A2 EP0082061 A2 EP 0082061A2 EP 82402226 A EP82402226 A EP 82402226A EP 82402226 A EP82402226 A EP 82402226A EP 0082061 A2 EP0082061 A2 EP 0082061A2
Authority
EP
European Patent Office
Prior art keywords
tritium
cathode
solution
palladium
electrolysis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP82402226A
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English (en)
French (fr)
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EP0082061A3 (en
EP0082061B1 (de
Inventor
Gilbert Bellanger
Pierre Giroux
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Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
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Commissariat a lEnergie Atomique CEA
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Publication date
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Publication of EP0082061A2 publication Critical patent/EP0082061A2/de
Publication of EP0082061A3 publication Critical patent/EP0082061A3/fr
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Publication of EP0082061B1 publication Critical patent/EP0082061B1/de
Expired legal-status Critical Current

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    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04—Treating liquids
    • G21F9/06—Processing

Definitions

  • the subject of the present invention is a method and a device for the treatment by electrolysis of solutions containing tritiated water such as effluents from plants for reprocessing irradiated nuclear fuels, water for cooling light water or water reactors. heavy and effluents from laboratories where tritium is handled.
  • solutions containing tritiated water such as effluents from plants for reprocessing irradiated nuclear fuels, water for cooling light water or water reactors. heavy and effluents from laboratories where tritium is handled.
  • aqueous solutions containing a large quantity of tritiated water for example a content of approximately 40 Ci / m 3 , are obtained at certain stages of reprocessing. These solutions are generally obtained during the concentration by evaporation of uranium, plutonium or fission product solutions, or during the regeneration treatment of nitric acid with a view to its recycling at the dissolving stage of irradiated fuel elements. . In the latter case, these solutions are obtained during the concentration of the nitric acid which has been formed by regenerating by means of water vapor the nitrogen oxides originating from the step of destruction of the nitric acid by the formalin. It is also possible to envisage higher concentrations, either by recycling the nitric solutions, or by isotopic concentration of the effluents.
  • the present invention specifically relates to a process for treating solutions containing tritiated water which makes it possible to solve this problem of the recovery of tritium under satisfactory conditions.
  • the cathode coated with porous palladium black thanks to the structure and the nature of the cathode coated with porous palladium black, it is possible to recover directly in the gaseous state, with good yields, the tritium released during the electrolysis, after its diffusion through the electrode wall and its desorption on the other side of the electrode.
  • the choice of a cathode of non-porous material, permeable to hydrogen and impermeable to other gases makes it possible to obtain, after release of the tritium at the cathode, an adsorption of the tritium by the cathode, then a diffusion of this in the cathode and its desorption on the other side of the cathode in the receiving compartment.
  • a slight depression is established in the receiving compartment, for example when the tritium is collected by pumping.
  • the first step constitutes the most important step because it determines the quantity of tritium which can be adsorbed then diffused by the wall of the cathode in contact with the electrolyte.
  • a cathode coated on its surface is used in contact with the solution to be electrolyzed from a deposit of porous palladium black.
  • this deposit makes it possible to increase the specific surface of the cathode and to give it a higher adsorption capacity with respect to tritium.
  • a second deposit on the desorption side is also favorable but in lesser proportions.
  • tritium can also be recovered in the form of solid metal tritiide by reacting it directly in the reception compartment with a compound capable of forming a metal tritiide. Mention may be made, as compounds capable of being used, of La-Ni c compounds, Fe-Ti compounds and palladium, alloyed or not.
  • a cathode covered with porous palladium black is used on its adsorption face and, preferably, also on its desorption face. Furthermore, the presence of traces of ferric oxide on the adsorption face of the cathode is favorable and the use of annealing to restore the cathode also makes it possible to improve the results obtained.
  • the cathode is advantageously made of palladium or a palladium alloy such as a palladium-silver alloy because these metals have the property of adsorbing very large quantities of tritium.
  • a palladium alloy such as a palladium-silver alloy
  • an alloy of palladium and silver with 25% silver is used because it has a permeability substantially equal to that of pure palladium and the property of not deteriorating after repeated cycles of heating and hydrogenation.
  • metals capable of adsorbing tritium can be used, for example, pure iron, nickel, platinum and their alloys.
  • T tritium
  • the secondary reactions to avoid are: because in this case, the tritium would be discharged directly into the electrolysis cell, instead of diffusing through the wall of the electrode.
  • the adsorption of tritium by palladium is improved by subjecting the palladium or palladium alloy electrode to an activation treatment comprising a step of coating the surface of the electrode which will be in contact with the solution to be electrolyzed, a layer of finely divided and porous palladium black.
  • This activation treatment can be carried out in the following manner: - the electrode is first subjected to an annealing heat treatment, then it is carried out on the surface of the electrode intended to be in contact with the solution to be electrolyzed a mechanical abrasion treatment using wet ferric oxide, the traces of which remain on the cathode act as an accelerator for the hydrogenation of palladium, and the surface thus treated is then coated with finely divided and porous palladium black.
  • the porous palladium black coating is formed by electrolysis of a solution of palladium chloride in dilute hydrochloric acid.
  • This electrolysis can be carried out at a current density of 150 mA / cm 2 for 4 min.
  • a deposit of palladium black with a thickness of 6 ⁇ m is obtained.
  • the annealing heat treatment makes it possible to increase the size of the meshes of the metal network of the cathode and thus to improve the diffusion of the tritium in the cathode.
  • the palladium electrodes are generally obtained by rolling and are therefore strongly hardened.
  • the grains appear little and are oriented in the direction of rolling.
  • recrystallization annealing is possible since the germs necessary for the growth of the crystals have been produced by work hardening, the most disturbed regions where the dislocation energy is concentrated playing the role of germs.
  • the metal is heated to a suitable temperature, the germs start to grow and the grain gets bigger; after a certain heating time which corresponds to the incubation period, the recrystallization actually begins.
  • time and temperature play an important role and temperature intervenes in a rather complex way.
  • the temperature is not high enough during the incubation period, the number of germs decreases and recrystallization can be suppressed, which corresponds to the phenomenon of restoration.
  • palladium electrodes good results are obtained by annealing at a temperature of around 650 ° C. for one hour under vacuum.
  • the hardness decreases, the mechanical tensions are reduced and the dislocations or other imperfections of the metallic network can move towards the surface of the electrode, from where a better diffusion of the tritium in the metallic network of palladium.
  • the mechanical abrasion treatment using ferric oxide as a hydrogenation accelerator makes it possible to modify the energy required to pass the chemisorbed hydrogen into hydrogen absorbed in the interstitial sites directly below the cathode surface.
  • Iron occupies a number of sites by lending electrons to the 4d band of palladium. This model of iron adsorption which covers the cathode surface increases the permeability of hydrogen in palladium with decrease in potential and increase in current.
  • This treatment acts on the amount of tritium released over time.
  • the deposition of a thin layer of finely divided and porous palladium black on the surface of the cathode in contact with the solution to be electrolyzed makes it possible to improve the adsorption and the diffusion of tritium.
  • the existence on the surface of a very finely divided deposit of palladium black promotes and multiplies the reactions which occur at the solid-solution interface to be electrolyzed.
  • a deposit of palladium black on the desorption face improves the diffusion.
  • the electrolyte added to the solution containing the tritiated water preferably consists of an alkali metal hydroxide such as sodium hydroxide or potassium hydroxide, which makes it possible to avoid as much as possible the formation of complex ions resulting from radiolysis phenomena and the presence of solvated electrons due to tritium.
  • an alkali metal hydroxide such as sodium hydroxide or potassium hydroxide
  • the electrolyte concentration of this solution is advantageously from 1 mol.l to 20 mol.l -1 .
  • electrolysis is carried out at a temperature higher than ambient temperature, for example at a temperature of 50 to 160 ° C. because, it is thus possible to increase the current density and cell yield without bubbles forming on the cathode.
  • the operation is carried out at a temperature of 80 ° C. since this avoids the technological constraints due to the use of high temperatures as well as the appearance of unfavorable phenomena such as corrosion or secondary reactions of radiolysis.
  • the cathode when the cathode is constituted by a wall of palladium or palladium alloy having a thickness of 50 to 250, tm, electrolysis is carried out with a current density between 60 and 150 milliamperes / cm 2 , at a temperature of 80 ° C.
  • the cathode is constituted by a hollow tube closed at one of its ends and arranged in the cell so as to be partially immersed in the electrolytic solution, the space defined at the interior of the tube constituting the tritium receiving compartment.
  • the device comprises means for extracting hydrogen and / or isotopes of hydrogen in the gaseous state, which have diffused in said receiving compartment, these means being constituted either by a suitable pump, or by a trap. based on metals and alloys such as LaNi . , Fe-fii, palladium alloyed or not forming hydrides.
  • the device preferably comprises means for heating the electrolytic solution present in said cell.
  • the cathode is preferably made of palladium or a palladium alloy, for example a palladium and silver alloy.
  • a palladium alloy for example a palladium and silver alloy.
  • this tube is covered externally and possibly internally with porous palladium black.
  • the anode is advantageously constituted by the wall of the electrolysis cell and it is made of stainless steel.
  • the palladium-silver alloy tube which constitutes the cathode is subjected to an annealing heat treatment, then its external surface is treated by mechanical abrasion using ferric oxide before being coated with palladium black by electrolysis. .
  • the device comprises an electrolysis cell 1 made, for example, of ceramic which is not soluble in an alkaline medium, of metal or of a non-corrodable metal alloy such as 316L 22 CND 17-13 steel. Preferably, it is made of passive stainless steel.
  • the cell 1 is closed in leaktight manner at its upper part by a cover 3. Inside the cell is disposed a cathode 5 constituted by a tube closed at its lower end, and the wall of the cell constitutes the anode 7 .
  • the device comprises a condenser 15 and an electrolytic solution supply line 17 provided with a valve 18 controlled by an electrical relay associated with the probes 11 and 13, as well as a line 19 for introducing a inert gas. Furthermore, the device comprises heating means 21 of the electrolysis cell constituted by electrical resistances controlled from a thermostat which ensures thermal regulation.
  • the cathode 5 is constituted by a hollow tube 5a of circular section having a thickness of 50 to 250 ⁇ m closed at its lower end which delimits the compartment 23 for receiving tritium connected at its upper part to a device for recovery of tritium.
  • This tritium recovery device must be sealed to maintain the high purity of the diffused tritium and it can be maintained under vacuum by means of a primary vane pump.
  • this device comprises a vacuum gauge and a pressure gauge to control the vacuum, an intermediate enclosure for storing tritium, a test tube for taking gaseous samples and a trap used for storing tritium in the form of tritiide.
  • the vacuum can be obtained through a pumping group.
  • the tube constituting the cathode 5 is made of a non-porous palladium-silver alloy, permeable to hydrogen and impermeable to other gases, and it has been annealed at a temperature of 650 ° C. for one hour under a vacuum of order of 1.35 Pa to remove the orientation of the grains due to rolling.
  • the external surface of the tube intended to be in contact with the solution to be electrolysed has undergone a mechanical abrasion treatment using a ferric oxide powder Fe 2 0 3 moistened with water, for a few minutes, as a palladium hydrogenation accelerator, then a layer of finely divided and porous palladium black with a thickness of 7 ⁇ m was deposited on this surface thus treated, in order to increase the active surface of palladium on contact electrically discharged tritium.
  • This deposit of finely divided and porous palladium black was produced by electrolysis of a solution of palladium chloride containing 4 g of PdCl 2 dissolved in 20 cm 3 of 12 mol / l HCl, then diluted to 500 cm 3 with distilled water, operating at a cathode current density of 150 mA / cm 2 at a temperature of 20 ° C, for 4 min.
  • the anode 7 is formed by the wall of the cell 1 and it is connected to the positive pole of the electric current generator.
  • Such an arrangement of the anode and the cathode makes it possible to obtain a good distribution of the current over the surface of the cathode and the formation of regular equipotentials.
  • the electrolysis current is programmed using a potentiostat operating in intensiostatic mode.
  • solutions containing tritiated water can be treated in the following manner te: the solution to be electrolyzed which is constituted by tritiated water containing from 1 to 20 mol.l -1 of sodium hydroxide is put into circulation in cell 1, via line 17.
  • This tritiated water was obtained by catalytic oxidation of gaseous effluents containing tritium.
  • the introduction of solution stops automatically.
  • the heating device is then switched on to bring the temperature of the solution to around 80 ° C.
  • argon is introduced via line 19 and the electrodes 5 and 7 are connected to the electric current generator to electrolyze the solution with a cathodic current density of 60 mA.cm 2 and obtain a release of gaseous tritium on the cathode 5.
  • the tritium is adsorbed by the cathode 5, then it diffuses inside the tube 5 normally under vacuum by pumping, but the This process can work when the pressure of the gases inside the tube is much higher than the pressure of the electrolysis cell. Under these conditions, it is possible to obtain a tritium flow rate of the order of 1 cm.min *.
  • the gases released during electrolysis i.e.
  • oxygen as well as the tritium which has not diffused in the tube 5 and the water vapor, are evacuated from the cell by the current d argon to the condenser 15 in which the water vapor is condensed and then recycled inside the cell 1.
  • the gases leaving the condenser will be sent in a catalytic recombination assembly to reform tritiated water which can then be recycled inside the cell.
  • the gas evacuation pipe leaving the condenser 15 can lead into an element for the catalytic oxidation of residual tritium, this element consisting of fixed palladium black. on alumina.
  • the tritium recombined with oxygen in the form of heavy water is then condensed in a heat exchanger and optionally recycled in cell 1. It is possible to connect a sampling bulb to the gas outlet pipe so as to analyze the gases extracted. , either at the outlet of the electrolysis cell, or after the catalytic oxidation element.
  • a device of this type has made it possible to obtain satisfactory results after operating periods of approximately six weeks without any disassembly of the cathode. At the end of this time, the latter showed no failure and the diffusion of tritium through its wall was carried out under good conditions.
  • the method and the device of the invention make it possible to solve the safety problems posed by the handling of tritiated water, the rejection of contaminated effluents, in particular as regards the hydrogen-tritium fraction released in the electrolysis tank. , as well as the problems of resistance of materials to tritiated water, radiolysis of tritiated water and interaction with the nitrogen in the air which leads to corrosive compounds.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
EP82402226A 1981-12-09 1982-12-06 Verfahren und Vorrichtung zur Aufarbeitung von tritiumoxydhaltigen Lösungen, dafür verwendbare Elektrode und ihr Herstellungsverfahren Expired EP0082061B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8123033A FR2517663B1 (fr) 1981-12-09 1981-12-09 Procede et dispositif de traitement d'effluents aqueux contenant de l'eau tritiee, electrode utilisable dans un tel dispositif et son procede de preparation
FR8123033 1981-12-09

Publications (3)

Publication Number Publication Date
EP0082061A2 true EP0082061A2 (de) 1983-06-22
EP0082061A3 EP0082061A3 (en) 1983-07-20
EP0082061B1 EP0082061B1 (de) 1988-06-29

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EP82402226A Expired EP0082061B1 (de) 1981-12-09 1982-12-06 Verfahren und Vorrichtung zur Aufarbeitung von tritiumoxydhaltigen Lösungen, dafür verwendbare Elektrode und ihr Herstellungsverfahren

Country Status (6)

Country Link
US (1) US4487670A (de)
EP (1) EP0082061B1 (de)
JP (1) JPS58113797A (de)
CA (1) CA1215020A (de)
DE (1) DE3278714D1 (de)
FR (1) FR2517663B1 (de)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0202699A1 (de) * 1985-04-25 1986-11-26 "Studiecentrum voor Kernenergie", "S.C.K." Elektrolyseur für hochaktiv tritiumhaltiges Wasser
DE3828279A1 (de) * 1987-08-21 1989-03-02 Doryokuro Kakunenryo Elektrolytische behandlung von radioaktivem fluessigen abfall
FR2690270A1 (fr) * 1992-04-21 1993-10-22 Framatome Sa Enceinte de séparation et de confinement de produits radioactifs contenus dans des effluents liquides et installation et procédé pour le traitement de ces effluents.

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DE3606316A1 (de) * 1986-02-27 1987-09-03 Kernforschungsz Karlsruhe Verfahren und vorrichtung zur dekontamination des abgases des brennstoffkreislaufs eines fusionsreaktors von tritium und/oder deuterium in chemisch gebundener form enthaltenden abgas-bestandteilen
WO1992022906A1 (en) * 1991-06-11 1992-12-23 Electric Power Research Institute, Inc. Methods for cleaning cathodes
AU2257392A (en) * 1991-06-11 1993-01-12 Electric Power Research Institute, Inc. Methods for forming films on cathodes
AU2336192A (en) * 1991-06-11 1993-01-12 Electric Power Research Institute, Inc. Apparatus for producing heat from deuterated palladium
US20020090047A1 (en) * 1991-10-25 2002-07-11 Roger Stringham Apparatus for producing ecologically clean energy
AU5738894A (en) * 1992-12-10 1994-07-04 Electric Power Research Institute, Inc. Methods for forming films on cathodes
EP0914668A2 (de) * 1995-06-06 1999-05-12 André Jouanneau Verfahren und vorrichtung zur erzeugung und verwendung eines plasmas
US6024935A (en) * 1996-01-26 2000-02-15 Blacklight Power, Inc. Lower-energy hydrogen methods and structures
IL134131A (en) * 1997-07-22 2005-08-31 Black Light Power Inc Inorganic hydrogen compounds, separation methods and fuel applications
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US20090129992A1 (en) * 1997-07-22 2009-05-21 Blacklight Power, Inc. Reactor for Preparing Hydrogen Compounds
CA2466953A1 (en) * 2001-11-14 2003-08-14 Blacklight Power, Inc. Hydrogen power, plasma, and reactor for lasing, and power conversion
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US20030129117A1 (en) * 2002-01-02 2003-07-10 Mills Randell L. Synthesis and characterization of a highly stable amorphous silicon hydride as the product of a catalytic hydrogen plasma reaction
US20040118348A1 (en) * 2002-03-07 2004-06-24 Mills Randell L.. Microwave power cell, chemical reactor, and power converter
CA2483780A1 (en) * 2002-05-01 2003-11-13 Blacklight Power, Inc. Diamond synthesis
EP1628909A2 (de) * 2003-04-15 2006-03-01 Blacklight Power, Inc. Plasmareaktor und verfahren zur herstellung von niederenergetischen wasserstoffspezies
US7188033B2 (en) * 2003-07-21 2007-03-06 Blacklight Power Incorporated Method and system of computing and rendering the nature of the chemical bond of hydrogen-type molecules and molecular ions
AU2004307452A1 (en) 2003-10-24 2005-05-06 Blacklight Power, Inc. Novel molecular hydrogen gas laser
EP1702212A4 (de) * 2004-01-05 2009-01-21 Blacklight Power Inc Verfahren und system zur berechnung und darstellung der beschaffenheit von atomen und atomionen
US20060088138A1 (en) * 2004-04-07 2006-04-27 Andre Jouanneau Method and apparatus for the generation and the utilization of plasma solid
US7689367B2 (en) 2004-05-17 2010-03-30 Blacklight Power, Inc. Method and system of computing and rendering the nature of the excited electronic states of atoms and atomic ions
US20070198199A1 (en) * 2004-07-19 2007-08-23 Mills Randell L Method and system of computing and rendering the nature of the chemical bond of hydrogen-type molecules and molecular ions
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US8597471B2 (en) 2010-08-19 2013-12-03 Industrial Idea Partners, Inc. Heat driven concentrator with alternate condensers
JP6549372B2 (ja) * 2014-12-16 2019-07-24 吉田　英夫 トリチウム水による汚染土壌および汚染水の除染方法および除染システム
US10385468B2 (en) 2016-06-06 2019-08-20 Ih Ip Holdings Limited Plasma frequency trigger
US11268202B2 (en) 2019-02-13 2022-03-08 Industrial Heat, Llc Methods for enhanced electrolytic loading of hydrogen
US10767273B2 (en) * 2019-02-13 2020-09-08 Ih Ip Holdings Limited Methods for enhanced electrolytic loading of hydrogen
CN112489847B (zh) * 2020-12-01 2023-05-05 中国工程物理研究院核物理与化学研究所 一种活化石墨减容处理方法
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0202699A1 (de) * 1985-04-25 1986-11-26 "Studiecentrum voor Kernenergie", "S.C.K." Elektrolyseur für hochaktiv tritiumhaltiges Wasser
DE3828279A1 (de) * 1987-08-21 1989-03-02 Doryokuro Kakunenryo Elektrolytische behandlung von radioaktivem fluessigen abfall
FR2690270A1 (fr) * 1992-04-21 1993-10-22 Framatome Sa Enceinte de séparation et de confinement de produits radioactifs contenus dans des effluents liquides et installation et procédé pour le traitement de ces effluents.
EP0568408A1 (de) * 1992-04-21 1993-11-03 Framatome Trennungs- und Verschlussraum für in flüssigen Abfällen enthaltender radioaktiver Substanzen, sowie Vorrichtung und Verfahren für deren Behandlung

Also Published As

Publication number Publication date
JPH0129439B2 (de) 1989-06-09
FR2517663A1 (fr) 1983-06-10
EP0082061A3 (en) 1983-07-20
DE3278714D1 (en) 1988-08-04
CA1215020A (en) 1986-12-09
US4487670A (en) 1984-12-11
JPS58113797A (ja) 1983-07-06
FR2517663B1 (fr) 1985-08-09
EP0082061B1 (de) 1988-06-29

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