EP0084521B1 - Cellule électrolytique pour la récupération de métaux et son fonctionnement - Google Patents

Cellule électrolytique pour la récupération de métaux et son fonctionnement Download PDF

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Publication number
EP0084521B1
EP0084521B1 EP83810013A EP83810013A EP0084521B1 EP 0084521 B1 EP0084521 B1 EP 0084521B1 EP 83810013 A EP83810013 A EP 83810013A EP 83810013 A EP83810013 A EP 83810013A EP 0084521 B1 EP0084521 B1 EP 0084521B1
Authority
EP
European Patent Office
Prior art keywords
cathode
cutter blade
metal
cell
shaft member
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.)
Expired
Application number
EP83810013A
Other languages
German (de)
English (en)
Other versions
EP0084521A2 (fr
EP0084521A3 (en
Inventor
Colin Charles Blake
Charles Clifford Owen Goodall
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Novartis AG
Original Assignee
Ciba Geigy AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Ciba Geigy AG filed Critical Ciba Geigy AG
Publication of EP0084521A2 publication Critical patent/EP0084521A2/fr
Publication of EP0084521A3 publication Critical patent/EP0084521A3/de
Application granted granted Critical
Publication of EP0084521B1 publication Critical patent/EP0084521B1/fr
Expired legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/06—Operating or servicing
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/06—Operating or servicing
    • C25C7/08—Separating of deposited metals from the cathode

Definitions

  • the invention relates to an electrolytic metal recovery cell with a housing provided with an inlet and outlet for a solution containing the metal to be recovered, in which an anode, a cylindrical cathode rotatably mounted in the housing and a cutting knife are accommodated, the cutting knife operating the cell from the whole Removed metal deposited on the cathode surface in powder form, and a method for controlling the operation of such a metal recovery cell, in which a rotating cylindrical cathode is brought into contact with a solution containing ions of the metal to be recovered under conditions such that the metal is deposited on the rotating cathode in powder form and wherein the deposited metal is removed from the cathode by means of a cutting knife.
  • a method of using a rotating cylindrical cathode electrolytic cell in such a manner that the metal is deposited on the rotating cylindrical cathode in powder form is described in GB-PS 1 505 736.
  • the cell comprises a cylindrical cathode which is rotatably supported in a housing which has an inlet and an outlet for the solution from which metal is to be recovered, and an anode and a device for removing metal deposited on the cathode in powder form.
  • the cell described in this GB-PS has been used in practice in particular for the recovery of silver from used photographic processing solutions. If the cell is used in the manner described in GB-PS, silver accumulates as a powdery precipitate on the rotating cathode and is removed by a scraper which is in engagement with the cathode during its rotation.
  • a scraper which is in engagement with the cathode during its rotation.
  • the method of removing the powdered metal precipitate from the rotating cathode by means of a scraper is not particularly effective, and in fact the use of the scraper has some drawbacks, in particular excessive use of the scraper bearing when metal is heavily deposited on the rotating cathode.
  • Priority EP-A-58 537 describes an electrolytic metal recovery cell with a housing provided with inlet and outlet for a solution containing the metal to be recovered, in which an anode, a cylindrical cathode rotatably mounted in the housing and a cutting knife are accommodated, the Cutting knife at Operation of the cell removed metal deposited from the entire cathode surface in powder form.
  • This cell is intended for the recovery of copper, the removal of the copper powder from the cathode surface being carried out continuously. This cell has no monitoring of the cathode potential and no activation of the cutting knife controlled afterwards.
  • the invention is intended to find a way out of the contradictory requirements set out above and to improve an electrolytic metal recovery cell of the type in question in such a way that the deposition of the metal in powder form is possible under stable operating conditions. H. especially also in cases of possible fluctuations in the metal ion concentration or other changes in the conditions of the electrolysis.
  • the electrolytic metal recovery cell according to the invention is characterized in that electrical means are provided which put the cutting knife into operation in predetermined time periods and whenever the cathode potential deviates by a predetermined amount from a potential value which characterizes the target conditions for the operation of the cell.
  • the method according to the invention for operating the cell is characterized in that the cathode potential is monitored with respect to a reference electrode, and in that the cutting knife is put into operation at preselected time intervals which preclude reaching a preselected maximum current and also when the monitored cathode potential is increased by a predetermined amount deviates from a potential value characterizing the target conditions for the operation of the cell.
  • the use of a cutting instead of a scraping action prevents the gradual build-up of thicker metal deposits on the rotating cathode, as could be done by sliding the scraper away over harder or more adherent deposits.
  • the commissioning of the cutting knife during predetermined periods should normally suffice to control the current, provided that the periods are selected depending on the parameters of the cell.
  • the cell is continuously monitored by checking the cathode potential and generating an imposed signal when the controlled potential deviates from a desired value.
  • an electrolytic metal recovery cell which comprises a cylindrical, cup-shaped housing part 1, which is liquid-tightly closed by a cover 2, so that both parts represent an outer housing of the cell, which is preferably made of plastic such.
  • B. is made of polyvinyl chloride.
  • the bottom of the housing part 1 is provided with a passage opening 3, into which an inlet connection 4 is inserted, while the cover 2 also has a passage opening 5 with an outlet connection 6 inserted into it.
  • a largely annular, cylindrical graphite anode 7 is fastened coaxially to the inner wall surface of the housing part 1 and has an axial gap 8, so that the anode in cross section comes close to the shape of a horseshoe.
  • a cylindrical cathode 9 is rotatably mounted in the cell housing and comprises a hollow cylinder 10 made of stainless steel, which is closed at its ends with plastic caps 11, which fit snugly into the cylinder, but have outwardly projecting flanges 12, the diameter of which is slightly larger than that of the cylinder.
  • the cathode is mounted on a drive shaft 14 which is carried in bearings 15 mounted on the cover 2 and which is driven by drive means (not shown) located outside the cell via a pulley 16.
  • the drive shaft 14 is sealed against the interior of the cell housing part 1 by surface seals 17.
  • the anode 7 and the cathode 9 are connected to a fixed voltage source via electrical lines indicated at 18 and 19 in FIG. 1, as will be described below in connection with FIG. 3.
  • a rotatable cutting knife carrier shaft 20 extends axially parallel with the drive shaft 14 and the cathode 9 through the cover 2 and lies essentially centrally in the anode gap 8.
  • the shaft 20 carries a cylindrical cutting knife holder 21, on which a cutting knife 22 is attached.
  • the shaft 20 and the holder 21 are preferably made of stainless steel and the cutting knife of stellite steel.
  • the cutting knife has a triangular cross section and extends helically along the cutting knife holder. For reasons to be explained further below, this screw line does not extend completely around the circumference of the Cutting knife holder around, but rather only around a part of this circumference, preferably corresponding to an angle of about 120 to 180 °.
  • the shaft 20 is rotated by means of a drive means 23 in the form of an electric cutting knife drive motor under the control of a timer 24 and is provided with a cam 25 which actuates a microswitch 26 arranged in a line 27 leading from the anode line 18 to the shaft 20, whereby at the beginning of the rotation of the shaft 20 of the cams 25, the microswitch 26 switches to the shaft 20 and thus to the cutting knife 22 by applying an anode current pulse.
  • the probe 28 of a saturated calomel electrode is passed through an opening in the side wall of the housing part 1 and an opening aligned with this opening in the anode 7 and is sealed therein by means of a seal 29.
  • the end of the probe is set at a certain distance from the cathode cylinder 10.
  • the cell voltage or the electrode potential is controlled in a known manner by a potentiostat using a calomel electrode as the reference electrode.
  • Fig. 3 shows the circuit diagram of an electrical arrangement for the purpose of such control of the cell.
  • the electrolytic recovery cell E is shown in dashed outline in the middle of the figure and comprises the anode 7, the cathode 9 and the cutting knife 22.
  • the anode and the cathode are connected to a stabilized current source SPS via electrical lines.
  • a millivolt meter MV indicates a signal which indicates the potential difference between the potential of the calomel electrode determined by the probe 28 and the potential generated at the cathode 9.
  • the potential difference is also passed to an isolating stage BA and transmitted through a feedback loop FBL to the stabilized current source SPS.
  • the isolating stage BA, the feedback loop FBL and the stabilized current source SPS together represent a potentiostat P which serves to stabilize the potential of the cathode 9 with respect to the calomel electrode.
  • the cutting knife 22 is shown in FIG. 3 as being able to be put into operation by the drive means 23 under the control of both the timer 24 and the limit signal amplifier LSA.
  • the limit signal amplifier LSA is connected to the output of the isolating stage BA and is arranged in such a way that when the probe potential drops below the limit set on the limit signal amplifier LSA, this amplifier starts the drive means 23 without taking into account the status of the timer 24.
  • the above-described electrolytic metal recovery cell is intended to electrolytically recover metal from a solution containing the metal and is particularly suitable for the recovery of silver metal from used photographic processing solutions.
  • the solution is introduced into the cell through the inlet nozzle 4 and leaves it again through the outlet nozzle 6, whereby it can be circulated through the cell several times in succession until the recovery is complete.
  • the cell uses a rotating cylindrical cathode 9 for the recovery, the operation of which has been described in the literature. Briefly, in the operation of such a cell, the cathode is rotated and metal is deposited as a powder on it, the electrolysis conditions being chosen so that the metal is deposited as a powder removable from the cathode.
  • the deposition of silver on the rotating cylindrical cathode has the advantages, on the one hand, that the cell can be constructed to have a high recovery capacity in relation to its size, and, on the other hand, that the powder is easily removed from the rotating cylinder and can then be separated by filtering.
  • the cell When preparing the present cell for commissioning, the cell is filled with a silver salt solution and the electrolysis conditions are first selected so that when the cathode is rotated, it is hard-plated with a thin layer of silver. The cell is then ready for start-up, and the solution to be treated is passed through the cell, the cathode is rotated, and the electrolysis conditions are now selected so that the silver in powder form is deposited on the rotating cathode.
  • the drive means 23 is turned on to set the shaft 20 in rotation and to remove deposited silver powder from the cathode by the cutting knife 22, whereupon the powder from the cell through the outlet port 6 rinsed out and collected in a suitable filter.
  • Fig. 2 shows the cutting knife 22 and the shaft 21 stationary, it can be seen that the cutting knife 22 extends helically around that part of the cutting knife holder 21 which is located away from the cathode.
  • the radial distance from the center of the cutting knife shaft 20 to the closest point to the edge of the flange 12 of the end cap 11 is equal to the radial distance from the center of the drive shaft 20 to the outermost part of the cutting knife 22.
  • the flanges 12 now protrude a certain distance beyond the cylinder 10 of the cathode 9, which allows the formation of the "hard-plated" metal layer mentioned above and the remaining of a very thin layer of powder deposited on it. Since the end caps 11 are made of plastic, it is easy to see that they do not have to be dimensioned exactly, since the first rotation of the cutting knife 22 shaves the edges of the flanges 12 to the required diameter.
  • the cathode rotates at a constant speed from 200 to 2000 rpm. can be, with practical operation about 1 000 U / min. to be favoured.
  • a suitable speed for the shaft 20 and the cutting knife is 1/4 to 3 rpm.
  • the timer 24 and the drive means 23 are set so that they allow the shaft 20 to perform an entire revolution or an integral number of revolutions, so that the cutting knife and shaft assume the same rest position with each revolution as shown in FIG. 2.
  • the cutting knife when it rotates and removes metal from the cathode, it only makes point contact with the metal. This reduces the stress on the knife and ensures that metal can be removed from the cathode by the knife, even if the electrolysis conditions have not been selected correctly or are subject to fluctuations and the silver on the cathode has been deposited not as a powder but as a coherent coating.
  • Another feature that helps to influence the cutting force is formed by the pitch angle of the helical cutting knife around the cutting knife holder 21, a larger pitch angle reducing the stress on the knife.
  • the helical knife should not extend completely around the circumference of the knife holder, but it has been found that a knife length over a circumferential angle of 120 to 180 ° represents a useful compromise between the two conflicting requirements.
  • the cam 25 actuates a microswitch 26 each time the knife drive shaft is rotated anew, which sends an anode pulse through the holder and knife, as a result of which silver deposited on the latter dissolves again.
  • the anode pulse is delivered directly from the anode.
  • the operating potential of the rotating cylindrical cathode is the most important factor in ensuring that the silver is electrolytically precipitated as a powder.
  • the potential near the cathode which is measured by the probe of the reference electrode, must be given a value which is above the cathode potential and which depends on the metal and on the distance between the probe and the cathode surface.
  • the probe 28 of the reference electrode RE is therefore at one end as close as possible to the cathode surface, i. H. located on the cylindrical surface defined by the edges of the flanges 12 and as far as possible from the influence of the anode.
  • the current used increases as the metal layer on the cathode thickens or when the metal ion concentration in the solution suddenly increases.
  • the increase in the current intensity causes an increased load on the current source, and the electrolytic deposition can then only be continued with an increased current source.
  • the potentiostat places limits on such an increase in the power supply.
  • an increase in the output power of the potentiostat also increases the costs for the components used and the complexity of the system. It is therefore desirable to keep the output power as low as possible.
  • the current used in electrodeposition can be controlled by removing the deposited metal.
  • the control of the current is achieved by operating the cutting knife 22, and this can be done when a maximum, previously selected current value is reached.
  • the period in which this value is reached may a. is subject to fluctuations depending on the metal ion concentration, and since this affects the thickness and to some extent also the type of deposition, its removal according to the invention is effected by the operation of the cutting knife during predetermined periods of time which are chosen to ensure that the preselected one Maximum current is never reached.
  • the cell of the invention is capable of treating spent photographic fixer solutions with relatively high silver concentrations using moderate power. If there is no cutting knife operating in the manner described above, a much larger power supply combined with significantly higher equipment costs is required to process the same solutions.
  • the cathode potential is immediately raised to its desired value when the cutting knife is actuated.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)

Claims (10)

1. Cellule électrolytique pour la récupération de métaux comprenant une enceinte (1, 2) qui est munie d'une entrée (4) et d'une sortie (6) pour une solution contenant le métal à récupérer et dans laquelle sont logées une anode (7), une cathode cylindrique (9) montée mobile en rotation dans l'enceinte et une lame (22), la lame (22), lors du fonctionnement de la cellule, enlevant de la totalité de la surface (10) de la cathode le métal déposé sous forme de poudre, caractérisée par le fait qu'il est prévu des moyens électriques qui mettent la lame en marche à des intervalles de temps prédéterminés et à tout moment lorsque le potentiel de la cathode présente un écart défini par rapport à une valeur de potentiel caractérisant les conditions de consigne établies pour le fonctionnement de la cellule.
2. Cellule électrolytique pour la récupération de métaux selon la revendication 1, caractérisée par le fait que la lame (22) est installée sur un arbre (20) qui peut être mis en rotation par un moyen d'entraînement (23), et, dans une zone correspondant au moins à la longueur de la cathode (9), s'étend en forme d'hélice autour de seulement une partie de la périphérie de l'arbre (20), la lame (22) étant disposée de manière qu'à la position de repos, la zone longitudinale, dépourvue de lame (22), de l'arbre (20), soit tournée du côté de la cathode (9) à distance de celle-ci et que lors de la rotation de l'arbre (20), la lame (22) pénètre avec une profondeur prédéterminée dans le métal déposé sur la cathode (9).
3. Cellule électrolytique pour la récupération de métaux selon là revendication 2, caractérisée par le fait que la lame (22) s'étend sur un angle de 120 à 180° autour de la périphérie de l'arbre (20).
4. Cellule électrolytique pour la récupération de métaux selon la revendication 2 ou 3, caractérisée par le fait que l'arbre (20) est réalisé en acier inoxydable et la lame (22) en acier stéllité.
5. Cellule électrolytique pour la récupération de métaux selon l'une des revendications 1 à 4, caractérisée par le fait qu'il est prévu des moyens par lesquels après la mise en route du moyen d'entraînement (23), des impulsions anodiques peuvent être délivrées à la lame (22).
6. Cellule électrolytique pour la récupération de métaux selon l'une des revendications 1 à 5, caractérisée par le fait qu'un potentiostat (P) et une électrode de référence (RE) sont prévus pour la surveillance du potentiel de la cathode en vue du maintien de sa valeur de consigne.
7. Procédé pour la commande du fonctionnement d'une cellule électrolytique pour la récupération de métaux, dans lequel on met une cathode cylindrique tournante (9) au contact d'une solution contenant des ions du métal à récupérer dans les conditions voulues pour que le métal se dépose sous forme de poudre sur la cathode tournante (9), et dans lequel on enlève de la cathode au moyen d'une lame (22), le métal déposé, caractérisé par le fait que l'on surveille le potentiel de la cathode par rapport à une électrode de référence et que l'on met la lame (22) en marche à des intervalles de temps présélectionnés excluant l'apparition d'un courant maximal prédéterminé, ainsi qu'en plus lorsque le potentiel surveillé de la cathode présente un écart défini par rapport à une valeur de potentiel caractérisant les conditions de consigne établies pour le fonctionnement de la cellule.
8. Procédé selon la revendication 7, caractérisé par le fait qu'on utilise une lame (22) qui, dans une zone correspondant au moins à la longueur de la cathode (9), s'étend en forme d'hélice autour d'une partie de la périphérie d'un arbre (20) entraîné par un moteur, que la cathode (9) tourne à une vitesse de rotation de 200 à 2000 tr/min. et que dans les intervalles de temps prédéterminés, l'arbre (20) tourne à une vitesse de 1/4 à 3 tours par minute.
9. Procédé selon la revendication 7 ou 8, caractérisé par le fait qu'au début de la rotation de l'arbre (20) des impulsions anodiques sont envoyées à la lame (22).
10. Procédé selon l'une des revendications 7 à 9, caractérisé par le fait que le métal est de l'argent et la solution une solution de fixage photographique usée.
EP83810013A 1982-01-19 1983-01-13 Cellule électrolytique pour la récupération de métaux et son fonctionnement Expired EP0084521B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
GB8201367 1982-01-19
GB8201367 1982-01-19
GB8207061 1982-03-11
GB8207061 1982-03-11

Publications (3)

Publication Number Publication Date
EP0084521A2 EP0084521A2 (fr) 1983-07-27
EP0084521A3 EP0084521A3 (en) 1983-08-03
EP0084521B1 true EP0084521B1 (fr) 1986-03-05

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP83810013A Expired EP0084521B1 (fr) 1982-01-19 1983-01-13 Cellule électrolytique pour la récupération de métaux et son fonctionnement

Country Status (3)

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US (1) US4406753A (fr)
EP (1) EP0084521B1 (fr)
DE (1) DE3362365D1 (fr)

Families Citing this family (12)

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Publication number Priority date Publication date Assignee Title
DE3832674A1 (de) * 1988-09-27 1990-03-29 Kodak Ag Metallrueckgewinnungs-vorrichtung
US5183544A (en) * 1991-01-03 1993-02-02 Xerox Corporation Apparatus for electrowinning of metal from a waste metal material
DE69214455T2 (de) * 1992-11-10 1997-04-30 Agfa Gevaert Nv Verwendung einer pH-empfindlichen Referenz-Elektrode für die elektrolytische Entsilberung
ES2107328B1 (es) * 1993-09-24 1998-05-16 Asturiana De Zinc Sa Procedimiento y maquina para la limpieza de anodos de cubas electroliticas.
US5454924A (en) * 1994-09-09 1995-10-03 Agfa-Gevaert N.V. Apparatus for the electrolytic recovery of silver from solutions containing silver
NL1006340C2 (nl) * 1997-06-17 1998-12-21 Rafael Technologie En Manageme Werkwijze en inrichting voor het winnen van metalen.
KR100299011B1 (ko) * 1999-06-30 2001-09-22 이재승 무기물 폐 슬러지로 부터 은을 회수하는 방법
DE10112075C1 (de) * 2001-03-12 2002-10-31 Eilenburger Elektrolyse & Umwelttechnik Gmbh Verfahren und Vorrichtung zur Rückgewinnung von Metallen, auch in Kombination mit anodischen Koppelprozessen
AU2004272647A1 (en) * 2003-09-16 2005-03-24 Global Ionix Inc. An electrolytic cell for removal of material from a solution
WO2010063071A1 (fr) * 2008-12-03 2010-06-10 Electrometals Technologies Limited Procédé et dispositif pour séparer un métal d’une cathode
ITRM20130094A1 (it) * 2013-02-19 2014-08-20 Antonino Abrami Metodo per il trattamento e valorizzazione in loco dei metalli residui della lavorazione pirolitica
EP3591082B1 (fr) * 2018-07-04 2020-11-25 ReMetall Deutschland AG Récipient d'électrolyse autoclave destiné à la récupération des plantinoïdes

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CA556000A (fr) * 1958-04-15 N. Brown Kenneth Procede pour produire electrolytiquement de la poudre d'argent
US1254056A (en) * 1915-07-29 1918-01-22 Nat Carbon Co Inc Process of making metal powder.
US1535577A (en) * 1923-01-04 1925-04-28 Cleave Arthur Harold Wyld Apparatus for the electrolytic deposition of metals
US1959376A (en) * 1930-09-26 1934-05-22 Nichols Copper Co Process for producing metal powders
US3560366A (en) * 1968-04-12 1971-02-02 Oscar Fisher Ag-o-mat silver recovery unit
GB1445505A (en) * 1974-06-26 1976-08-11 Ciba Geigy Ag Electrolytic recovery of silver manufacture of knitted articles
GB1505736A (en) * 1975-02-25 1978-03-30 Nat Res Dev Electrolytic production of metals
DE7905205U1 (de) * 1979-02-24 1979-05-31 Dr. Eugen Duerrwaechter Doduco, 7530 Pforzheim Vorrichtung zum elektrolytischen rueckgewinnen von edelmetallen
US4292163A (en) * 1980-01-16 1981-09-29 King Arthur S Liquid treater having electrode stripper
JPS57152482A (en) * 1981-02-13 1982-09-20 Nat Res Dev Electrodeposition cell

Also Published As

Publication number Publication date
DE3362365D1 (en) 1986-04-10
EP0084521A2 (fr) 1983-07-27
EP0084521A3 (en) 1983-08-03
US4406753A (en) 1983-09-27

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