EP0607535B1 - Procédé électrolytique de dissolution de platine d'impuretés métalliques du platine et/ou d'alliages métalliques du platine - Google Patents
Procédé électrolytique de dissolution de platine d'impuretés métalliques du platine et/ou d'alliages métalliques du platine Download PDFInfo
- Publication number
- EP0607535B1 EP0607535B1 EP93118980A EP93118980A EP0607535B1 EP 0607535 B1 EP0607535 B1 EP 0607535B1 EP 93118980 A EP93118980 A EP 93118980A EP 93118980 A EP93118980 A EP 93118980A EP 0607535 B1 EP0607535 B1 EP 0607535B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- platinum
- platinum metal
- hydrochloric acid
- process according
- anode
- 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 - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
Definitions
- the present invention relates to an electrolytic process for dissolving platinum, platinum metal impurities and / or platinum metal alloys, in particular those with a proportion of Rh, Pd, Ir, Au and Ag in aqueous hydrochloric acid.
- the platinum metals are usually in solid form, such as granules, sheets, chips, wires, etc.
- the method according to the invention can also be used to dissolve powders, sludges and precious metals which are located on ceramics, quartz parts, aluminum oxide or silicates.
- platinum metals in the form of granules, sheets or wires are digested with chlorine and hydrochloric acid.
- the platinum metal salts or platinum metal acids formed are rinsed off with aqueous hydrochloric acid.
- the addition of hydrochloric acid and the introduction of Chlorine gas takes place alternately. The process works with a continuously decreasing platinum surface. A targeted addition of hydrochloric acid is not possible. Therefore, no concentrated precious metal solutions can be produced. If the amount of platinum metal is reduced, a high excess of chlorine must be used.
- the invention was therefore based on the object of providing a method for dissolving platinum, platinum metal impurities and / or platinum metal alloys, which works with little outlay in terms of apparatus and safety technology and an acceptable ecological burden.
- platinum metal salts and / or platinum metal acids in hydrochloric acid, the solubility of the platinum or the platinum metal alloys increases sharply and that this dissolving process can be carried out electrolytically.
- the invention therefore relates to an electrolytic process for dissolving platinum, platinum metal impurities and / or platinum metal alloys, in particular from those with a proportion of Rh, Pd, Ir, Au and Ag in aqueous hydrochloric acid, which is characterized in that the dissolving process in an electrolysis cell, which is divided by a cation exchange membrane, optionally in the presence of platinum metal salts or platinum metal acids at temperatures between 50 to 110 ° C and under potentiostatic or voltage-controlled conditions of 2.5 V to 8 V and a current density of 0.3 to 7.0 A / dm 2 .
- the platinum metal to be dissolved is switched as an anode in the electrolysis cell, while platinum, titanium or graphite is used as the cathode.
- the cathode and anode compartment is filled with 6 to 8 N hydrochloric acid and the voltage selected so that the chlorine gas required for better dissolution develops electrolytically.
- the method according to the invention preferably works under potentiostatic or voltage-controlled conditions of 5 V to 7.5 V and a current density of 4.4 to 6.6 A / dm 2 and in a temperature range from 60 to 100 ° C., in particular at 80 ° C.
- the solution is only heated in the anode and cathode compartments at the beginning of the electrolysis.
- the dissolving temperature then sets itself because the process according to the invention works exothermic.
- the platinum metal solution has a concentration between 1 to 700 g / l.
- concentration between 1 to 700 g / l.
- concentrated platinum metal solutions preferably between 10 and 150 g / l.
- the dissolving process must be stopped because the platinum metal salts or acids crystallize out.
- a Teflon membrane (Nafion® membrane) is generally used as the preferred cation exchange membrane loaded with sulfonic acid groups.
- hydrochloric acid is consumed in the anode compartment due to the development of chlorine gas, its concentration remains constant because water molecules are transported into the cathode compartment with the hydrogen ions.
- the dilute hydrochloric acid is withdrawn periodically in the cathode compartment and the loss of concentration is replaced by the addition of concentrated hydrochloric acid.
- the diluted acid is used to dilute concentrated hydrochloric acid for the anode compartment.
- Rh Pd, Ir, Au, Ag, Cu, Fe, Co, Ni, Sb, As, Pb, Cd, Al, Mn, Mo, Si, Zn, Sn, Zr, as components of the platinum metal impurities or platinum metal alloys. W, Ti and Cr in question.
- 500 g of platinum granules are dissolved in an electrolysis cell, which is divided by a cation exchange membrane.
- the anode compartment is filled with 1 l of 8 N HCl.
- the cathode compartment also contains 8 N HCl.
- the platinum to be dissolved serves as the anode, platinum, titanium or carbon is used as the cathode.
- the electrolysis bath is heated to a temperature of 80 ° C. A voltage of 5 V is applied to the cell and work is carried out at a current density of 6.6 A / dm 2 .
- the hydrochloric acid concentration in the cathode and anode compartments is checked and readjusted.
- the hydrochloric platinum solution contained in the anode compartment has a concentration of 650 g platinum / l.
- the platinum granules are dissolved to a residual content of 3% platinum.
- 250 g of platinum-iridium-1 granules are placed in an electrolysis cell, which is divided by a cation exchange membrane filled and 500 ml of 8 N hydrochloric acid in the anode compartment and 250 ml of 8 N hydrochloric acid in the cathode compartment.
- a titanium sheet serves as the cathode and the platinum-iridium-1 granules to be dissolved as the anode.
- the hydrochloric acid in the anode and cathode compartments is heated to 80 ° C.
- a voltage of 6 V is applied to the electrolysis cell and work is carried out at a current density of 5.25 A / dm 2 .
- the electrolysis is stopped after 12 hours.
- the hydrochloric acid platinum-iridium solution has a platinum metal content of 550 g / l.
- the platinum-iridium granules are 95% dissolved.
- 250 g of platinum-rhodium-10 wire residues are placed in the anode compartment of the electrolytic cell, which is divided by a cation exchange membrane.
- a titanium sheet is used as the cathode, and the platinum-rhodium-10 to be dissolved serves as the anode.
- the electrolytic cell is filled with 8 N hydrochloric acid.
- the temperature of the bath is set at 80 to 100 ° C.
- a voltage of 7.5 V is applied to the apparatus and work is carried out at a current density of 6.6 A / dm 2 .
- the hydrochloric acid concentration is checked during the electrolysis and the specified starting concentration is maintained by adding hydrochloric acid.
- the concentration of the platinum metal solution is 330 g / l.
- the platinum-rhodium-10 wires are 90% dissolved.
- 300 g of platinum metal sponge with a composition of 59% platinum, 1% rhodium and 40% palladium are placed in an electrolysis cell which is divided by a cation exchange membrane.
- a titanium sheet serves as the cathode and the platinum metal sponge as the anode.
- the anode compartment is filled with 1 l and the cathode compartment with 500 ml of 6 N hydrochloric acid.
- the hydrochloric acid is heated to 60 ° C.
- a voltage of 5 V is applied to the electrolysis cell and the current density is 4.4 A / dm 2 .
- the hydrochloric acid concentration is kept constant during the electrolysis.
- the electrolysis is stopped after 10 hours.
- the concentration of the platinum metal solution is 635 g / l.
- the platinum metal sponge is 98% dissolved.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Claims (10)
- Procédé d'électrolyse pour dissoudre du platine, des impuretés de platine et/ou des alliages de platine, notamment ceux contenant du Rh, Pd, Ir, Au et Ag dans une solution aqueuse d'acide chlorhydrique, caractérisé par le fait que le platine à dissoudre est connecté comme anode et par le fait que le processus de dissolution se déroule dans une cellule d'électrolyse qui est divisée par une membrane échangeuse de cations, le cas échéant en présence de sels de platine ou d'acides de platine, à des températures comprises entre 50 et 100 °C et dans des conditions potentiostatiques ou avec une tension contrôlée comprise entre 2,5 et 8 V et une densité de courant comprise entre 0,3 et 7,0 A/dm2.
- Procédé selon la revendication 1, caractérisé par le fait qu'on utilise comme cathode du platine, du titane ou du graphite.
- Procédé selon les revendications 1 à 2, caractérisé par le fait que l'on utilise comme membrane échangeuse de cations une membrane en téflon.
- Procédé selon les revendications 1 à 3, caractérisé par le fait que la chambre de cathode et la chambre d'anode de la cellule d'électrolyse sont remplies d'acide chlorhydrique 6 à 8N et que la tension est choisie de manière à produire du gaz chlorhydrique, le contact entre le platine de l'anode et l'acide contenant du platine et le gaz chlorhydrique ayant lieu de manière pulsatoire.
- Procédé selon au moins une des revendications 1 à 4, caractérisé par le fait que le processus de dissolution se déroule dans des conditions potentiostatiques ou avec une tension contrôlée comprise entre 5 V à 7,5 V et une densité de courant comprise entre 4,4 et 6,6 A/dm2.
- Procédé selon au moins une des revendications 1 à 5, caractérisé par le fait que la concentration en acide chlorhydrique dans la chambre d'anode reste constante, la perte de volume en acide chlorhydrique résultant de la formation de la formation de gaz chlorhydrique étant compensée de manière continue.
- Procédé selon au moins une des revendications 1 à 6, caractérisé par le fait que dans la chambre de cathode, l'acide chlorhydrique apauvri est périoidiquement soutiré et que la baisse de concentration est compensée par l'addition d'acide chlorhydrique concentré.
- Procédé selon au moins une des revendications 1 à 7, caractérisé par le fait que le processus de dissolution se déroule dans une plage de température comprise entre 60 et 100 °C.
- Procédé selon la revendication 8, caractérisé par le fait que le processus de dissolution se déroule sous une température de 80 °C.
- Procédé selon au moins une des revendications 1 à 9, caractérisé par le fait que la solution de platine présente une concentration comprise entre 1 et 700 g/l.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4243698 | 1992-12-18 | ||
| DE4243698A DE4243698C1 (de) | 1992-12-18 | 1992-12-18 | Elektrolytisches Verfahren zum Lösen von Platin, Platinmetallverunreinigungen und/oder Platinmetallegierungen |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0607535A1 EP0607535A1 (fr) | 1994-07-27 |
| EP0607535B1 true EP0607535B1 (fr) | 1996-07-03 |
Family
ID=6476276
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP93118980A Expired - Lifetime EP0607535B1 (fr) | 1992-12-18 | 1993-11-25 | Procédé électrolytique de dissolution de platine d'impuretés métalliques du platine et/ou d'alliages métalliques du platine |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US5423957A (fr) |
| EP (1) | EP0607535B1 (fr) |
| JP (1) | JP3229988B2 (fr) |
| AT (1) | ATE140043T1 (fr) |
| CA (1) | CA2111791C (fr) |
| DE (2) | DE4243698C1 (fr) |
| FI (1) | FI100606B (fr) |
| RU (1) | RU2094534C1 (fr) |
| ZA (1) | ZA938996B (fr) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5783062A (en) * | 1995-08-04 | 1998-07-21 | Rhone-Poulenc Chimie | Process for the treatment, by an electrochemical route, of compositions containing precious metals with a view to their recovery |
| DE19829274C2 (de) * | 1998-07-01 | 2002-06-20 | Otb Oberflaechentechnik Berlin | Verfahren zur Rückgewinnung von Edelmetallen |
| RU2164554C1 (ru) * | 2000-01-26 | 2001-03-27 | Карманников Владимир Павлович | Способ выделения благородных металлов из раствора |
| US7255798B2 (en) * | 2004-03-26 | 2007-08-14 | Ion Power, Inc. | Recycling of used perfluorosulfonic acid membranes |
| GB0408805D0 (en) * | 2004-04-08 | 2004-05-26 | Accentus Plc | Precious metal recovery |
| RU2307203C1 (ru) * | 2006-02-14 | 2007-09-27 | Государственное образовательное учреждение высшего профессионального образования "Воронежский государственный технический университет" | Способ электролитического растворения сплавов платиновых металлов |
| DE102006056017B4 (de) * | 2006-11-23 | 2016-02-18 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verfahren zur Rückgewinnung von Edelmetallen |
| JP5431909B2 (ja) * | 2009-12-22 | 2014-03-05 | 田中貴金属工業株式会社 | 白金の電解溶出方法及び電解処理装置 |
| JP7275629B2 (ja) * | 2018-05-16 | 2023-05-18 | 住友金属鉱山株式会社 | 硫酸溶液の製造方法 |
| CN114892016A (zh) * | 2022-05-12 | 2022-08-12 | 昆明理工大学 | 一种从高含银物料中分段式协调氯酸钠浸出金铂钯的方法 |
| CN115976545A (zh) * | 2022-12-23 | 2023-04-18 | 西安汇创贵金属新材料研究院有限公司 | 一种铂片的电化学溶解方法 |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD63880A (fr) * | ||||
| US1467202A (en) * | 1921-02-26 | 1923-09-04 | Slatineanu Eulampiu | Process of and apparatus for separating platinum from platiniferous materials |
| SU496239A1 (ru) * | 1974-05-23 | 1975-12-25 | Институт физико-органической химии АН Белорусской ССР | Способ извлечени платины из отработанного алюмоплатинового катализатора |
| US4382845A (en) * | 1981-08-10 | 1983-05-10 | Chevron Research Company | Selective electrowinning of palladium |
| JPS6230827A (ja) * | 1985-04-25 | 1987-02-09 | Chlorine Eng Corp Ltd | 貴金属の溶解方法 |
| EP0242111B1 (fr) * | 1986-04-07 | 1992-07-01 | Tosoh Corporation | Procédé de production d'un sel métallique par électrolyse |
-
1992
- 1992-12-18 DE DE4243698A patent/DE4243698C1/de not_active Expired - Fee Related
-
1993
- 1993-11-25 AT AT93118980T patent/ATE140043T1/de not_active IP Right Cessation
- 1993-11-25 EP EP93118980A patent/EP0607535B1/fr not_active Expired - Lifetime
- 1993-11-25 DE DE59303139T patent/DE59303139D1/de not_active Expired - Fee Related
- 1993-12-01 ZA ZA938996A patent/ZA938996B/xx unknown
- 1993-12-16 FI FI935660A patent/FI100606B/fi not_active IP Right Cessation
- 1993-12-17 RU RU9393056628A patent/RU2094534C1/ru not_active IP Right Cessation
- 1993-12-17 CA CA002111791A patent/CA2111791C/fr not_active Expired - Fee Related
- 1993-12-17 JP JP34328993A patent/JP3229988B2/ja not_active Expired - Fee Related
- 1993-12-20 US US08/170,423 patent/US5423957A/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CA2111791C (fr) | 2003-11-04 |
| FI100606B (fi) | 1998-01-15 |
| DE59303139D1 (de) | 1996-08-08 |
| DE4243698C1 (de) | 1994-03-24 |
| EP0607535A1 (fr) | 1994-07-27 |
| ATE140043T1 (de) | 1996-07-15 |
| CA2111791A1 (fr) | 1994-06-19 |
| FI935660L (fi) | 1994-06-19 |
| JP3229988B2 (ja) | 2001-11-19 |
| RU2094534C1 (ru) | 1997-10-27 |
| US5423957A (en) | 1995-06-13 |
| ZA938996B (en) | 1994-08-03 |
| FI935660A0 (fi) | 1993-12-16 |
| JPH06280076A (ja) | 1994-10-04 |
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