EP0255451B1 - Verfahren zur Ausser- und Wiederinbetriebsetzung einer elektrolytischen Raffinierungsanlage - Google Patents
Verfahren zur Ausser- und Wiederinbetriebsetzung einer elektrolytischen Raffinierungsanlage Download PDFInfo
- Publication number
- EP0255451B1 EP0255451B1 EP87420172A EP87420172A EP0255451B1 EP 0255451 B1 EP0255451 B1 EP 0255451B1 EP 87420172 A EP87420172 A EP 87420172A EP 87420172 A EP87420172 A EP 87420172A EP 0255451 B1 EP0255451 B1 EP 0255451B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- electrolyte
- copper
- restarting
- stoppage
- tanks
- 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
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000007670 refining Methods 0.000 title claims abstract description 8
- 239000003792 electrolyte Substances 0.000 claims abstract description 39
- 239000010949 copper Substances 0.000 claims abstract description 28
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052802 copper Inorganic materials 0.000 claims abstract description 25
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 13
- 230000004087 circulation Effects 0.000 claims abstract description 9
- 239000000654 additive Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 230000002035 prolonged effect Effects 0.000 claims abstract description 6
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000013078 crystal Substances 0.000 claims abstract description 3
- 230000000996 additive effect Effects 0.000 claims abstract 5
- 230000001105 regulatory effect Effects 0.000 claims abstract 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 18
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- 238000007792 addition Methods 0.000 claims description 9
- 229910052801 chlorine Inorganic materials 0.000 claims description 9
- 239000000460 chlorine Substances 0.000 claims description 9
- 229920000159 gelatin Polymers 0.000 claims description 9
- 235000019322 gelatine Nutrition 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000009434 installation Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000012937 correction Methods 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 5
- 239000001828 Gelatine Substances 0.000 claims 4
- 239000001117 sulphuric acid Substances 0.000 claims 2
- 235000011149 sulphuric acid Nutrition 0.000 claims 2
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 230000000750 progressive effect Effects 0.000 abstract description 3
- -1 Cu2+ ions Chemical class 0.000 abstract 1
- 230000001276 controlling effect Effects 0.000 abstract 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 108010010803 Gelatin Proteins 0.000 description 5
- 229910052785 arsenic Inorganic materials 0.000 description 5
- 239000008273 gelatin Substances 0.000 description 5
- 235000011852 gelatine desserts Nutrition 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000003303 reheating Methods 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 230000009897 systematic effect Effects 0.000 description 2
- 229910052714 tellurium Inorganic materials 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
-
- 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
Definitions
- the invention relates to a process for prolonged shutdown and subsequent restarting of copper electrolytic refining tanks, which process makes it possible to obtain commercial grade metal from the first cycle after restarting.
- HC quality high conductivity
- This purification which makes it possible to eliminate the usual impurities such as: Ag, As, Au, Pb, Ni, Co, Sn, Se, Te, Zn, Bi, Fe, is carried out by electrolysis with soluble anode, in an electrolyte with base of copper sulphate and sulfuric acid, maintained at around 60 ° C, by auxiliary heating, at a current density of the order of 300 A / m2.
- Certain impurities pass into the sludge (Ag, Au, Pb, Sn, Se, Te, etc.), others, such as Ni, As, Co remain dissolved in the electrolyte, only the copper depositing at the cathode, at a purity which can reach 99.95%.
- the quality of the cathodic deposit is appreciably improved by a continuous supply in the electrolyte, of organic substances, and in particular of gelatin and thiourea, as well as chlorine, (introduced in the form of HCl).
- the raw copper to be refined is introduced into the tanks in the form of anode plates several centimeters thick, the life of which can be, for example, of the order of about twenty days.
- Refined copper is deposited on thin cathode sheets called "starting sheets" in the form of a massive, compact deposit, the thickness of which gradually increases.
- starting sheets thin cathode sheets
- the cathodes are harvested for the first time, and the starting cathode sheets are renewed. Used anodes are recycled in the foundry.
- the cathode primers, or starting sheets, are obtained in special electrolysis sections (so-called “stripper” sections) in which the cathodes are laminated copper plates (mother plates) on both sides of which a thin deposit is caused. copper (0.8 mm).
- the electrolyte is kept in circulation in the tanks.
- the liquors arrive at the head of the tank and at the bottom, the exit at the bottom of the tank and at the top. Maintaining the temperature is ensured by steam reheating because the Joule effect, due to the low electrolysis voltage (approx. 0.3 volts), is insufficient to maintain the bath at the optimum temperature, l '' from 50 to 60 ° C.
- the electrolyte is enriched in soluble impurities (Ni and As) and is concentrated in copper sulfate.
- Proper electrolysis involves maintaining the copper content of the bath at a given level (40-45 g / I of Cu) and keeping the concentrations of impurities below a certain limit (10 g / I of As and Ni). We are therefore permanently led to purify the electrolyte, and to adjust its Cu content.
- a certain proportion is taken daily, for example 2 / 100th of the total volume, from which a purification is carried out by sequence.
- the copper is extracted by electrolysis in an insoluble anode (lead anode with 6% antimony). It is de-coppering. Cathodes are obtained, of non-commercial quality, which are recycled in the foundry to obtain anode plates.
- An electrolytic copper refining plant operates continuously. However, it can be subject to shutdowns, of more or less long duration, either scheduled or accidental: Breakage of the electrical supply lines, breakdown of a rectifier, or other technical or human failure.
- the subject of the present invention is precisely a process for prolonged shutdown and subsequent restarting of the electrolytic cells, making it possible to obtain refined copper of commercial quality from the first cathode cycle, and this in complete safety for the personnel. and for equipment.
- the implementation of the process also ensures the production of commercial quality cathodes from the first cathode cycle, when the duration of the shutdown is limited to only a few days.
Landscapes
- 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)
- Wire Bonding (AREA)
- Electrotherapy Devices (AREA)
- Separation By Low-Temperature Treatments (AREA)
- Treatment Of Steel In Its Molten State (AREA)
Claims (4)
1. Verfahren zum längeren Außerbetriebsetzen und zum Wiederanfahren einer Anlage zur elektrolytischen Kupferraffination mit löslichen Anoden aus zu raffinierendem Kupfer, Kathodenplatten, auf denen sich das gereinigte Kupfer abscheidet, einem wässerigen Elektrolyt auf Basis von Kupfersulfat und Schwefelsäure sowie Zusatzstoffen, der mittels einer Hilfsheizung auf einer Temperatur von 50 bis 60 °C gehalten und in dauernden Umlauf gebracht wird, welche Anlage außerdem Wannen zur Bildung von Startkathodenfolien aus Mutterplatten aufweist, gekennzeichnet durch die Abfolge der folgenden Schritte:
a) für das Außerbetriebsetzen senkt man allmählich den Kupfergehalt des Elektrolyten bis auf 40 g/I, wobei man die Zugaben von Zusatzstoffen, die Gelatine, Thioharnstoff, Chlor sind, beibehält. Die Zusammensetzung des Elektrolyten muß reguliert werden, damit außerdem der Gehalt an H2 S04 in der Größenordnung von 180 g/I ist; unterbricht man gleichzeitig den Elektrolysestrom, die Aufheizung und den Umlauf des Elektrolyten; senkt man das Niveau des Elektrolyten etwas unterhalb des oberen Randes der Kathodenplatten; bedeckt man die Wannen mit einer wärmeisolierenden Verkleidung und läßt den Elektrolyt in den Wannen durch Bildung feiner CuS04-Kristalle kristallisieren.
b) für das Wiederanfahren setzt man den Umlauf des Elektrolyten während 24 Stunden wieder in Gang; setzt man die Aufheizung des Elektrolyten zum Erreichen der Temperatur von 50 °C in 48 Stunden wieder in Gang und nimmt dabei die Zusätze von Thioharnstoff und Chlor mit normalem Durchsatz wieder auf; überprüft man dann die Zusammensetzung und die Homogenität des Elektrolytbades und nimmt erforderlichenfalls Korrekturen vor; schaltet man den Elektrolysestrom mit einer Anfangsstärke unter 10 % der Nennstärke wieder ein und nimmt gleichzeitig die Gelatinezugaben wieder auf; steigert man fortschreitend die Stärke des Elektrolysestroms mit einem linearen Stärkeanstieg in Stufen von 500 A, wobei einige Stunden jede Stufenänderung trennen, derart, daß die Nennstärke in etwa 48 Stunden erreicht wird. Die Abschnitte, wo die Anoden nicht dauernd im Elektrolyt umspült werden, schließt man von wiedereinschalten aus und führt sie fortlaufend wieder ein, nachdem der Gleichgewichtsbereich erreicht ist.
2. Verfahren nach dem Anspruch 1, dadurch gekennzeichnet, daß bei der längeren Außerbetriebsetzung die Wannen zur Bildung von Startkathodenfolien (Mutterplatten) mit der Kupferabscheidung auf den Mutterfolien außer Betrieb gesetzt werden, die mit warmem Wasser gewaschen und während der ganzen Dauer des Betriebsstillstands außerhalb des Elektrolyten gelagert werden.
3. Verfahren nach dem Anspruch 1, dadurch gekennzeichnet, daß man zum Wiederanfahren den Elektrolysestrom mit einer Anfangsstärke im Bereich von 5 bis 6 % der Nennstärke wiedereinschaltet.
4. Verfahren zum Außerbetriebsetzen und zum Wiederanfahren einer Anlage zur elektrolytischen Kupferraffination mit löslichen Anoden aus zu raffinierenden Kupfer, Kathodenplatten, auf denen sich das gereinigte Kupfer abscheidet, einem wässerigen Elektrolyt auf Basis von Kupfersulfat und Schwefelsäure sowie Zusatzstoffen, der mittels einer Hilfsheizung auf einer Temperatur von 50 bis 60 °C gehalten und in dauernden Umlauf gebracht wird, welche Anlage außerdem Wannen zur Bildung von Startkathodenfolien aus Mutterplatten aufweist, dadurch gekennzeichnet, daß man für eine zwei Wochen nicht übersteigende Außerbetriebsetzung eine elektrische Abschaltung vornimmt und den Elektrolyt im Umlauf, in der Zusammensetzung und auf der Temperatur beibehält;
- die Zugaben von Zusatzstoffen, die Thioharnstoff, Chlor, Gelatine sind, bis zum elektrischen Abschalten auf ihrem normalen Gehalt beibehalten und beim Wiederanfahren wiederaufgenommen werden;
- während der Außerbetriebsphase die Zugaben von Gelatine ausgesetzt und die Zugaben von Thioharnstoff+ Chlor auf der Basis von 2/3 des normalen Gehalts beibehalten werden;
- ab dem Beginn der Außerbetriebsetzung die Kathodengruppen auf Unterlageteilen derart angezogen werden, daß das Niveau des Elektrolyten unterhalb der Lochungsprägungen der Kathode ist;
- die Wannen zur Bildung von Kathodenfolien mit Kupferabscheidung stillgesetzt werden, die Kathodenfolien mit warmem Wasser gewaschen und während der ganzen Dauer des Betriebsstillstands außerhalb des Elektrolyten gelagert werden;
- beim Wiederanfahren der Anstieg der Stromstärke in Stufen von 500 A (für eine Nennstärke von 9 bis 10 kA) linear ist, wobei einige Stunden jede Stufenänderung trennen, um so die Nennstärke zu erreichen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT87420172T ATE56487T1 (de) | 1986-06-25 | 1987-06-22 | Verfahren zur ausser- und wiederinbetriebsetzung einer elektrolytischen raffinierungsanlage. |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR8609409 | 1986-06-25 | ||
| FR8609409A FR2600674B1 (fr) | 1986-06-25 | 1986-06-25 | Procede d'arret et de remise en marche d'une installation de raffinage electrolytique |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0255451A1 EP0255451A1 (de) | 1988-02-03 |
| EP0255451B1 true EP0255451B1 (de) | 1990-09-12 |
Family
ID=9336835
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP87420172A Expired - Lifetime EP0255451B1 (de) | 1986-06-25 | 1987-06-22 | Verfahren zur Ausser- und Wiederinbetriebsetzung einer elektrolytischen Raffinierungsanlage |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US4746409A (de) |
| EP (1) | EP0255451B1 (de) |
| AT (1) | ATE56487T1 (de) |
| CA (1) | CA1312303C (de) |
| DE (1) | DE3764901D1 (de) |
| ES (1) | ES2017751B3 (de) |
| FI (1) | FI83886C (de) |
| FR (1) | FR2600674B1 (de) |
| MX (1) | MX168446B (de) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113279023B (zh) * | 2021-05-28 | 2023-05-26 | 金川集团股份有限公司 | 金属溶液提纯用循环净化除杂釜及除杂方法 |
| CN113755893B (zh) * | 2021-09-15 | 2024-04-30 | 内蒙古锦联铝材有限公司 | 一种应对铝电解系列长时间大幅度降负荷的处理方法 |
| CN116083970A (zh) * | 2022-12-23 | 2023-05-09 | 河南豫光锌业有限公司 | 一种锌电解系统结晶清理期间析出锌含铅的控制方法 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1614668A (en) * | 1927-01-18 | Copper-extraction process | ||
| US4251334A (en) * | 1980-03-17 | 1981-02-17 | Olin Corporation | Method and apparatus for controlled, low current start-up of one of a series of electrolytic cells |
-
1986
- 1986-06-25 FR FR8609409A patent/FR2600674B1/fr not_active Expired
-
1987
- 1987-06-22 ES ES87420172T patent/ES2017751B3/es not_active Expired - Lifetime
- 1987-06-22 EP EP87420172A patent/EP0255451B1/de not_active Expired - Lifetime
- 1987-06-22 AT AT87420172T patent/ATE56487T1/de not_active IP Right Cessation
- 1987-06-22 DE DE8787420172T patent/DE3764901D1/de not_active Expired - Lifetime
- 1987-06-23 US US07/065,388 patent/US4746409A/en not_active Expired - Fee Related
- 1987-06-23 MX MX007042A patent/MX168446B/es unknown
- 1987-06-23 CA CA000540375A patent/CA1312303C/fr not_active Expired - Fee Related
- 1987-06-24 FI FI872805A patent/FI83886C/fi not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| FR2600674A1 (fr) | 1987-12-31 |
| MX168446B (es) | 1993-05-25 |
| US4746409A (en) | 1988-05-24 |
| FR2600674B1 (fr) | 1988-08-26 |
| FI83886B (fi) | 1991-05-31 |
| ES2017751B3 (es) | 1991-03-01 |
| CA1312303C (fr) | 1993-01-05 |
| DE3764901D1 (de) | 1990-10-18 |
| FI83886C (fi) | 1991-09-10 |
| FI872805A0 (fi) | 1987-06-24 |
| ATE56487T1 (de) | 1990-09-15 |
| FI872805L (fi) | 1987-12-26 |
| EP0255451A1 (de) | 1988-02-03 |
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