CA2457071C - Hydrogen evolution inhibiting additives for zinc electrowinning - Google Patents
Hydrogen evolution inhibiting additives for zinc electrowinning Download PDFInfo
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- CA2457071C CA2457071C CA002457071A CA2457071A CA2457071C CA 2457071 C CA2457071 C CA 2457071C CA 002457071 A CA002457071 A CA 002457071A CA 2457071 A CA2457071 A CA 2457071A CA 2457071 C CA2457071 C CA 2457071C
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- cpc
- zinc
- zinc electrowinning
- electrowinning
- current efficiency
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- 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
- C25C1/16—Electrolytic production, recovery or refining of metals by electrolysis of solutions of zinc, cadmium or mercury
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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)
- Manufacture And Refinement Of Metals (AREA)
- Primary Cells (AREA)
Abstract
A cetylpyridinium salt, cetylpyridinium chloride (CPC) is used as a hydrogen evolution inhibitor (a current efficiency improver) in a commercial zinc electrowinning process. Zinc electrowinning compositions containing a) antimony and b) antimony and glue were tested. Adding CPC at a 0.05mM concentration to the electrowinning liquor resulted in increased current efficiency for both electrolytes.
Description
HYDROGEN EVOLUTION INHIBITING ADDITIVES FOR ZINC ELECTROWINNING
FIELD
The invention is related to additives for zinc electrowinning that inhibit hydrogen evolution and/or improve current efficiency for zinc electrodeposition, specifically cetylpyridinium-based additives.
BACKGROUND
Improving the energy efficiency of the zinc electrowinning process by inhibition of the parasitic hydrogen evolution reaction, which occurs in parallel with zinc deposition, is of major technological and commercial interest. One way of minimizing the cathodic hydrogen evolution is by the use of additives, generally organic compounds, which selectively increase the hydrogen evolution overpotential. Mackinnon et a1.
(Journal of Applied Electrochemistry, Volume 20, pages 728-736, 1990) and Scott et al. (Journal of Applied Electrochemistry, Volume 18, pages 120=127, 1988) describe the use of animal glue in combination with antimony to improve the current efficiency for zinc electrowinning when compared to additive-free electrolytes.
There is a need for improved additives that minimize hydrogen evolution during zinc electrowinning while providing the same or improved performance over traditional additives_ Therefore, it is an object of this invention to provide improved additives for zinc electrowinning that minimize hydrogen evolution while providing similar or improved performance over traditional additives.
S UNWARY
Cetylpyridinium chloride (CPC), a cetylpyridinium salt, was tested as an additive in a zinc electrowinning process in two separate zinc electrowinning electrolyte compositions: 1) with antimony and 2) with both antimony and glue.
The CPC additive had the most significant influence in the presence of antimony or antimony + glue combination, where it increased the current efficiency by 23.2% and 7.6%, respectively.. Moreover, the presence of 0.05 mM CPC did not increase the overall.cell voltage.
DETAILED DESCRIPTION
Methods And Apparatus Commercial beaker test cells containing a commercial electrowinning electrolyte (liquor) were connected to a power supply and placed in a 37 °C water bath. The anodes and cathodes were made of lead and aluminium, respectively. The laboratory supplied MSDS sheet indicated for the electrolyte the following composition: zinc sulfate 28 - 34% by weight, magnesium sulfate 9 - 15 g/l (grams/litre) and manganese 1.5 - 2.5 g/1.
After allowing the temperature inside the test cells to reach the desired value of 37 °C, a constant current of 0.045 A, representing an electrowinning current density of 450 - amperes/meter2, was applied for either 4 or 20 hours to a non-agitated electrolyte. After completion of the experiment the electrode assembly was removed from the glass beaker, rinsed with distilled water and the cathode deposit carefully scraped off and weighed with four digits precision using a digital Mettler AE 100 analytical balance. The test cells were rinsed between experiments with distilled water and acetone in order to remove traces of the organic additives. Replicates were also performed and the standard deviation was estimated.
The zinc electrodeposition current efficiency was calculated based on Faraday's law:
CE(%) _ ' ~ F ~ nzd .100 ( 1 ) I~t~AZn where CE- current efficiency for Zn electrodeposition (o) z - no. of electrons exchanged [=2]
F - Faraday's number [=96485.3 C mol-1]
and - amount of zinc deposit (g) I- applied current [=0.045 A]
t - time (s) AZ" - atomic weight of zinc [=65.39] .
The cetylpyridinium chloride (CPC) (e. g. Sigma-Aldrich, U.S.) had the following structure:
CayHas~Cl C~
~N~(CH2)~4 ~CH3 Example 1 Zinc Electrowinning Liquor with antimony present Antimony (Sb) in 0.04 mg/1 (milligrams/litre) concentration was added as antimony - potassium tartrate to the zinc electrowinning electrolyte. Both four and twenty hour runs were performed. The experimental results of the four-hour runs are summarized in Table 1.
without the CPC additive present in the electrolyte, Sb had a detrimental effect on the current efficiency, i.e. between 65.1% (cell no. 15) and 74.7% (cell no. 14). On average, the current efficiency without the CPC additive present was 69.9%.
Adding CPC improved the current efficiency on average by 23.2%, i . e. from 69 . 9 0 to 93 . 1 0 .
Table 1: Effect of CPC on the current efficiency of zinc electrowinning in the electrolyte containing 0.04 mg/1 Sb (as Sb-tartrate).
Conditions: Current Average efficiency (~) Temperature : 3 7 C per Cell Cs No .
Time : 4 hours 14 15 No additive ' 74.7 65.1 69.9 +1.0 6.8 CPC 0.05 mM (mM = 93.7 92..7 93.1 millimolar) 2.g 0.9 rn The effect of CPC in~longer-term (20 hours) experiment is shown in Table 2. Without the CPC additive, the current efficiency of cell no. 15 was only 36.6%, whilst with 0.05 mM
CPC present the zinc electrowinning current efficiency was 58.9%. Thus, with the CPC additive the current efficiency was higher by 22.3%.
FIELD
The invention is related to additives for zinc electrowinning that inhibit hydrogen evolution and/or improve current efficiency for zinc electrodeposition, specifically cetylpyridinium-based additives.
BACKGROUND
Improving the energy efficiency of the zinc electrowinning process by inhibition of the parasitic hydrogen evolution reaction, which occurs in parallel with zinc deposition, is of major technological and commercial interest. One way of minimizing the cathodic hydrogen evolution is by the use of additives, generally organic compounds, which selectively increase the hydrogen evolution overpotential. Mackinnon et a1.
(Journal of Applied Electrochemistry, Volume 20, pages 728-736, 1990) and Scott et al. (Journal of Applied Electrochemistry, Volume 18, pages 120=127, 1988) describe the use of animal glue in combination with antimony to improve the current efficiency for zinc electrowinning when compared to additive-free electrolytes.
There is a need for improved additives that minimize hydrogen evolution during zinc electrowinning while providing the same or improved performance over traditional additives_ Therefore, it is an object of this invention to provide improved additives for zinc electrowinning that minimize hydrogen evolution while providing similar or improved performance over traditional additives.
S UNWARY
Cetylpyridinium chloride (CPC), a cetylpyridinium salt, was tested as an additive in a zinc electrowinning process in two separate zinc electrowinning electrolyte compositions: 1) with antimony and 2) with both antimony and glue.
The CPC additive had the most significant influence in the presence of antimony or antimony + glue combination, where it increased the current efficiency by 23.2% and 7.6%, respectively.. Moreover, the presence of 0.05 mM CPC did not increase the overall.cell voltage.
DETAILED DESCRIPTION
Methods And Apparatus Commercial beaker test cells containing a commercial electrowinning electrolyte (liquor) were connected to a power supply and placed in a 37 °C water bath. The anodes and cathodes were made of lead and aluminium, respectively. The laboratory supplied MSDS sheet indicated for the electrolyte the following composition: zinc sulfate 28 - 34% by weight, magnesium sulfate 9 - 15 g/l (grams/litre) and manganese 1.5 - 2.5 g/1.
After allowing the temperature inside the test cells to reach the desired value of 37 °C, a constant current of 0.045 A, representing an electrowinning current density of 450 - amperes/meter2, was applied for either 4 or 20 hours to a non-agitated electrolyte. After completion of the experiment the electrode assembly was removed from the glass beaker, rinsed with distilled water and the cathode deposit carefully scraped off and weighed with four digits precision using a digital Mettler AE 100 analytical balance. The test cells were rinsed between experiments with distilled water and acetone in order to remove traces of the organic additives. Replicates were also performed and the standard deviation was estimated.
The zinc electrodeposition current efficiency was calculated based on Faraday's law:
CE(%) _ ' ~ F ~ nzd .100 ( 1 ) I~t~AZn where CE- current efficiency for Zn electrodeposition (o) z - no. of electrons exchanged [=2]
F - Faraday's number [=96485.3 C mol-1]
and - amount of zinc deposit (g) I- applied current [=0.045 A]
t - time (s) AZ" - atomic weight of zinc [=65.39] .
The cetylpyridinium chloride (CPC) (e. g. Sigma-Aldrich, U.S.) had the following structure:
CayHas~Cl C~
~N~(CH2)~4 ~CH3 Example 1 Zinc Electrowinning Liquor with antimony present Antimony (Sb) in 0.04 mg/1 (milligrams/litre) concentration was added as antimony - potassium tartrate to the zinc electrowinning electrolyte. Both four and twenty hour runs were performed. The experimental results of the four-hour runs are summarized in Table 1.
without the CPC additive present in the electrolyte, Sb had a detrimental effect on the current efficiency, i.e. between 65.1% (cell no. 15) and 74.7% (cell no. 14). On average, the current efficiency without the CPC additive present was 69.9%.
Adding CPC improved the current efficiency on average by 23.2%, i . e. from 69 . 9 0 to 93 . 1 0 .
Table 1: Effect of CPC on the current efficiency of zinc electrowinning in the electrolyte containing 0.04 mg/1 Sb (as Sb-tartrate).
Conditions: Current Average efficiency (~) Temperature : 3 7 C per Cell Cs No .
Time : 4 hours 14 15 No additive ' 74.7 65.1 69.9 +1.0 6.8 CPC 0.05 mM (mM = 93.7 92..7 93.1 millimolar) 2.g 0.9 rn The effect of CPC in~longer-term (20 hours) experiment is shown in Table 2. Without the CPC additive, the current efficiency of cell no. 15 was only 36.6%, whilst with 0.05 mM
CPC present the zinc electrowinning current efficiency was 58.9%. Thus, with the CPC additive the current efficiency was higher by 22.3%.
Table 2: Effect of CPC on the zinc electrowinning current efficiency in 20 hour experiment with 0.04 mg/1 Sb in the electrolyte.
Conditions: Current efficiency (%) Temperature : 3 7 per Cel l No .
C
Time: 20 hours 15 No additive 36.6 CPC 0.05 mM 58.9 '5 Example 2 Zinc E~ectrowinning Liquor with both antimony and glue Similar experiments to those in Example 1 were performed with an electrolyte containing 0.04 mg/1 of Sb and 10 mg/1 of glue (e. g. "pearl glue" supplied by Hudson Industries, Johnstown, New York). Both 4 and 20 hour runs were carried out.
The effect of the CPC additive on the zinc electrowinning current efficiency in the 4 hour runs is shown in Table 3.
The presence of glue minimizes to a certain extent the negative effect of antimony, yielding current efficiencies between 88.9% and 90%. However, adding 0.05 mM CPC brought about additional increases of current efficiency, i.e. from 89.4% on average in the absence to 97% in the presence of CPC
(Table 3).
Conditions: Current efficiency (%) Temperature : 3 7 per Cel l No .
C
Time: 20 hours 15 No additive 36.6 CPC 0.05 mM 58.9 '5 Example 2 Zinc E~ectrowinning Liquor with both antimony and glue Similar experiments to those in Example 1 were performed with an electrolyte containing 0.04 mg/1 of Sb and 10 mg/1 of glue (e. g. "pearl glue" supplied by Hudson Industries, Johnstown, New York). Both 4 and 20 hour runs were carried out.
The effect of the CPC additive on the zinc electrowinning current efficiency in the 4 hour runs is shown in Table 3.
The presence of glue minimizes to a certain extent the negative effect of antimony, yielding current efficiencies between 88.9% and 90%. However, adding 0.05 mM CPC brought about additional increases of current efficiency, i.e. from 89.4% on average in the absence to 97% in the presence of CPC
(Table 3).
Table 3: Effect of CPC on the current efficiency of zinc electrowinning in the electrolyte containing 0.04 mg/1 Sb (as Sb-tartrate) + 10 mg/1 glue.
Conditions: Current Average efficiency Temperature: 37 C (%) per CB (~) Cell No.
Time : 4 hours 13 16 No additive 88.9 90.0 89.4 0.9 0.8 CPC 0.05 mM 98.3 95.8 97.0 1.8 .
The 20 hour experiments (Table 4) showed that CPC in 0.05 mM concentration increased the current efficiency of cell no. 16 from 77_2% to 87.3%.
Table 4: Effect of CPC on the zinc electrowinning current efficiency in 20 hour experiment with 0.04 mg/1 Sb and 10 mg/1 glue in the electrolyte.
Conditions: Current efficiency (o) per Temperature : 3 7 Cel l No .
C
Time: 20 hours 16 No additive 77.2 CPC 0.05 mM 87.3 The cell voltage is another important figure of merit of the electrowinning process. An increase in the cell voltage represents an increase in the amount of energy required and, therefore, a less efficient electrowinning process. Table 5 shows that using 0.05 mM CPC in conjunction with Sb and glue did not induce an increase of the cell voltage.
Table 5: Effect of CPC on the average cell voltage in 4 hour experiments with 0.04 mg/1 Sb and 10 mg/1 glue in the electrolyte.
Conditions: Average cell voltage ~(v) Temperature: 37 C
Time: 4 hours No additive 2.83 CPC 0.05 mM 2.83 Accordingly, while this invention has been described with reference to illustrative embodiments, this description is not intended to be construed in a limiting sense. Various modifications of the illustrative embodiments, as well as other embodiments of the invention, will be apparent to persons skilled in the art upon reference to this description. It is therefore contemplated that the appended claims will cover any such modifications or embodiments as fall within the scope of the invention.
Conditions: Current Average efficiency Temperature: 37 C (%) per CB (~) Cell No.
Time : 4 hours 13 16 No additive 88.9 90.0 89.4 0.9 0.8 CPC 0.05 mM 98.3 95.8 97.0 1.8 .
The 20 hour experiments (Table 4) showed that CPC in 0.05 mM concentration increased the current efficiency of cell no. 16 from 77_2% to 87.3%.
Table 4: Effect of CPC on the zinc electrowinning current efficiency in 20 hour experiment with 0.04 mg/1 Sb and 10 mg/1 glue in the electrolyte.
Conditions: Current efficiency (o) per Temperature : 3 7 Cel l No .
C
Time: 20 hours 16 No additive 77.2 CPC 0.05 mM 87.3 The cell voltage is another important figure of merit of the electrowinning process. An increase in the cell voltage represents an increase in the amount of energy required and, therefore, a less efficient electrowinning process. Table 5 shows that using 0.05 mM CPC in conjunction with Sb and glue did not induce an increase of the cell voltage.
Table 5: Effect of CPC on the average cell voltage in 4 hour experiments with 0.04 mg/1 Sb and 10 mg/1 glue in the electrolyte.
Conditions: Average cell voltage ~(v) Temperature: 37 C
Time: 4 hours No additive 2.83 CPC 0.05 mM 2.83 Accordingly, while this invention has been described with reference to illustrative embodiments, this description is not intended to be construed in a limiting sense. Various modifications of the illustrative embodiments, as well as other embodiments of the invention, will be apparent to persons skilled in the art upon reference to this description. It is therefore contemplated that the appended claims will cover any such modifications or embodiments as fall within the scope of the invention.
Claims (9)
1. A method of improved zinc electrowinning, comprising:
adding a cetylpyridinium salt additive to a zinc electrowinning electrolyte.
adding a cetylpyridinium salt additive to a zinc electrowinning electrolyte.
2. A method according to claim 1, wherein said cetylpyridinium salt is a cetylpyridinium halide.
3. A method according to claim 2, wherein said cetylpyridinium halide is cetylpyridinium chloride.
4. A method according to claim 3, wherein said cetylpyridinium chloride is at 0.05 millimolar (mM) concentration in said zinc electrowinning liquor.
5. A method according to claim 1, wherein said zinc electrowinning electrolyte contains zinc sulfate.
6. A method according to claim 1, wherein said zinc electrowinning electrolyte contains antimony.
7. A method according to claim 1, wherein said zinc electrowinning electrolyte contains glue.
8. A method according to claim 7, wherein said glue is animal glue.
9. A method according to claim 8, wherein said animal glue is gelatin.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US31182501P | 2001-08-14 | 2001-08-14 | |
| US60/311,825 | 2001-08-14 | ||
| PCT/CA2002/001250 WO2003016593A2 (en) | 2001-08-14 | 2002-08-13 | Hydrogen evolution inhibiting additives for zinc electrowinning |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2457071A1 CA2457071A1 (en) | 2003-02-27 |
| CA2457071C true CA2457071C (en) | 2007-05-29 |
Family
ID=23208657
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002457071A Expired - Fee Related CA2457071C (en) | 2001-08-14 | 2002-08-13 | Hydrogen evolution inhibiting additives for zinc electrowinning |
Country Status (16)
| Country | Link |
|---|---|
| US (1) | US20050011769A1 (en) |
| EP (1) | EP1417357B1 (en) |
| JP (1) | JP2004537653A (en) |
| KR (1) | KR100599993B1 (en) |
| CN (1) | CN100342061C (en) |
| AU (1) | AU2002322888B2 (en) |
| BR (1) | BR0211933A (en) |
| CA (1) | CA2457071C (en) |
| DE (1) | DE60203301T2 (en) |
| ES (1) | ES2238586T3 (en) |
| HK (1) | HK1075920A1 (en) |
| MX (1) | MXPA04001459A (en) |
| NO (1) | NO20040651L (en) |
| RU (1) | RU2288299C2 (en) |
| WO (1) | WO2003016593A2 (en) |
| ZA (1) | ZA200405167B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100540748C (en) * | 2006-06-15 | 2009-09-16 | 云南冶金集团总公司 | Assembled gelatin additive |
| CN103993330A (en) * | 2014-05-07 | 2014-08-20 | 成都理工大学 | Zinc electrolysis technology of zinc ammonia complex aqueous solution |
| CN106676578B (en) * | 2015-11-11 | 2018-09-28 | 沈阳有色金属研究院 | A kind of new and effective joint additive of Zinc electrolysis |
| CN110512236B (en) * | 2019-09-27 | 2021-05-04 | 中国科学院长春应用化学研究所 | Combined additive and application thereof in zinc electrodeposition |
| CN115133159A (en) * | 2022-09-01 | 2022-09-30 | 河南师范大学 | Functional aqueous zinc ion battery electrolyte and preparation method and application thereof |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4028199A (en) * | 1974-08-05 | 1977-06-07 | National Development Research Corporation | Method of producing metal powder |
| CA1064852A (en) * | 1975-12-31 | 1979-10-23 | Cominco Ltd. | Method for evaluating a system for electrodeposition of metals |
| CA1111125A (en) * | 1978-07-05 | 1981-10-20 | Robert C. Kerby | Method and apparatus for control of electrowinning of zinc |
| US4699696A (en) * | 1986-04-15 | 1987-10-13 | Omi International Corporation | Zinc-nickel alloy electrolyte and process |
| US4717458A (en) * | 1986-10-20 | 1988-01-05 | Omi International Corporation | Zinc and zinc alloy electrolyte and process |
| CN1023818C (en) * | 1991-03-19 | 1994-02-16 | 昆明工学院 | Vacuum distillation zinc extraction method of hot galvanizing residue |
| US5635051A (en) * | 1995-08-30 | 1997-06-03 | The Regents Of The University Of California | Intense yet energy-efficient process for electrowinning of zinc in mobile particle beds |
| US6086691A (en) * | 1997-08-04 | 2000-07-11 | Lehockey; Edward M. | Metallurgical process for manufacturing electrowinning lead alloy electrodes |
| CN1065919C (en) * | 1998-04-24 | 2001-05-16 | 昆明理工大学 | Vacuum distillation of hard zinc to extract zinc and to concentrate germanium, indium and silver |
| US6238542B1 (en) * | 1998-09-15 | 2001-05-29 | Thomas Helden | Water soluble brighteners for zinc and zinc alloy electrolytes |
| EP1013799A1 (en) * | 1998-12-23 | 2000-06-28 | Half Tone Ltd. | Solution and process for the electrodeposition of gold and gold alloys |
-
2002
- 2002-08-13 US US10/486,711 patent/US20050011769A1/en not_active Abandoned
- 2002-08-13 EP EP02754027A patent/EP1417357B1/en not_active Expired - Lifetime
- 2002-08-13 DE DE60203301T patent/DE60203301T2/en not_active Expired - Fee Related
- 2002-08-13 MX MXPA04001459A patent/MXPA04001459A/en not_active Application Discontinuation
- 2002-08-13 KR KR1020047002247A patent/KR100599993B1/en not_active IP Right Cessation
- 2002-08-13 AU AU2002322888A patent/AU2002322888B2/en not_active Ceased
- 2002-08-13 ES ES02754027T patent/ES2238586T3/en not_active Expired - Lifetime
- 2002-08-13 CA CA002457071A patent/CA2457071C/en not_active Expired - Fee Related
- 2002-08-13 JP JP2003520877A patent/JP2004537653A/en not_active Ceased
- 2002-08-13 CN CNB028160207A patent/CN100342061C/en not_active Expired - Fee Related
- 2002-08-13 WO PCT/CA2002/001250 patent/WO2003016593A2/en active IP Right Grant
- 2002-08-13 RU RU2004107493/02A patent/RU2288299C2/en not_active IP Right Cessation
- 2002-08-13 BR BR0211933-1A patent/BR0211933A/en not_active IP Right Cessation
-
2004
- 2004-02-13 NO NO20040651A patent/NO20040651L/en not_active Application Discontinuation
- 2004-06-29 ZA ZA200405167A patent/ZA200405167B/en unknown
-
2005
- 2005-09-14 HK HK05108025A patent/HK1075920A1/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| WO2003016593A3 (en) | 2003-10-09 |
| NO20040651L (en) | 2004-04-16 |
| RU2004107493A (en) | 2005-06-10 |
| BR0211933A (en) | 2004-10-26 |
| US20050011769A1 (en) | 2005-01-20 |
| DE60203301D1 (en) | 2005-04-21 |
| KR100599993B1 (en) | 2006-07-13 |
| EP1417357A2 (en) | 2004-05-12 |
| ES2238586T3 (en) | 2005-09-01 |
| EP1417357B1 (en) | 2005-03-16 |
| WO2003016593A2 (en) | 2003-02-27 |
| HK1075920A1 (en) | 2005-12-30 |
| KR20040044443A (en) | 2004-05-28 |
| AU2002322888B2 (en) | 2007-06-21 |
| CN1653209A (en) | 2005-08-10 |
| DE60203301T2 (en) | 2006-04-13 |
| RU2288299C2 (en) | 2006-11-27 |
| MXPA04001459A (en) | 2005-02-17 |
| ZA200405167B (en) | 2005-06-27 |
| CN100342061C (en) | 2007-10-10 |
| JP2004537653A (en) | 2004-12-16 |
| CA2457071A1 (en) | 2003-02-27 |
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| EEER | Examination request | ||
| MKLA | Lapsed |