CN107675212B - A kind of Zinc electrolysis fluorine-resistant lead base composite anode and preparation method thereof - Google Patents
A kind of Zinc electrolysis fluorine-resistant lead base composite anode and preparation method thereof Download PDFInfo
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- CN107675212B CN107675212B CN201710973173.5A CN201710973173A CN107675212B CN 107675212 B CN107675212 B CN 107675212B CN 201710973173 A CN201710973173 A CN 201710973173A CN 107675212 B CN107675212 B CN 107675212B
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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
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
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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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
Abstract
The invention discloses a kind of Zinc electrolysis fluorine-resistant lead base composite anodes and preparation method thereof.Composite film CaO-MnO is deposited in Pb or Pb alloy surface using electrochemical deposition method2‑PbO2.The introducing of CaO can intercept the fluorine ion to Pb substrate diffusion transport, inhibit corrosion of the fluorine to Pb substrate, improve the combination of substrate and film layer.The MnO of Dispersed precipitate2It can inhibit MnO in film layer2/PbO2‑PbSO4/MnO2The formation of laminated construction improves oxidation film layer internal stability.The composite anode can intercept the fluorine to lead substrate transport and improve oxidation film layer internal stability, the significant service life for extending lead base composite anode in fluorine-containing sulfuric acid system.
Description
Technical field
A kind of Zinc electrolysis fluorine-resistant lead base composite anode and preparation method thereof belongs to electrochemistry and field of material technology.
Background technique
With the fast development of zinc abstraction industry, zinc concentrate grade gradually declines, and mineral composition is increasingly sophisticated.In this background
Under, the concentration of fluorine gradually rises in zinc abstraction system.Mainly there is the source of fluorine in Zn system: the fluoride in zinc concentrate, lead zinc
The zinc oxide fumes etc. of joint smeltery lead system.By high temperature firing method process can volatilize remove 70% or so fluorine, be left
30% or so fluorine then enters electrolyte.In electrodeposition process, due to the open circuit of not no fluorine, fluorine in electrolyte is caused constantly to be accumulated, it is dense
Degree gradually rises.In addition, the direct leaching-out technique of zinc concentrate has abandoned traditional calcining process, all fluorine all enter in concentrate
Electrolyte, Funing tablet are much higher than traditional roasting-leaching process.Therefore, with the popularization of direct leaching-out technique, fluorine is to Zinc electrolysis work
The influence of sequence will be highlighted further, cause the concern of the whole industry.
Fluorine initially causes industry concern to be because its corrosion for aggravating cathode Al plate causes stripping zinc difficult in turn.As fluorine is dense
Degree rises, and influence of the fluorine to lead-based anode also gradually shows.Influence for fluorine to lead anode performance, research is reported both at home and abroad
It focuses mostly in fluorine to Pb/PbO2The influence of the analysis oxygen behavior of electrode.Applicant's early-stage study fluorine is to Pb-Ag anode oxidation membrane
The influence of property and corrosion behavior.Research is found in H2SO4System, fluorine (100 mg L-1) addition make Pb-Ag substrate corrosion hole
Hole is increased, and aperture increases, corrosion depth deepens.The main mechanism of fluorine aggravation Pb-Ag anodic attack are as follows: first, fluorine has height anti-
Activity is answered, at polarization initial stage, fluorine is directly contacted with Pb substrate, aggravates substrate Pb2+Oxidation dissolution；Second, raw in high fluorine solution
At film layer gap and crack it is more, consistency is low, increase substrate and electrolyte contacts probability.Containing fluoro- manganese electrolyte system,
The film layer of Pb base anode surface is in MnO2/(PbO2-PbSO4)/MnO2There is acutely concussion, show to contain in laminated construction, anode potential
Fluorine system film layer is easy to fall off, and stability is poor.Based on early-stage study as a result, it can be concluded that improving lead-based anode in fluorine-containing, manganese
Stability and service life key in sulfuric acid solution are to inhibit fluorine to the corrosion of substrate and improve the stability of film layer.
For the constantly soaring problem of Funing tablet in Zinc electrolysis electrolyte, a large amount of fluorine removal research is carried out both at home and abroad.It is main
It is divided into two major classes, one kind is to carry out vaporization at high temperature fluorine removal to zinc calcine in firing method process, and another kind of is in wet process
Electrolyte is carried out to precipitate/adsorption-defluorination.A large amount of research work has been put into the exploitation of defluorinating agent and design direction both at home and abroad
Make.The study found that Ca salt has excellent Fluoride-Absorption Capacity, this mainly has benefited from CaF 2 Solubility product is small, easily forms insoluble chemical combination
Object is simultaneously separated from solution.By the inspiration that sulfuric acid system defluorinating agent is studied, this patent is proposed the Ca salt fluorine removal in solution
Agent is introduced into film layer, i.e., CaO is introduced into film layer, during military service CaO can intercept to lead base bottom spread fluorine from
Son alleviates corrosion of the fluorine to substrate, improves the combination stability of substrate and film layer.
In addition, film layer is in MnO in manganese containing solution2/(PbO2-PbSO4)/MnO2Laminated construction, MnO in the structure2Layer with
PbO2-PbSO4Layer between combine it is weaker, film layer is easy to fall off, and film layer internal stability is poor, and film layer pays no attention to the protective effect of substrate
Think.Therefore, improving film layer internal stability is also the important channel for improving lead-based anode service life.To prevent laminated construction
It generates, this patent proposes the MnO that Dispersed precipitate is deposited in film layer2Particle, the MnO dispersed in film layer2Particle can inhibit film layer
External Mn2+Quick oxide deposition, eliminate laminated construction, and then improve film layer stability.
Summary of the invention
For lead-based anode in fluorine-containing sulfuric acid system the undesirable disadvantage of corrosion resistance, propose a kind of Zinc electrolysis fluorine-resistant
Lead base composite anode, composite anode film layer are CaO-MnO2-PbO2, the introducing of CaO can slow down corrosion of the fluorine to substrate；Disperse
The MnO of distribution2Particle can inhibit laminated construction to generate, and promote film layer internal stability, improve protection of the film layer to substrate.
A kind of Zinc electrolysis fluorine-resistant lead base composite anode, membranous layer ingredient CaO, MnO2, PbO, MnO2Particle in film layer more
Dissipate distribution.
Further, CaO grain graininess is 50 nm ~ 100 μm, CaO granule content 1 wt.% ~ 10 wt.%.
Further, MnO2Grain graininess is 50 nm ~ 500 μm, MnO2Granule content 1 wt.% ~ 30 wt.%.
Further, composite anode substrate is Pb or Pb alloy, and wherein alloying element is selected from Ag, Ca, Sn, Sb, Se,
At least one of Co, Ce, Nd, Al, preferably Ag, Ca, at least one of Co and Nd；Underlying structure can for plate,
Cellular, rodlike middle one kind.
On the other hand, the present invention provides a kind of sides for preparing Zinc electrolysis fluorine-resistant lead base composite anode as described above
Method deposits composite film CaO-MnO in Pb or Pb alloy surface using electrochemical deposition method2-PbO2.In deposition process, the source Ca
For CaO particle, the source Pb is Pb (NO3)2, the source Mn is suspension MnO2Particle.Deposition process uses alkaline electrolysis liquid system, pH control
In 8-12, electrolyte temperature control is at 25 ~ 70 DEG C, 200 ~ 2000 r/min of mixing speed.
Further, electrolyte composition includes 1 ~ 10 g/L CaO, 0.5 ~ 2 mol/L Pb2+、1 ~ 20 g/L
MnO2。
Further, depositional mode can aoxidize electro-deposition with constant current or constant pressure.The control of Constant Electric Current depositing current density 2 ~
100 mA cm-2, constant pressure electro-deposition control of Electric potentials is in 1.2 ~ 3.0 V vs SCE (saturated calomel electrode).
Further, Pb or Pb alloy substrates are in horizontal positioned in electrodeposition process.
The present invention proposes Pb (Pb alloy)/CaO-MnO2-PbO2The introducing of composite anode, CaO significantly slows fluorine to substrate
Corrosion, meanwhile, the MnO of Dispersed precipitate2Particle inhibits laminated construction to generate, and promotes membranous layer stability, improves film layer to substrate
Protective effect.Comprehensive CaO and MnO2Bring positive influence, the composite anode are expected to improve lead-based anode in fluorine-containing sulfuric acid system
Stability and extend service life.
Specific embodiment
The contents of the present invention are described in detail with the following Examples.
Comparative example 1
Using pure Pb plate as electrode, electrolyte group becomes 20 g/L CaO, 1.0 mol/L Pb2+、10 g/L MnO2, pH=
8,1500 r/min of mixing speed, electrolyte temperature are 35 DEG C, constant potential (2.0 V vs. Hg/Hg2SO4) under the conditions of deposit 50
Min obtains Pb/CaO-MnO2-PbO2Composite anode, CaO grain graininess is 55 nm, CaO particle in the composite anode film layer
15 wt.% of content；MnO2Grain graininess is 100 μm, MnO2Granule content 5 wt.%, MnO2Particle Dispersed precipitate in film layer,
The anode is in the H for containing 100 mg/L fluorine2SO4Constant current polarization (500 A m in (160 g/L) solution-2) after 72h, substrate corrosion
Pattern compares Pb/PbO2Anodic attack hole reduce 58%, average corrosion aperture reduce 80%, but due in oxidation film layer CaO contain
It measures excessively high, causes film layer resistance big, anode potential improves about 30%.
Embodiment 1
Using pure Pb plate as electrode, electrolyte group becomes 5 g/L CaO, 1.0 mol/L Pb2+、10 g/L MnO2, pH=
8,1500 r/min of mixing speed, electrolyte temperature are 35 DEG C, constant potential (2.0 V vs. Hg/Hg2SO4) under the conditions of deposit 50
Min obtains Pb/CaO-MnO2-PbO2Composite anode, CaO grain graininess is 50 nm, CaO particle in the composite anode film layer
2 wt.% of content；MnO2Grain graininess is 100 μm, MnO2Granule content 5 wt.%, MnO2Particle Dispersed precipitate in film layer, should
Anode is in the H for containing 100 mg/L fluorine2SO4Constant current polarization (500 A m in (160 g/L) solution-2) after 72h, substrate corrosion shape
Looks compare Pb/PbO2Anodic attack hole reduces 50%, and average corrosion aperture reduces 70%.
Embodiment 2
Using Pb-Ag plate as electrode, electrolyte group becomes 10 g/L CaO, 0.5 mol/L Pb2+、5 g/L MnO2, pH=
10,800 r/min of mixing speed, electrolyte temperature are 55 DEG C, and current density is 50 mA cm-2Under the conditions of deposit 15 min, obtain
Obtain Pb/CaO-MnO2-PbO2Composite anode, CaO grain graininess is 100 μm in the composite anode film layer, CaO granule content 8
wt.%；MnO2Grain graininess is 100 nm, MnO2Granule content 20 wt.%, MnO2Particle Dispersed precipitate in film layer, the anode
In the H for containing 200 mg/L fluorine2SO4Constant current polarization (500 A m in (160 g/L) solution-2) after 72h, substrate corrosion pattern phase
Compared with Pb/PbO2Anodic attack hole reduces 70%, and average corrosion aperture reduces 80%.
Embodiment 3
Using Pb-Ag-Ca plate as electrode, electrolyte group becomes 7 g/L CaO, 2 mol/L Pb2+、18 g/L MnO2, pH
=9,2000 r/min of mixing speed, electrolyte temperature are 40 DEG C, constant potential (2.7 V vs. Hg/Hg2SO4) under the conditions of deposit
40 min obtain Pb/CaO-MnO2-PbO2Composite anode, CaO grain graininess is 1 μm, CaO in the composite anode film layer
10 wt.% of grain content；MnO2Grain graininess is 50 nm, MnO2Granule content 28 wt.%, MnO2Particle disperse point in film layer
Cloth, the anode is in the H for containing 120 mg/L fluorine2SO4Constant current polarization (500 A m in (160 g/L) solution-2) after 9 days, substrate
Erosion profile compares Pb/PbO2Anodic attack hole reduces 55%, and average corrosion aperture reduces 65%, and corrosion depth reduces 60%.
Embodiment 4
Using Pb-Co plate as electrode, electrolyte group becomes 5 g/L CaO, 1.2 mol/L Pb2+、12 g/L MnO2, pH=
11,200 r/min of mixing speed, electrolyte temperature are 25 DEG C, constant current (10 mA cm-2) under the conditions of deposit 60 min, obtain
Pb/CaO-MnO2-PbO2Composite anode, CaO grain graininess is 50 μm in the composite anode film layer, CaO granule content 1
wt.%；MnO2Grain graininess is 500 μm, MnO2Granule content 30 wt.%, MnO2Particle Dispersed precipitate in film layer, the anode
In floride-free H2SO4Constant current polarization (500 A m in (160 g/L) solution-2) after 72h, substrate corrosion pattern compares Pb/PbO2
Anodic attack hole reduces 20%, and average corrosion aperture reduces 10%.
Embodiment 5
Using Pb-Ag-Nd plate as electrode, electrolyte group becomes 6 g/L CaO, 0.7 mol/L Pb2+、20 g/L MnO2,
PH=12,1500 r/min of mixing speed, electrolyte temperature are 70 DEG C, constant current (100 mA cm-2) under the conditions of deposit 15
Min obtains Pb/CaO-MnO2-PbO2Composite anode, CaO grain graininess is 75 μm in the composite anode film layer, CaO particle
5 wt.% of content；MnO2Grain graininess is 300 μm, MnO2Granule content 15 wt.%, MnO2Particle Dispersed precipitate in film layer,
The anode is in the H for containing 250 mg/L fluorine2SO4Constant current polarization (500 A m in (160 g/L) solution-2) after 72h, substrate corrosion
Pattern compares Pb/PbO2Anodic attack hole reduces 75%, and average corrosion aperture reduces 82%, and average corrosion depth reduces 65%.
Claims (8)
1. a kind of Zinc electrolysis fluorine-resistant lead base composite anode, it is characterised in that: membranous layer ingredient CaO, MnO2、PbO2, MnO2Particle
The Dispersed precipitate in film layer.
2. a kind of Zinc electrolysis according to claim 1 fluorine-resistant lead base composite anode, it is characterised in that: CaO grain graininess
For 50 nm ~ 100 μm, CaO granule content 1 wt.% ~ 10 wt.%.
3. a kind of Zinc electrolysis according to claim 1 fluorine-resistant lead base composite anode, it is characterised in that: MnO2Grain graininess
For 50 nm ~ 500 μm, MnO2Granule content 1 wt.% ~ 30 wt.%.
4. a kind of Zinc electrolysis according to claim 1 fluorine-resistant lead base composite anode, it is characterised in that: composite anode substrate
For Pb or Pb alloy, wherein alloying element is selected from Ag, Ca, Sn, Sb, Se, Co, Ce, Nd, at least one of Al；
Underlying structure is plate, cellular, rodlike middle one kind.
5. a kind of method for preparing the Zinc electrolysis fluorine-resistant lead base composite anode as described in claim 1-4 any one, feature
It is: composite film CaO-MnO is deposited in Pb or Pb alloy surface using electrochemical deposition method2-PbO2；In deposition process, Ca
Source is CaO particle, and the source Pb is Pb (NO3)2, the source Mn is suspension MnO2Particle；Deposition process uses alkaline electrolysis liquid system, pH control
System is in 8-12, and electrolyte temperature control is at 25 ~ 70 DEG C, 200 ~ 2000 r/min of mixing speed.
6. the preparation method of a kind of Zinc electrolysis fluorine-resistant lead base composite anode according to claim 5, it is characterised in that: electrolysis
Liquid composition includes 1 ~ 10 g/L CaO, 0.5 ~ 2 mol/L Pb2+、1 ~ 20 g/L MnO2。
7. the preparation method of a kind of Zinc electrolysis fluorine-resistant lead base composite anode according to claim 5, which is characterized in that deposition
Mode is that constant current or constant pressure aoxidize electro-deposition；Constant Electric Current depositing current density is controlled in 2 ~ 100 mA cm-2, constant pressure electro-deposition
Control of Electric potentials is in 1.2 ~ 3.0 V vs SCE (saturated calomel electrode).
8. the preparation method of a kind of Zinc electrolysis fluorine-resistant lead base composite anode according to claim 5, which is characterized in that electricity is heavy
Pb or Pb alloy substrates are in horizontal positioned during product.
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| CN109468666B (en) * | 2019-01-16 | 2019-10-25 | 江西理工大学 | The method for preparing anode using the Zinc electrolysis earth of positive pole |
| CN110144607B (en) * | 2019-07-08 | 2020-06-12 | 西安泰金工业电化学技术有限公司 | Preparation method of anti-deformation titanium anode for hydrometallurgy |
| CN114411201B (en) * | 2022-02-15 | 2023-06-20 | 江西理工大学 | Pb/Pb-Mn anode for zinc electrodeposition and preparation method thereof |
| CN114411206B (en) * | 2022-02-17 | 2023-05-09 | 江西理工大学 | Composite anode for zinc electrodeposition and preparation method thereof |
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| CN101001693A (en) * | 2004-07-23 | 2007-07-18 | 三井金属矿业株式会社 | Fluorine absorption/desorption agent for electrolysis solution in zinc electrolytic refining, and method for removing fluorine using said fluorine absorption/desorption agent |
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| AU751315B2 (en) * | 1999-01-13 | 2002-08-15 | Rsr Technologies, Inc. | Electrowinning anodes which rapidly produce a protective oxide coating |
| CN101001693A (en) * | 2004-07-23 | 2007-07-18 | 三井金属矿业株式会社 | Fluorine absorption/desorption agent for electrolysis solution in zinc electrolytic refining, and method for removing fluorine using said fluorine absorption/desorption agent |
| CN101886170A (en) * | 2010-06-29 | 2010-11-17 | 白银先达科技服务有限责任公司 | Production process for isolating fluorine and chlorine by acid extraction during electrolytic zinc production |
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