CN109536994A - A kind of method that electrodeposition process prepares metallic lead - Google Patents
A kind of method that electrodeposition process prepares metallic lead Download PDFInfo
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- CN109536994A CN109536994A CN201910064363.4A CN201910064363A CN109536994A CN 109536994 A CN109536994 A CN 109536994A CN 201910064363 A CN201910064363 A CN 201910064363A CN 109536994 A CN109536994 A CN 109536994A
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- 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
- C25C1/18—Electrolytic production, recovery or refining of metals by electrolysis of solutions of lead
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Abstract
The invention belongs to a kind of methods that metallurgical technology field more particularly to electrodeposition process prepare metallic lead.Include the following steps: that 1.8~2.3:1 is mixed in molar ratio by urea and imidazolitm chloride, forms urea-imidazolitm chloride class ionic liquid；Lead oxide powder is added in urea-imidazolitm chloride class ionic liquid, stirring, lead oxide powder is dissolved in urea-imidazolitm chloride class ionic liquid and molar concentration is 0.07~0.08mol/L；It inserts electrodes into the urea-imidazolitm chloride class ionic liquid for dissolved lead oxide powder, carries out electro-deposition, wherein being electrodeposited in constant potential is -0.4~-1.0V vs.Ag, constant current density is 2~8mA/cm2Under conditions of carry out.This method is using lead oxide as raw material, and smelting process green is clean, no three wastes, and urea and imidazolitm chloride ionic liquid are mixed, and reduces production cost.
Description
Technical field
The invention belongs to a kind of methods that metallurgical technology field more particularly to electrodeposition process prepare metallic lead.
Background technique
Lead is the third-largest non-ferrous metal that yield is only second to aluminium and copper.Commercial lead smelting is divided into two steps of thick refining and refining
Suddenly, it includes lead concentrate desulfurization (galena-vulcanized lead is baked with agglomeration, and lead oxide is obtained), reduction melting (reductive coke oxygen that lead, which slightly refines,
Change lead, obtain lead bullion), the separation of slag lead and the processes such as lead bullion output, obtain leaded 95%~98% lead bullion.
However, lead bullion pyrometallurgical smelting process process is complicated, smelting temperature is up to 1250 DEG C, needs to consume a large amount of electric power and coal
Etc. energy resources, bring huge pressure to ecological environment.Contain more impurity in the lead bullion obtained by smelting reduction, need to lead to
It crosses pyro-refining or electrorefining and further purifies lead bullion, wherein electrorefining is containing H2SiF6And PbSiF6It is water-soluble
It is carried out in liquid, finally obtains leaded 99.9% or more lead bullion.Further, since the technical level of medium-sized and small enterprises is low, environmental consciousness
It is thin, lead waste water, exhaust gas and waste residue are discharged in violation of rules and regulations, and government regulation dynamics is inadequate in addition, and many lead contamination things still have occurred
Part.Therefore, the green energy conservation low consumption low-carbon metallurgical technology for developing lead, finding a kind of low-temperature electrolytes electrolytic preparation metallic lead has
Significance.
Aqueous solution electrodeposition lead is generally with Pb (NO3)2For solute, alkaline solution (such as NaOH solution) or nitrate,
Halide salt, acetate, methane sulfonates and borofluoride solution in carry out, but electrolytic process is difficult to avoid that analysis in aqueous solution
The generation of hydrogen side reaction, current efficiency is low, and the metallic lead that electro-deposition obtains on matrix and rough, is dendroid.It is related
There are many Research Literature report of ionic liquid electrodeposition metallic lead.For example, Wang et al. is with PbCl2For raw material, in 1- methyl -3-
Electro-deposition lead in butyl imidazolitm chloride-aluminium chloride；Katayama et al. is with Pb (TFSA)2For raw material, 25 DEG C of BMPTFSA from
Electro-deposition lead in sub- liquid；Tsai et al. is with TeCl4And PbCl2For raw material, in 1- ethyl -3- butyl imidazole tetrafluoroborate
Electro-deposition Te, Pb and PbTe alloy；Simons et al. is with Pb (NTf2)2For raw material, in 20 DEG C of [C2mim][NTf2] ionic liquid
Electro-deposition lead in body.Above-mentioned ionic liquid has tasteless non-ignitable, steam forces down, can operating temperature range wide (- 40~300 DEG C),
Electrochemical window mouth width (be greater than 3V), the advantages that thermal stability is good, the liberation of hydrogen that can occur to avoid aqueous solution electrodeposition lead is secondary anti-
It answers.
But the raw material that above-mentioned ionic liquid lead electro-deposition uses is PbCl2、Pb(TFSA)2With Pb (NTf2)2Deng cost
It is higher, and electrolytic process anode generates chlorine, needs to increase device for recovering tail gas.In addition, above-mentioned ionic liquid has water suction
Property, price costly, hinders its popularization and application industrially.
Summary of the invention
(1) technical problems to be solved
For existing technical problem, the present invention provides a kind of method that electrodeposition process prepares metallic lead, this method
It is middle that raw material is used as using lead oxide, electrolytic process anode generation oxygen, without increasing device for recovering tail gas, and by urea and chlorination
Imidazole ion liquid mixing, reduces production cost.
(2) technical solution
The present invention provides a kind of method that electrodeposition process prepares metallic lead, includes the following steps:
S1, by urea and imidazolitm chloride, 1.8~2.3:1 is mixed in molar ratio, forms urea-imidazolitm chloride class ionic liquid
Body；
The imidazolitm chloride includes the mixture of 1- ethyl -3- methylimidazolium chloride and 1- butyl -3- methylimidazolium chloride,
Wherein, 1- ethyl -3- methylimidazolium chloride and 1- butyl -3- methylimidazolium chloride molar ratio are 0.1~0.5:1；
S2, lead oxide powder is added in the urea-imidazolitm chloride class ionic liquid, is stirred, the lead oxide powder
Being dissolved in the molar concentration in urea-imidazolitm chloride class ionic liquid and in urea-imidazolitm chloride class ionic liquid is 0.07
~0.08mol/L；
S3, it inserts electrodes into the urea-imidazolitm chloride class ionic liquid for dissolved lead oxide powder, it is heavy to carry out electricity
Product, wherein the urea-imidazolitm chloride class ionic liquid temperature for having dissolved lead oxide powder is 100~140 DEG C, electro-deposition
It is -0.4~-1.0V vs.Ag in constant potential, constant current density is 2~8mA/cm2Under conditions of carry out.
Further, further includes: electrode, urea-imidazolitm chloride class of cleaning electrode surface adhesion are taken out after S4, electro-deposition
Ionic liquid obtains metallic lead in electrode surface after drying.
Further, in the step S2, lead oxide powder is added in the urea-imidazolitm chloride class ionic liquid,
Stir 4~12h.
Further, in the step S3, the time of electro-deposition is 0.1~1h.
Further, in the step S1, urea and imidazolitm chloride are mixed under an inert atmosphere.
Further, the step S2~S4 is carried out under air atmosphere.
Further, in the step S3, electrode includes working electrode, reference electrode and auxiliary electrode；
The working electrode is one of copper, tungsten, nickel, titanium, silver and stainless steel；
The reference electrode is Ag/AgCl；
The auxiliary electrode is one of tungsten, nickel, titanium, gold, silver, platinum and stainless steel.
(3) beneficial effect
The beneficial effects of the present invention are:
1, the raw material that the present invention uses is lead oxide, and electrode is inert metal, thus electrodeposition process anode is oxygen, yin
Extremely metallic lead, smelting process green is clean, and no three wastes meets low-carbon, low temperature, low energy consumption, short route, environmentally friendly green
The requirement of technique.
2, the method for the present invention is mixed by urea and imidazolitm chloride ionic liquid as electrolyte, and urea price is more just
Preferably, production cost is reduced, and the urea-imidazolitm chloride eutectic solvent formed is insensitive to water and air, does not need
The electro-deposition of lead is carried out in glove box.
3, imidazolitm chloride ionic liquid electrochemical window used in the present invention is wider (about 3V), can be to avoid in aqueous solution
The liberation of hydrogen side reaction that electro-deposition lead occurs, electrolytic process current efficiency is high, while electrolyte may be reused.
Detailed description of the invention
Fig. 1 is the XRD spectrum for the metallic lead that electro-deposition obtains in the embodiment of the present invention 1；
Fig. 2 is the SEM spectrum for the metallic lead that electro-deposition obtains in the embodiment of the present invention 1；
Fig. 3 is the EDS map for the metallic lead that electro-deposition obtains in the embodiment of the present invention 1.
Specific embodiment
In order to preferably explain the present invention, in order to understand, with reference to the accompanying drawing, by specific embodiment, to this hair
It is bright to be described in detail.
Embodiment 1
S1, at room temperature, by urea and imidazolitm chloride, 1.8:1 is mixed in molar ratio, controls 100 DEG C of temperature, after agitated
Form colourless as clear as crystal urea-imidazolitm chloride class ionic liquid (i.e. electrolyte).Wherein, imidazolitm chloride is by molar ratio
1- ethyl -3- the methylimidazolium chloride of 0.5:1 and 1 butyl -3- methylimidazolium chloride mix.
S2, lead oxide solid powder is added in urea-imidazolitm chloride class ionic liquid, stirs 4h, makes lead oxide solid
Powder is dissolved completely in urea-imidazolitm chloride class ionic liquid, and lead oxide is in urea-imidazolitm chloride class ionic liquid
Molar concentration is 0.07mol/L.
S3, will be using copper as working electrode, Ag/AgCl is reference electrode, and titanium is that the electrode of auxiliary electrode is inserted and contains lead oxide
Electrolyte in, control the electrolyte containing lead oxide temperature be 100 DEG C, under the conditions of constant potential -0.4V (vs.Ag) into
Row electro-deposition 0.1h.
Electrode is taken out after S4, electro-deposition, with a small amount of electrolyte of acetone and distilled water cleaning electrode surface adhesion, after dry
Metallic lead is obtained on copper surface.
As shown in Figure 1, 2, 3, respectively XRD, SEM and EDS map of metallic lead obtained in the present embodiment.
The current efficiency of the present embodiment electrodeposit metals lead process is 96.17%, energy consumption 0.11kWh/kg-Pb.
Embodiment 2
S1, at room temperature, by urea and 1- methyl -3- methylimidazolium chloride ionic liquid, 2:1 is mixed in molar ratio, control
150 DEG C of temperature, it is (i.e. electric that colourless as clear as crystal urea -1- methyl -3- methylimidazolium chloride class ionic liquid is formed after agitated
Solve matter).
S2, lead oxide solid powder is added in urea -1- methyl -3- methylimidazolium chloride class ionic liquid, stirring
12h is dissolved completely in lead oxide solid powder in urea -1- methyl -3- methylimidazolium chloride class ionic liquid, and lead oxide
Molar concentration in urea -1- methyl -3- methylimidazolium chloride class ionic liquid is 0.08mol/L.
S3, will be using stainless steel as working electrode, Ag/AgCl is reference electrode, and nickel is that the electrode of auxiliary electrode is inserted containing aerobic
In the electrolyte for changing lead, the temperature of electrolyte of the control containing lead oxide is 140 DEG C, in constant potential -1.0V (vs.Ag) condition
Lower progress electro-deposition 1h.
Electrode is taken out after S4, electro-deposition, with a small amount of electrolyte of acetone and distilled water cleaning electrode surface adhesion, after dry
Metallic lead is obtained in stainless steel surface.
The current efficiency of the present embodiment electrodeposit metals lead process is 67.2%, energy consumption 0.57kWh/kg-Pb.
Embodiment 3
S1, at room temperature, by urea and 1- ethyl -3- methylimidazolium chloride ionic liquid, 2.3:1 is mixed in molar ratio, control
130 DEG C of temperature processed, colourless as clear as crystal urea -1- ethyl -3- methylimidazolium chloride class ionic liquid is formed (i.e. after agitated
Electrolyte).
S2, lead oxide solid powder is added in urea -1- ethyl -3- methylimidazolium chloride class ionic liquid, stirs 6h,
It is dissolved completely in lead oxide solid powder in urea -1- ethyl -3- methylimidazolium chloride class ionic liquid, and lead oxide is being urinated
Molar concentration in element -1- ethyl -3- methylimidazolium chloride class ionic liquid is 0.072mol/L.
S3, will be using nickel as working electrode, Ag/AgCl is reference electrode, and stainless steel is that the electrode of auxiliary electrode is inserted containing aerobic
In the electrolyte for changing lead, the temperature of electrolyte of the control containing lead oxide is 110 DEG C, in constant potential -0.6V (vs.Ag) condition
Lower progress electro-deposition 0.5h.
Electrode is taken out after S4, electro-deposition, with a small amount of electrolyte of acetone and distilled water cleaning electrode surface adhesion, after dry
Metallic lead is obtained in nickel surface.
The current efficiency of the present embodiment electrodeposit metals lead process is 83.52%, energy consumption 0.22kWh/kg-Pb.
Embodiment 4
S1, at room temperature, by urea and 1- propyl -3- methylimidazolium chloride ionic liquid, 2.2:1 is mixed in molar ratio, control
110 DEG C of temperature processed, colourless as clear as crystal urea -1- propyl -3- methylimidazolium chloride class ionic liquid is formed (i.e. after agitated
Electrolyte).
S2, lead oxide solid powder is added in urea -1- propyl -3- methylimidazolium chloride class ionic liquid, stirs 5h,
It is dissolved completely in lead oxide solid powder in urea -1- propyl -3- methylimidazolium chloride class ionic liquid, and lead oxide is being urinated
Molar concentration in element -1- propyl -3- methylimidazolium chloride class ionic liquid is 0.075mol/L.
S3, will be using titanium as working electrode, Ag/AgCl is reference electrode, and tungsten is that the electrode of auxiliary electrode is inserted and contains lead oxide
Electrolyte in, control the electrolyte containing lead oxide temperature be 120 DEG C, under the conditions of constant potential -0.8V (vs.Ag) into
Row electro-deposition 0.8h.
Electrode is taken out after S4, electro-deposition, with a small amount of electrolyte of acetone and distilled water cleaning electrode surface adhesion, after dry
Metallic lead is obtained on titanium surface.
The current efficiency of the present embodiment electrodeposit metals lead process is 75.29%, energy consumption 0.37kWh/kg-Pb.
Embodiment 5
S1, at room temperature, by urea and 1- amyl -3- methylimidazolium chloride ionic liquid, 2:1 is mixed in molar ratio, control
80 DEG C of temperature, it is (i.e. electric that colourless as clear as crystal urea -1- amyl -3- methylimidazolium chloride class ionic liquid is formed after agitated
Solve matter).
S2, lead oxide solid powder is added in urea -1- amyl -3- methylimidazolium chloride class ionic liquid, stirring
10h is dissolved completely in lead oxide solid powder in urea -1- amyl -3- methylimidazolium chloride class ionic liquid, and lead oxide
Molar concentration in urea -1- amyl -3- methylimidazolium chloride class ionic liquid is 0.078mol/L.
S3, will be using tungsten as working electrode, Ag/AgCl is reference electrode, silver be auxiliary electrode electrode insert contains lead oxide
Electrolyte in, control the electrolyte containing lead oxide temperature be 130 DEG C, in constant current density 2mA/cm2Under the conditions of into
Row electro-deposition 0.6h.
Electrode is taken out after S4, electro-deposition, with a small amount of electrolyte of acetone and distilled water cleaning electrode surface adhesion, after dry
Metallic lead is obtained on tungsten surface.
The current efficiency of the present embodiment electrodeposit metals lead process is 77.32%, energy consumption 0.22kWh/kg-Pb.
Embodiment 6
S1, at room temperature, by urea and 1- amyl -3- methylimidazolium chloride ionic liquid, 2:1 is mixed in molar ratio, control
110 DEG C of temperature, it is (i.e. electric that colourless as clear as crystal urea -1- amyl -3- methylimidazolium chloride class ionic liquid is formed after agitated
Solve matter).
S2, lead oxide solid powder is added in urea -1- amyl -3- methylimidazolium chloride class ionic liquid, stirs 7h,
It is dissolved completely in lead oxide solid powder in urea -1- amyl -3- methylimidazolium chloride class ionic liquid, and lead oxide is being urinated
Molar concentration in element -1- amyl -3- methylimidazolium chloride class ionic liquid is 0.08mol/L.
S3, will be using copper as working electrode, Ag/AgCl is reference electrode, and platinum is that the electrode of auxiliary electrode is inserted and contains lead oxide
Electrolyte in, control the electrolyte containing lead oxide temperature be 100 DEG C, in constant current density 8mA/cm2Under the conditions of into
Row electro-deposition 0.3h.
Electrode is taken out after S4, electro-deposition, with a small amount of electrolyte of acetone and distilled water cleaning electrode surface adhesion, after dry
Metallic lead is obtained on copper surface.
In above-described embodiment 1~6, the preparation of urea-imidazolitm chloride class ionic liquid is being full of argon in the step S1
It is carried out in the glove box of gas, wherein the content of oxygen and water is lower than 0.1ppm, and the step S2~S4 is carried out under air atmosphere.
Urea-imidazolitm chloride class ionic liquid after electro-deposition can be recycled.Anode in electrodeposition process produces
Object is oxygen, and cathode product is metallic lead, and smelting process green is clean, and no three wastes meets low-carbon, low temperature, low energy consumption, short stream
The requirement of journey, environmentally friendly friendly process.
The technical principle of the invention is described above in combination with a specific embodiment, these descriptions are intended merely to explain of the invention
Principle shall not be construed in any way as a limitation of the scope of protection of the invention.Based on explaining herein, those skilled in the art
It can associate with other specific embodiments of the invention without creative labor, these modes fall within this hair
Within bright protection scope.
Claims (6)
1. a kind of method that electrodeposition process prepares metallic lead, which comprises the steps of:
S1, by urea and imidazolitm chloride, 1.8~2.3:1 is mixed in molar ratio, forms urea-imidazolitm chloride class ionic liquid, institute
State the mixture that imidazolitm chloride includes 1- ethyl -3- methylimidazolium chloride and 1- butyl -3- methylimidazolium chloride, wherein 1- second
Base -3- methylimidazolium chloride and 1- butyl -3- methylimidazolium chloride molar ratio are 0.1~0.5:1；
S2, lead oxide powder is added in the urea-imidazolitm chloride class ionic liquid, is stirred, the lead oxide powder dissolution
Molar concentration in urea-imidazolitm chloride class ionic liquid and in urea-imidazolitm chloride class ionic liquid is 0.07~
0.08mol/L；
S3, it inserts electrodes into the urea-imidazolitm chloride class ionic liquid for dissolved lead oxide powder, carries out electro-deposition,
Wherein, the urea-imidazolitm chloride class ionic liquid temperature for having dissolved lead oxide powder is 100~140 DEG C, is electrodeposited in perseverance
Determining current potential is -0.4~-1.0V vs.Ag, and constant current density is 2~8mA/cm2Under conditions of carry out.
2. the method that electrodeposition process according to claim 1 prepares metallic lead, which is characterized in that further include:
Electrode, urea-imidazolitm chloride class ionic liquid of cleaning electrode surface adhesion, in electricity after drying are taken out after S4, electro-deposition
Pole surface obtains metallic lead.
3. the method that electrodeposition process according to claim 1 prepares metallic lead, which is characterized in that, will in the step S2
Lead oxide powder is added in the urea-imidazolitm chloride class ionic liquid, stirs 4~12h.
4. the method that electrodeposition process according to claim 1 prepares metallic lead, which is characterized in that in the step S3, electricity
The time of deposition is 0.1~1h.
5. the method that electrodeposition process according to claim 1 prepares metallic lead, which is characterized in that in the step S1,
Urea and imidazolitm chloride are mixed under inert atmosphere.
6. the method that electrodeposition process according to claim 2 prepares metallic lead, which is characterized in that the step S2~S4 exists
It is carried out under air atmosphere.
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Cited By (1)
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| CN110629253A (en) * | 2019-09-29 | 2019-12-31 | 昆明理工大学 | Method for electrorefining lead bullion by using ionic liquid and method for recovering metal bismuth and silver |
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| CN108315763A (en) * | 2018-05-09 | 2018-07-24 | 东北大学 | A method of preparing metallic zinc using ionic liquid electrolytic oxidation zinc |
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Application publication date: 20190329 |