CN108611664A - A method of preparing metallic lead using ionic liquid electrolytic oxidation lead - Google Patents
A method of preparing metallic lead using ionic liquid electrolytic oxidation lead Download PDFInfo
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- CN108611664A CN108611664A CN201810437781.9A CN201810437781A CN108611664A CN 108611664 A CN108611664 A CN 108611664A CN 201810437781 A CN201810437781 A CN 201810437781A CN 108611664 A CN108611664 A CN 108611664A
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- lead
- ionic liquid
- copper sheet
- stainless steel
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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
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/34—Electrolytic production, recovery or refining of metals by electrolysis of melts of metals not provided for in groups C25C3/02 - C25C3/32
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Abstract
The present invention relates to a kind of method preparing metallic lead using ionic liquid electrolytic oxidation lead, this method is using a substituted imidazole ion liquid dissolving lead oxide as electrolyte；Using copper sheet or stainless steel as cathode, inert electrode is anode, and direct electrolytic oxidation lead prepares metallic lead；Copper sheet or stainless steel substrates are taken out after electrolysis, obtain the metallic lead for being deposited on surface.The present invention uses medium of the substituted imidazole ionic liquid as electrolytic preparation metal, and electrolytic process can be made to carry out at a lower temperature, corrosion of the electrolyte to equipment is alleviated while energy saving, and the yield of metallic lead is made to reach 99%；The ionic liquid price of use is relatively cheap, fusing point is low, can reduce production cost；The metal ion source used is lead oxide, and what is be precipitated on inert anode is oxygen, and there are no pollution to the environment.In addition, the method for the present invention process is simple, it is easy to operate.
Description
Technical field
The present invention relates to a kind of methods preparing metallic lead using ionic liquid electrolytic oxidation lead, belong to metallurgical technology neck
Domain.
Background technology
Solubility property (solubility and solution rate) of the metal oxide usually in cryogenic media is poor, thus current metal
The electrolysis of oxide mainly carries out in high-temperature molten salt.It, should although high temperature fused salt electrolysis can realize the large-scale production of metal
Method there are electrolysis temperatures it is high, energy consumption is big, complicated for operation, discharge amount of exhaust gas is more a series of problems, such as.Add in energy shortage, pollution
Under acute severe situation, how to realize that the energy-saving and emission-reduction of metal electrodeposition and green production are a problem to be solved.Therefore, it looks for
Just show particularly important to a kind of pollution-free low temperature green solvent of metal oxide that can dissolve.
Ionic liquid, refer to room temperature or close at room temperature present liquid, completely by organic cation and inorganic the moon
From molecular liquid substance, also referred to as room temperature molten salt.Ionic liquid is lower melting-point main as ionic compound
The reason is that because the asymmetry of certain substituent groups in its structure prevent ion from being regularly piled into crystal caused by.Common sun from
Son has quaternary ammonium salt ion, quaternary phosphine salt ion, imidazolium ion and pyrroles's salt ion etc., and anion has halide ion, tetrafluoro boric acid
Radical ion, hexafluorophosphoricacid acid ions etc..
Ionic liquid is a kind of ideal room temperature fused salt, has the advantages that high-temperature molten salt and organic solvent, is at room temperature
The metal and its alloy that ability electro-deposition obtains in high-temperature molten salt can be obtained, but be only based at present using lead chloride anhydrous
AlCl3Electrolytic chlorination lead prepares metallic lead in the ionic liquid being mixed to prepare with chlorination 1- butyl -3- methylimidazoles, but
Organic salt and AlCl in reaction3Relative mole content need stringent control, because of AlCl3In acidity when excessive；When organic salt excess
In alkalinity；And the variation of acid-base property will cause metal ion to generate different substances, and be chlorine in anode precipitation, to the person
Body has certain harmfulness, and can generate pollution to environment.
Invention content
(1) technical problems to be solved
In order to solve the above problem of the prior art, the present invention provides a kind of golden using the preparation of ionic liquid electrolytic oxidation lead
The method for belonging to lead, and carries out at a lower temperature, energy saving, alleviate equipment corrosion and easily operated, while on anode
What is be precipitated is oxygen, environmentally safe.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include：
A method of metallic lead being prepared using ionic liquid electrolytic oxidation lead, method includes the following steps：
The preparation of S1, electrolyte：Lead oxide is added in the ionic liquid of heating, is uniformly mixed to form ionic liquid
Electrolyte；
S2, electrolytic preparation metal：Using copper sheet or stainless steel as cathode, inert electrode as anode, in constant potential or
Under constant current, electro-deposition is carried out to il electrolyte described in step S1；
The copper sheet or stainless steel substrates are taken out after S3, electrolysis, obtain the metal for being deposited on its surface.
Method as described above, it is preferable that in step sl, the ionic liquid is a substituted imidazole ionic liquid,
Wherein, cation can be selected from：1- methylimidazoles, 1- ethyl imidazol(e)s, 1- propyl imidazoles, 1- butyl imidazoles, 1- amyls imidazoles, 1- oneself
At least one of base imidazoles, 1- heptyl imidazoles, 1- octylimidazoles, 1- nonyls imidazoles, 1- decyl imidazoles etc.；Or aforementioned substitution miaow
At least one of the derivative of azole cation；
It can be selected from anion：F-、Cl-、Br-、I-、BF4 -、PF6 -、NO3 -、N(CN)2 -、CF3SO3 -、N(CF3SO2)2 -In
It is at least one.
Method as described above, it is preferable that in step sl, the temperature of the heating is 90~100 DEG C, the stirring
Speed is 300~700r/min.
Method as described above, it is preferable that in step sl, the lead oxide in ionic liquid a concentration of 0.5~
3mol/L。
Method as described above, it is preferable that in step s 2, current potential is -0.4~-1.0V, institute to the constant potential in order to control
Stating constant current, cathode-current density is 0.01~0.04A/cm in order to control2。
Method as described above, it is preferable that in step s 2, the temperature for controlling electrolysis is 90~120 DEG C.
When electrolysis temperature is controlled at 90~120 DEG C, lead oxide can be made to be dissolved completely in ionic liquid, reaction is made to fill
Point.
Method as described above, it is preferable that in step s 2, the inert electrode is nickel, titanium, platinum, gold or other inertia
Metal electrode.
Method as described above, it is preferable that in step s 2, the time of the electro-deposition is 1~4h.
Method as described above, it is preferable that in step s3, the copper sheet or stainless steel substrates are cleaned simultaneously with second alcohol and water
The metallic lead for being deposited on its surface is obtained after drying.
Method as described above, it is preferable that in step s 2, the copper sheet or stainless steel need to carry out pre-treatment：Using
Sand paper polishes to the surface of copper sheet or stainless steel, keeps copper sheet and stainless steel surface smooth, then cleaned with EtOH Sonicate ripple, so
It is cleaned with deionized water, is used after finally drying afterwards.
(3) advantageous effect
The beneficial effects of the invention are as follows：
After the substituted imidazole ion liquid dissolving lead oxide that the present invention uses electrolytic preparation gold is carried out as electrolyte
Belong to lead, a substituted imidazole ionic liquid used can be such that electrolytic process carries out at a lower temperature, while energy saving
Corrosion of the electrolyte to equipment is alleviated, and the yield of metallic lead is made to reach 99%；The ionic liquid price of use is relatively just
Preferably, fusing point is low, and reusable, can reduce production cost.The metal ion source used in the present invention is lead oxide, in inertia
What is be precipitated on anode is oxygen, and there are no pollution to the environment.In addition, the method for the present invention process is simple, it is easy to operate.
Description of the drawings
Fig. 1 is the SEM figures of the metallic lead prepared in the embodiment of the present invention 5；
Fig. 2 is the EDS figures of the metallic lead prepared in the embodiment of the present invention 5；
Fig. 3 is the XRD diagram of the metallic lead prepared in the embodiment of the present invention 5.
Specific implementation mode
The present invention, which is directed to while how improving metal quality, eliminates harm of the electrodeposit liquid to environment, in ionic liquid
Numerous studies have been carried out, discovery is worked as can dissolve lead oxide using a substituted imidazole ionic liquid at a certain temperature, into
One step, pure metallic lead can be prepared by carrying out electro-deposition, and principle is contained in a substituted imidazole compound structure used
One amino (- NH) not replaced by alkyl, with certain activity, thus can react with lead oxide and make oxidation
Lead is dissolved in ionic liquid.Ionic liquid dissolved with lead oxide is electrolysed as electrolyte, preferably copper sheet or stainless
Steel determines that under certain current potential, metal ion can be reduced simultaneously as cathode, inert electrode as anode, by a large number of experiments
It is enriched on cathode, and the precipitated oxygen on inert anode, to prepare pure metal, and there are no pollution to the environment, electrolysis
Liquid is also reusable, to cost-effective.It is low that the present invention solves lead oxide solubility in cryogenic media simultaneously, it is difficult to
The problem of electrolytic oxidation lead obtains metallic lead and pollutes environment in the prior art under low temperature.
Ionic liquid used in the present invention is a substituted imidazole ionic liquid, wherein cation uses：1- methyl miaows
Azoles, 1- ethyl imidazol(e)s, 1- propyl imidazoles, 1- butyl imidazoles, 1- amyls imidazoles, 1- hexyl imidazoliums, 1- heptyl imidazoles, 1- octyl miaows
Any one or a few in azoles, 1- nonyls imidazoles, 1- decyl imidazoles etc., which mixes, or a substituted imidazole noted earlier is cationic spreads out
Any one or a few in biology；Anion can be used：F-、Cl-、Br-、I-、BF4 -、PF6 -、NO3-、N(CN)2-、CF3SO3-、
N(CF3SO2)2 -In any one or a few when, when temperature is 90~100 DEG C, be used equally for dissolving lead oxide, it is available
Carry out the pure metallic lead of electrolytic preparation.Wherein, a substituted imidazole ionic liquid can pass through acquisition purchased in market.
In order to preferably explain the present invention, in order to understand, below in conjunction with the accompanying drawings, by specific implementation mode, to this hair
It is bright to be described in detail.
Embodiment 1
The method for preparing metallic lead using ionic liquid low-temperature electrolytic lead oxide is carried out according to following processing step：
(1) preparation of electrolyte：The 1- methylimidazole villiaumite ionic liquids of appropriate mass are weighed, cation therein is 1-
Methylimidazole, anion F-, control heating temperature is 100 DEG C, and mixing speed 300r/min is then slowly added to PbO, stirs
It mixes to be uniformly mixed and forms il electrolyte, and make PbO a concentration of in 1- methylimidazole villiaumite ionic liquids
0.5mol/L；
(2) electrolytic preparation metallic lead：Using copper sheet as cathode, nickel sheet is 120 DEG C as anode, control electrolysis temperature,
Using constant potential mode, controlling potential is -1.0V, the electro-deposition 1h in the electrolyte of step (1)；
(3) copper sheet is taken out after being electrolysed, cleaned with second alcohol and water and obtains the metallic lead for being deposited on its surface after drying.
Embodiment 2
The method for preparing metallic lead using ionic liquid low-temperature electrolytic lead oxide is carried out according to following processing step：
(1) preparation of electrolyte：The 1- ethyl imidazol(e) chloride salt ions liquid of appropriate mass is weighed, cation therein is 1-
Ethyl imidazol(e), anion Cl-, control heating temperature is 90 DEG C, and mixing speed 400r/min is then slowly added to PbO, stirs
It mixes to be uniformly mixed and forms il electrolyte, wherein making a concentration of 1.0mol/L of PbO；
(2) electrolytic preparation metallic lead：Using stainless steel as cathode, titanium sheet is 110 as anode, control electrolysis temperature
DEG C, using constant current mode, control current density is 0.01A/cm2, the electro-deposition 2h in the electrolyte of step (1)；
(3) stainless steel substrates are taken out after being electrolysed, cleaned with second alcohol and water and obtain the gold for being deposited on its surface after drying
Belong to lead.
Embodiment 3
The method for preparing metallic lead using ionic liquid low-temperature electrolytic lead oxide is carried out according to following processing step：
(1) preparation of electrolyte：The 1- propyl imidazole bromide ionic liquids of appropriate mass are weighed, cation therein is 1-
Propyl imidazole, anion Br-, control heating temperature is 100 DEG C, and mixing speed 500r/min is then slowly added to PbO,
It is uniformly mixed to form il electrolyte, a concentration of 1.5mol/L of wherein PbO；
(2) electrolytic preparation metallic lead：Using copper sheet as cathode, platinized platinum is 100 DEG C as anode, control electrolysis temperature,
Using constant potential mode, controlling potential is -0.9V, the electro-deposition 3h in the electrolyte of step (1)；
(3) copper sheet is taken out after being electrolysed, cleaned with second alcohol and water and obtains the metallic lead for being deposited on its surface after drying.
Embodiment 4
The method for preparing metallic lead using ionic liquid low-temperature electrolytic lead oxide is carried out according to following processing step：
(1) preparation of electrolyte：The 1- butyl imidazole metal iodide ions liquid of appropriate mass is weighed, cation therein is 1-
Butyl imidazole, anion I-, control heating temperature is 100 DEG C, and mixing speed 600r/min is then slowly added to PbO, stirs
It mixes to be uniformly mixed and forms il electrolyte, a concentration of 2.0mol/L of wherein PbO；
(2) electrolytic preparation metal：Using copper sheet as cathode, platinized platinum is 90 DEG C as anode, control electrolysis temperature, is used
Constant potential mode, controlling potential are -0.8V, the electro-deposition 2h in the electrolyte of step (1)；
(3) copper sheet is taken out after being electrolysed, cleaned with second alcohol and water and obtains the metallic lead for being deposited on its surface after drying.
Embodiment 5
The method for preparing metallic lead using ionic liquid low-temperature electrolytic lead oxide is carried out according to following processing step：
(1) preparation of electrolyte：Weigh the 1- amyl tetrafluoroborate ionic liquids of appropriate mass, sun therein from
Son is 1- amyl imidazoles, anion BF4 -, control heating temperature is 100 DEG C, mixing speed 700r/min, is then slowly added
Enter PbO, is uniformly mixed to form il electrolyte, a concentration of 2.0mol/L of wherein PbO；
(2) electrolytic preparation metallic lead：Using copper sheet as cathode, for platinized platinum as anode, control electrolysis temperature is 90 DEG C, is adopted
With constant potential mode, controlling potential is -0.4V, the electro-deposition 2h in the electrolyte of step (1)；
(3) copper sheet is taken out after being electrolysed, cleaned with second alcohol and water and obtains the metallic lead for being deposited on its surface after drying.
In the above-described embodiments, ionic liquid purity >=99% of use, lead oxide >=99%, cathode copper sheet purity >=
99.99%, when the copper sheet of cathode is replaced with stainless steel, it can prepare corresponding metal, wherein the copper sheet of use and not
Rust steel is needed before use by following processing procedure：It is polished copper sheet and stainless steel surface using different model sand paper, makes copper sheet
It is smooth with stainless steel surface, then cleaned with EtOH Sonicate ripple, it is then cleaned with deionized water, last drying for standby.
In in embodiments the step of (1), ZNCL-BS type intelligent digital magnetic force heating plates can be used and heated,
In step (2), 30 type potentiostats of AUTOLAB PGSTAT can be used and be electrolysed.And the metal to being prepared in each embodiment
The pattern and ingredient that metal is analyzed using Japanese Shimadzu SSX-550 types scanning electron microscope (SEM), using the subsidiary energy of SEM
Chromatic dispersion quantity X-ray spectrum (EDS) analyzes the chemical composition of metal, using Dutch Panaco MPDDY2094 type X-ray diffractometers
(XRD) product object phase composition is analyzed.Illustrate that the present invention prepares the pattern of metallic lead and pure by taking metallic lead prepared by embodiment 5 as an example
Degree.
It is the smooth densification of lead layer that the SEM of prepared metallic lead schemes, prepares as can be seen from Figure as shown in Figure 1；Fig. 2 institutes
The EDS figures of prepared metallic lead are shown as, illustrate the smooth densification of lead layer, the lead-coat surface composition of preparation is mainly Pb elements,
And other impurity peaks are not contained；It is illustrated in figure 3 the XRD diagram of prepared metallic lead, illustrates that the coating prepared is metallic lead, it is pure
Degree is high, up to 99%.
The above described is only a preferred embodiment of the present invention, being not the limitation for doing other forms to the present invention, appoint
What those skilled in the art can be changed or be modified as the equivalence enforcement of equivalent variations using technology contents disclosed above
Example.But it is every without departing from technical solution of the present invention content, according to the technical essence of the invention to appointing made by above example
What simple modification, equivalent variations and remodeling, still falls within the protection domain of technical solution of the present invention.
Claims (10)
1. a kind of method preparing metallic lead using ionic liquid electrolytic oxidation lead, which is characterized in that its method includes following step
Suddenly：
The preparation of S1, electrolyte：Lead oxide is added in the ionic liquid of heating, is uniformly mixed to form ionic liquid electrolysis
Liquid；
S2, electrolytic preparation metallic lead：Using copper sheet or stainless steel as cathode, inert electrode is as anode, in constant potential or perseverance
Under electric current, electro-deposition is carried out to il electrolyte described in step S1；
The copper sheet or stainless steel substrates are taken out after S3, electrolysis, obtain the metallic lead for being deposited on its surface.
2. the method as described in claim 1, which is characterized in that in step sl, the ionic liquid is a substituted imidazole
Ionic liquid, wherein cation is selected from：1- methylimidazoles, 1- ethyl imidazol(e)s, 1- propyl imidazoles, 1- butyl imidazoles, 1- amyl miaows
At least one of azoles, 1- hexyl imidazoliums, 1- heptyl imidazoles, 1- octylimidazoles, 1- nonyls imidazoles, 1- decyl imidazoles；Or it is aforementioned
At least one of the derivative of one substituted imidazole cationoid；
It is selected from anion：F-、Cl-、Br-、I-、BF4 -、PF6 -、NO3 -、N(CN)2 -、CF3SO3 -Or N (CF3SO2)2 -In at least one
Kind.
3. the method as described in claim 1, which is characterized in that in step sl, the temperature of the heating is 90~100 DEG C,
The speed of the stirring is 300~700r/min.
4. the method as described in claim 1, which is characterized in that in step sl, the lead oxide is dense in ionic liquid
Degree is 0.5~3mol/L.
5. the method as described in claim 1, which is characterized in that in step s 2, current potential is -0.4 to the constant potential in order to control
~-1.0V, cathode-current density is 0.01~0.04A/cm to the constant current in order to control2。
6. the method as described in claim 1, which is characterized in that in step s 2, the temperature for controlling electrolysis is 90~120 DEG C.
7. the method as described in claim 1, which is characterized in that in step s 2, the inert electrode is nickel, titanium, platinum or gold.
8. the method as described in claim 1, which is characterized in that in step s 2, the time of the electro-deposition is 1~4h.
9. the method as described in claim 1, which is characterized in that in step s3, to the copper sheet or stainless steel substrates ethyl alcohol
It is cleaned with water and obtains the metallic lead for being deposited on its surface after drying.
10. method as claimed in any one of claims 1-9 wherein, which is characterized in that in step s 2, the copper sheet or stainless steel
It needs to carry out pre-treatment：It is polished the surface of copper sheet or stainless steel using sand paper, keeps copper sheet and stainless steel surface smooth, then
It is cleaned with EtOH Sonicate ripple, is then cleaned with deionized water, used after finally drying.
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| CN201810437781.9A CN108611664A (en) | 2018-05-09 | 2018-05-09 | A method of preparing metallic lead using ionic liquid electrolytic oxidation lead |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109536993A (en) * | 2019-01-23 | 2019-03-29 | 东北大学 | A kind of method of electrodeposit metals zinc in eutectic solvent |
| CN109536994A (en) * | 2019-01-23 | 2019-03-29 | 东北大学 | A kind of method that electrodeposition process prepares metallic lead |
| CN110860294A (en) * | 2019-11-27 | 2020-03-06 | 河北科技大学 | Preparation method of copper-lead composite metal catalyst and application of copper-lead composite metal catalyst |
-
2018
- 2018-05-09 CN CN201810437781.9A patent/CN108611664A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109536993A (en) * | 2019-01-23 | 2019-03-29 | 东北大学 | A kind of method of electrodeposit metals zinc in eutectic solvent |
| CN109536994A (en) * | 2019-01-23 | 2019-03-29 | 东北大学 | A kind of method that electrodeposition process prepares metallic lead |
| CN110860294A (en) * | 2019-11-27 | 2020-03-06 | 河北科技大学 | Preparation method of copper-lead composite metal catalyst and application of copper-lead composite metal catalyst |
| CN110860294B (en) * | 2019-11-27 | 2022-10-25 | 河北科技大学 | Method for preparing formic acid by electrochemical reduction reaction of carbon dioxide by using copper-lead composite metal as electrode |
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