CN108315763A - A method of preparing metallic zinc using ionic liquid electrolytic oxidation zinc - Google Patents
A method of preparing metallic zinc using ionic liquid electrolytic oxidation zinc Download PDFInfo
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- CN108315763A CN108315763A CN201810437866.7A CN201810437866A CN108315763A CN 108315763 A CN108315763 A CN 108315763A CN 201810437866 A CN201810437866 A CN 201810437866A CN 108315763 A CN108315763 A CN 108315763A
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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
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
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Abstract
The present invention relates to a kind of method preparing metallic zinc using ionic liquid electrolytic oxidation zinc, this method is using a substituted imidazole ion liquid dissolving zinc oxide as electrolyte；Using copper sheet or stainless steel as cathode, inert electrode prepares metal as anode, direct electrolytic oxidation object；Copper sheet or stainless steel substrates are taken out after electrolysis, obtain the metallic zinc for being deposited on surface.The present invention uses medium of the substituted imidazole ionic liquid as electrolytic preparation metallic zinc, 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 zinc 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 zinc 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 zinc using ionic liquid electrolytic oxidation zinc, belong to metallurgical technology neck
Domain.
Background technology
Solubility property (solubility and solution rate) of the zinc oxide usually in cryogenic media is poor, thus current zinc oxide
Electrolysis mainly carries out in high-temperature molten salt.Although high temperature fused salt electrolysis can realize that the large-scale production of metal, this method exist
A series of problems, such as electrolysis temperature is high, energy consumption is big, complicated for operation, discharge amount of exhaust gas is more.In energy shortage, the sternness of pollution aggravation
Under situation, how to realize that the energy-saving and emission-reduction of metal electrodeposition and green production are a problem to be solved.Therefore, a kind of energy is found
Enough the pollution-free low temperature green solvent of dissolving zinc oxide just shows particularly important.
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..Compared with other solvents, ionic liquid has many unique characteristics, such as nontoxic, steam
It forces down, thermal stability height, high, non-combustible, the electrochemical window mouth width of conductivity 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 at present also only using based on anhydrous AlCl3
It is electrolysed AlCl in the ionic liquid being mixed to prepare with chlorination 1- butyl -3- methylimidazoles3Metallic aluminium is prepared, also there are other gold
Belong to chloride based on AlCl3Respectively with chlorinated butyl pyridine, chlorination 1- ethyl-3-methylimidazoles, chlorination 1- butyl -3- methyl
The mixed liquor electro-deposition of the compositions such as imidazoles obtains the alloy of metal or metal and aluminium, but in utilization zinc chloride in gold, platinum, tungsten and glass
Electrodeposition process on carbon electrode as a result, it has been found that there is undercurrent potential phenomenon on metal electrode, and only has ternary on glass-carbon electrode
Nucleation process；What is obtained under overvoltage is the alloy of zinc and aluminium, can not prepare pure metallic zinc.It is organic in the reaction
Salt and AlCl3Relative mole content need stringent control, because of AlCl3In acidity when excessive；In alkalinity when organic salt excess；And
The variation of acid-base property will cause metal ion to generate different substances, such as Ag+It is bare ion under acidic environment, and in alkalinity
It is then combined with Cl- under environment, therefore usually need to make buffer with NaCl.The electrochemical window range of this class I liquid I is generally 2~
4V, but due to AlCl3Easily water suction thus can only use in dry conditions.When based on AlCl3Ionic liquid when being in neutrality,
Since alkyl imidazolium cation is weakly acidic, and paired anion is in then alkalescent, and the electrochemical window of this class I liquid I is logical
Often be higher than 4V, but shortcoming be its anion be easy and AlCl3Equal highly acids substance reacts, for example, PF6 -Meet AlCl3
Generate PF5Gas and fluorine chloro-aluminate, and meet water and partial hydrolysis then occurs and generates a certain amount of HF, have to body certain
Harmfulness, also pollute 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 zinc
The method for belonging to zinc, 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 zinc being prepared using ionic liquid electrolytic oxidation zinc, method includes the following steps：
The preparation of S1, electrolyte：Zinc oxide is added in the ionic liquid of heating, is uniformly mixed to form ionic liquid
Electrolyte；
S2, electrolytic preparation metallic zinc：Use copper sheet or stainless steel for cathode, inert electrode is 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 zinc 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.；An or aforementioned substitution
At least one of derivative of alkyl imidazolium 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 zinc 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, zinc 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 zinc 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：
The substituted imidazole ionic liquid that the present invention uses is to zinc oxide electrolytic preparation metal, a substituted imidazole ion
Liquid can be such that electrolytic process carries out at a lower temperature, and corrosion of the electrolyte to equipment is alleviated while energy saving, and
And the yield of metallic zinc is made to reach 99%；The ionic liquid price of use is relatively cheap, fusing point is low, can reduce production cost.This
The metal ion source used in invention is zinc oxide, and what is be precipitated on inert anode is oxygen, and there are no pollution to the environment.In addition,
The method of the present invention, process is simple, easy to operate.
Description of the drawings
Fig. 1 is the SEM figures of the metallic zinc prepared in the embodiment of the present invention 4；
Fig. 2 is the EDS figures of the metallic zinc prepared in the embodiment of the present invention 4；
Fig. 3 is the XRD diagram of the metallic zinc prepared in the embodiment of the present invention 4.
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, have been found when solvable at certain lower temperature to zinc oxide using a substituted imidazole ionic liquid
Solution, pure metallic zinc can be prepared by carrying out electro-deposition, and principle is to contain one in a substituted imidazole compound structure used
A amino (- NH) not replaced by alkyl, with certain activity, thus can react with zinc oxide and make zinc oxide
It is dissolved in ionic liquid.Ionic liquid dissolved with zinc oxide is electrolysed as electrolyte, preferably copper sheet or stainless steel
As cathode, inert electrode determines that under certain current potential, zinc ion can be reduced and be enriched with as anode, by a large number of experiments
On cathode, and the precipitated oxygen on inert anode, to prepare pure metallic zinc, and there are no pollution to the environment, electrolyte
It is also reusable, to cost-effective.It is low to solve zinc oxide solubility in cryogenic media simultaneously, it is difficult to electric at low temperature
Solve the problems such as zinc oxide obtains metal and existing method pollution environment.
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；It is with anion：F-、Cl-、Br-、I-、BF4 -、PF6 -、NO3 -、N(CN)2 -、CF3SO3 -、N
(CF3SO2)2 -Any one of or it is several when, when temperature is 90~100 DEG C, be used equally for dissolving zinc oxide, available incoming call
Solution prepares pure metallic zinc.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 zinc using ionic liquid low-temperature electrolytic zinc 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 ZnO, stirs
It mixes to be uniformly mixed and forms il electrolyte, and make zinc oxide a concentration of in 1- methylimidazole villiaumite ionic liquids
0.5mol/L；
(2) electrolytic preparation metal：Using copper sheet as cathode, for nickel sheet as anode, control electrolysis temperature is 120 DEG C, is adopted
With 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 zinc for being deposited on its surface after drying.
Embodiment 2
The method for preparing metallic zinc using ionic liquid low-temperature electrolytic zinc 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 ZnO, stirs
It mixes to be uniformly mixed and forms il electrolyte, wherein making a concentration of 1.0mol/L of zinc oxide；
(2) electrolytic preparation metallic zinc：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 zinc.
Embodiment 3
The method for preparing metallic zinc using ionic liquid low-temperature electrolytic zinc 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 ZnO,
It is uniformly mixed to form il electrolyte, wherein a concentration of 1.5mol/L of zinc oxide；
(2) electrolytic preparation metallic zinc：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 zinc for being deposited on its surface after drying.
Embodiment 4
The method for preparing metallic zinc using ionic liquid low-temperature electrolytic zinc 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 ZnO, stirs
It mixes to be uniformly mixed and forms il electrolyte, the wherein a concentration of 2.0mol/L of zinc oxide ZnO；
(2) electrolytic preparation metallic zinc：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 -0.8V, 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 zinc for being deposited on its surface after drying.
Embodiment 5
The method for preparing metallic zinc using ionic liquid low-temperature electrolytic zinc 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 ZnO, be uniformly mixed to form il electrolyte, wherein a concentration of 2.0mol/L of zinc oxide；
(2) electrolytic preparation metallic zinc：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 zinc for being deposited on its surface after drying.
In the above-described embodiments, ionic liquid purity >=99% of use, zinc oxide >=99%, cathode copper sheet purity >=
99.99%, when the copper sheet of cathode is replaced with stainless steel, can prepare corresponding metallic zinc, wherein the copper sheet of use and
Stainless 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
Piece and stainless steel surface are smooth, then are cleaned with EtOH Sonicate ripple, are 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.By embodiment 4 prepare metallic zinc for come illustrate the present invention prepare metal pattern and at
Point and purity.It is the SEM figures of prepared metallic zinc as shown in Figure 1, the smooth densification of zinc layers prepared as can be seen from Figure is such as schemed
2 show EDS (energy dispersion X-ray spectrum) figure of prepared metallic zinc, the results showed that the Zinc Deposit ingredient of preparation
Mainly Zn elements, and do not contain other impurity peaks；Illustrate that obtained Coating composition is single, purity is relatively high.As shown in Figure 3
For the XRD diagram of prepared metallic zinc, as a result illustrate that the coating prepared is that metallic zinc purity 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 zinc using ionic liquid electrolytic oxidation zinc, which is characterized in that its method includes following step
Suddenly：
The preparation of S1, electrolyte：Zinc oxide is added in the ionic liquid of heating, is uniformly mixed to form ionic liquid electrolysis
Liquid；
S2, electrolytic preparation metallic zinc：Use copper sheet or stainless steel for cathode, inert electrode is anode, in constant potential or constant current
Under, 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 zinc 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 zinc 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 metal 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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| CN201810437866.7A CN108315763A (en) | 2018-05-09 | 2018-05-09 | A method of preparing metallic zinc using ionic liquid electrolytic oxidation zinc |
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Cited By (5)
| 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 |
| CN110919023A (en) * | 2019-11-19 | 2020-03-27 | 吉林大学 | Method for preparing multi-dendritic platinum-based nano material by zinc ion induction |
| CN114959796A (en) * | 2022-05-18 | 2022-08-30 | 贵州省新材料研究开发基地 | Additive for electrolyzing metal manganese and application of additive in electrolyzing manganese |
| CN115491722A (en) * | 2022-09-22 | 2022-12-20 | 东北大学 | Method for preparing metal zinc at low temperature by using salt electrolyte in solvent |
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2018
- 2018-05-09 CN CN201810437866.7A patent/CN108315763A/en not_active Withdrawn
Cited By (6)
| 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 |
| CN110919023A (en) * | 2019-11-19 | 2020-03-27 | 吉林大学 | Method for preparing multi-dendritic platinum-based nano material by zinc ion induction |
| CN114959796A (en) * | 2022-05-18 | 2022-08-30 | 贵州省新材料研究开发基地 | Additive for electrolyzing metal manganese and application of additive in electrolyzing manganese |
| CN114959796B (en) * | 2022-05-18 | 2023-09-29 | 贵州省新材料研究开发基地 | Additive for electrolytic manganese metal and application of additive in electrolytic manganese |
| CN115491722A (en) * | 2022-09-22 | 2022-12-20 | 东北大学 | Method for preparing metal zinc at low temperature by using salt electrolyte in solvent |
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Application publication date: 20180724 |