CN103031571A - Method for electrodepositing gallium at low temperature by using ionic liquid - Google Patents
Method for electrodepositing gallium at low temperature by using ionic liquid Download PDFInfo
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- CN103031571A CN103031571A CN2012105396805A CN201210539680A CN103031571A CN 103031571 A CN103031571 A CN 103031571A CN 2012105396805 A CN2012105396805 A CN 2012105396805A CN 201210539680 A CN201210539680 A CN 201210539680A CN 103031571 A CN103031571 A CN 103031571A
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Abstract
The invention relates to a method for electrodepositing gallium at low temperature by using an ionic liquid, which comprises the following steps: heating an ionic liquid used as an electrolyte to a colorless transparent state, dissolving gallium chloride in the ionic liquid, and electrodepositing the gallium chloride in the solution, wherein gallium is generated at the cathode of the electrolytic bath, and chlorine gas is emitted at the anode. In the electrodeposition process, the bath voltage of the electrolytic bath is higher than the decomposition voltage of gallium chloride, and lower than that of the electrochemical window of the ionic liquid. The invention has the advantages of low operating temperature, low energy consumption and low apparatus corrosiveness, can greatly lower the production cost, and is environment-friendly.
Description
Technical field
The invention belongs to the chemical field of metallurgy, be specifically related to a kind of method of utilizing ionic liquid low temp. electric deposition gallium.
Background of invention
At present, the industrial electro deposition is produced some problems that gallium exists, the problems such as such as high energy consumption,, etching apparatus unfriendly to environment, cost is large, contaminate environment.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, proposed a kind of method of utilizing ionic liquid low temp. electric deposition gallium.
In order to reach above-mentioned technical purpose, the technical solution used in the present invention is: ionic liquid is heated to the water white transparency state, then gallium chloride is dissolved in the ionic liquid, form gallium chloride solution; Again gallium chloride solution is carried out galvanic deposit, generate gallium on the negative electrode of electrolyzer, emit chlorine on the anode; Wherein, in the electrodeposition process, the bath voltage of electrolyzer is higher than the gallium chloride decomposition voltage, and the bath voltage of electrolyzer is lower than the electrochemical window of ionic liquid.
Described ionic liquid is to be heated to the water white transparency state by oil bath.
Described ionic liquid is one or more the mixture in the ionic liquid of following negatively charged ion and cation composition; Wherein, positively charged ion be alkyl imidazole salt, Fixanol, alkyl pyrroles salt, alkyl quaternary ammonium salts, alkyl quaternary phosphonium salt, fluoro-alkyl imidazole salts, fluoro-alkyl pyridinium salt, fluoro-alkyl pyrroles salt, fluoro-alkyl quaternary ammonium salt or fluoro-alkyl season phosphonium salt, negatively charged ion is Cl
-, AlCl
4 -, BF
4 -, PF
6 -, NO
3 -, N (CF
3SO
2)
2 -Or CF
3SO
3 -
The anode of described electrolyzer is metal platinum or purity greater than 99.9% high pure metal tungsten, and negative electrode is the solid gallium sheet.
The dc electrodeposition mode is adopted in described galvanic deposit, and the current density of negative electrode is controlled at 5～100A/m
2, bath voltage is 1.0～3V, and the pole span between negative electrode and the anode is 15～60mm, and the electrolyzer electrodeposition temperature is controlled at 25～150 ℃.
Described electrolyzer inner anode and cathode surface are parallel to each other.
At least be provided with one group in the described electrolyzer with electrode that anode-cathode-the anode mode is arranged.
Further, described ionic liquid is chloro 1-ethyl-3-methylimidazole and/or chloro 1-butyl-3 Methylimidazole.
The present invention is with gallium chloride (GaCl
3) be raw material, take ionic liquid as ionogen, first gallium chloride is dissolved in wherein, adopt again direct supply to carry out galvanic deposit.Melt salt because ionic liquid is a kind of room temperature that is made of ion fully, usually formed by the asymmetric organic cation of geometry and inorganic or organic anion.Compare with conventional solvent, ionic liquid has the characteristics such as chemical heat stability is high, not flammable, steam forces down, specific conductivity high, toxicity is little, electrochemical window is wide; And ionic liquid of the present invention has good solubility to gallium chloride, ionic liquid can at room temperature can be obtained the metal that the ability galvanic deposit obtains in high-temperature molten salt as ionogen, but do not have again the such severe corrosive of high-temperature molten salt.So the service temperature of galvanic deposit gallium of the present invention is low, less energy consumption, little to equipment corrosion, will greatly reduce production costs, and is environmentally friendly.
Further, can also carry out the fluoro processing to the positively charged ion in the ionic liquid in order to improve its electrochemical stability.
Embodiment
Embodiment 1:
Chloro 1-ethyl-3-methylimidazole ([Emim] Cl) ionic liquid is heated to the water white transparency state under 60 ℃ constant temperature oil bath, then under magnetic agitation with gallium chloride (GaCl
3) be dissolved in the chloro 1-ethyl-3-methylimidazole ionic liquid, form gallium chloride solution; Again take two parallel purity at the tungsten more than 99.9% as anode, the solid metal gallium is that negative electrode carries out galvanic deposit to gallium chloride solution, produces chlorine on the anode, separates out solid gallium on the negative electrode; Wherein, the electrolyzer inner anode is parallel with cathode surface, and anode and negative electrode are arranged in the mode of anode-cathode-anode; The current density of negative electrode is controlled at 80A/m
2, bath voltage is 2.8V, the pole span 15mm between negative electrode and the anode, and 50 ℃ of electrodeposition temperatures, electrodeposition time are 0.5h.
Embodiment 2:
Chloro 1-butyl-3-Methylimidazole ([Bmim] Cl) ionic liquid is heated to the water white transparency state under 60 ℃ constant temperature oil bath, then under magnetic agitation with gallium chloride (GaCl
3) be dissolved in chloro 1-butyl-3-Methylimidazole ionic liquid, form gallium chloride solution; Again take two parallel purity at the tungsten more than 99.9% as anode, the solid metal gallium is that negative electrode carries out galvanic deposit to gallium chloride solution, produces chlorine on the anode, separates out solid gallium on the negative electrode; Wherein, the electrolyzer inner anode is parallel with cathode surface, and anode and negative electrode are arranged in the mode of anode-cathode-anode; The current density of negative electrode is controlled at 80A/m
2, bath voltage is 3.0V, the pole span 14mm between negative electrode and the anode, and 50 ℃ of electrodeposition temperatures, electrodeposition time are 0.5h.
Embodiment 3:
Chloro 1-ethyl-3-methylimidazole ([Emim] Cl) ionic liquid is heated to the water white transparency state under 60 ℃ constant temperature oil bath, then under magnetic agitation with gallium chloride (GaCl
3) be dissolved in the chloro 1-ethyl-3-methylimidazole ionic liquid, form gallium chloride solution; Take two parallel metal platinum as anode, the solid metal gallium is that negative electrode carries out galvanic deposit to gallium chloride solution, produces chlorine on the anode, separates out solid gallium on the negative electrode again; Wherein, the electrolyzer inner anode is parallel with cathode surface, and anode and negative electrode are arranged in the mode of anode-cathode-anode; The current density of negative electrode is controlled at 5A/m
2, bath voltage is 3.0V, the pole span 21mm between negative electrode and the anode, and 150 ℃ of electrodeposition temperatures, electrodeposition time are 2.0h.
Embodiment 4:
Chloro 1-butyl-3-Methylimidazole ([Bmim] Cl) and chloro 1-ethyl-3-methylimidazole ([Emim] Cl) mixed ionic liquid are heated to the water white transparency state under 60 ℃ constant temperature oil bath, then under magnetic agitation with gallium chloride (GaCl
3) be dissolved in chloro 1-butyl-3-Methylimidazole and chloro 1-ethyl-3-methylimidazole ([Emim] Cl) mixed ionic liquid, form gallium chloride solution; Again take two parallel purity at the tungsten more than 99.9% as anode, the solid metal gallium is that negative electrode carries out galvanic deposit to gallium chloride solution, wherein, the electrolyzer inner anode is parallel with cathode surface, anode and negative electrode are arranged in the mode of anode-cathode-anode; The current density of negative electrode is controlled at 32A/m
2, bath voltage is 1.0V, the pole span 45mm between negative electrode and the anode, and 80 ℃ of electrodeposition temperatures, electrodeposition time is 2.5h, produces chlorine on the anode, separates out solid gallium on the negative electrode.
Embodiment 5:
Chloro 1-butyl-3-Methylimidazole ([Bmim] Cl) ionic liquid is heated to the water white transparency state under 60 ℃ constant temperature oil bath, then under magnetic agitation with gallium chloride (GaCl
3) be dissolved in chloro 1-butyl-3-Methylimidazole ionic liquid, form gallium chloride solution; Again take two parallel purity at the tungsten more than 99.9% as anode, the solid metal gallium is that negative electrode carries out galvanic deposit to gallium chloride solution, produces chlorine on the anode, separates out solid gallium on the negative electrode; Wherein, the electrolyzer inner anode is parallel with cathode surface, and anode and negative electrode are arranged in the mode of anode-cathode-anode-cathode-anode; The current density of negative electrode is controlled at 100A/m
2, bath voltage is 1.0V, the pole span 60mm between negative electrode and the anode, and 25 ℃ of electrodeposition temperatures, electrodeposition time are 2.5h.
Claims (7)
1. a method of utilizing ionic liquid low temp. electric deposition gallium is characterized in that: ionic liquid is heated to the water white transparency state, then gallium chloride is dissolved in the ionic liquid, form gallium chloride solution; Again gallium chloride solution is carried out galvanic deposit, generate gallium on the negative electrode of electrolyzer, emit chlorine on the anode; Wherein, in the electrodeposition process, the bath voltage of electrolyzer is higher than the gallium chloride decomposition voltage, and the bath voltage of electrolyzer is lower than the electrochemical window of ionic liquid.
2. the method for utilizing ionic liquid low temp. electric deposition gallium according to claim 1, it is characterized in that: described ionic liquid is to be heated to the water white transparency state by oil bath.
3. the method for gallium is produced in galvanic deposit according to claim 1, it is characterized in that: described ionic liquid is one or more the mixture in the ionic liquid of following negatively charged ion and cation composition; Wherein, positively charged ion be alkyl imidazole salt, Fixanol, alkyl pyrroles salt, alkyl quaternary ammonium salts, alkyl quaternary phosphonium salt, fluoro-alkyl imidazole salts, fluoro-alkyl pyridinium salt, fluoro-alkyl pyrroles salt, fluoro-alkyl quaternary ammonium salt or fluoro-alkyl season phosphonium salt, negatively charged ion is Cl
-, AlCl
4 -, BF
4 -, PF
6 -, NO
3 -, N (CF
3SO
2)
2 -Or CF
3SO
3 -
4. the method for utilizing ionic liquid low temp. electric deposition gallium according to claim 1 is characterized in that: the anode of described electrolyzer is metal platinum or purity greater than 99.9% high pure metal tungsten, and negative electrode is the solid gallium sheet.
5. the method for utilizing ionic liquid low temp. electric deposition gallium according to claim 1, it is characterized in that: the dc electrodeposition mode is adopted in described galvanic deposit, and the current density of negative electrode is controlled at 5～100A/m
2, bath voltage is 1.0～3V, and the pole span between negative electrode and the anode is 15～60mm, and the electrolyzer electrodeposition temperature is controlled at 25～150 ℃.
6. the method for utilizing ionic liquid low temp. electric metal refining gallium according to claim 1, it is characterized in that: described electrolyzer inner anode and cathode surface are parallel to each other.
7. it is characterized in that according to claim 1 or the 6 described methods of utilizing ionic liquid low temp. electric metal refining gallium: be provided with at least one group in the described electrolyzer with electrode that anode-cathode-the anode mode is arranged.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104141151A (en) * | 2014-08-06 | 2014-11-12 | 哈尔滨工业大学 | Method for forming metal simple substance through ionic liquid in electrolytic deposition mode |
| CN104499002A (en) * | 2014-12-10 | 2015-04-08 | 上海大学 | Method for preparing copper-iron nano plated layer from low-grade sulfide ore through direct electro-deposition |
| CN105567987A (en) * | 2016-01-08 | 2016-05-11 | 石棉县亿欣钙业有限责任公司 | Method for extracting vanadium and tellurium simultaneously from waste residues |
| CN105624404A (en) * | 2016-01-08 | 2016-06-01 | 石棉县亿欣钙业有限责任公司 | Environmental-friendly comprehensive utilization method for waste residues |
| CN108728641A (en) * | 2018-06-22 | 2018-11-02 | 汉能新材料科技有限公司 | A kind of recovery method of GaAs waste material |
| CN111321427A (en) * | 2020-03-05 | 2020-06-23 | 惠州大亚湾艾利荣化工科技有限公司 | Method for low-temperature and low-pressure electrolysis of aluminum by using ionic liquid electrolyte |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104141151A (en) * | 2014-08-06 | 2014-11-12 | 哈尔滨工业大学 | Method for forming metal simple substance through ionic liquid in electrolytic deposition mode |
| CN104499002A (en) * | 2014-12-10 | 2015-04-08 | 上海大学 | Method for preparing copper-iron nano plated layer from low-grade sulfide ore through direct electro-deposition |
| CN105567987A (en) * | 2016-01-08 | 2016-05-11 | 石棉县亿欣钙业有限责任公司 | Method for extracting vanadium and tellurium simultaneously from waste residues |
| CN105624404A (en) * | 2016-01-08 | 2016-06-01 | 石棉县亿欣钙业有限责任公司 | Environmental-friendly comprehensive utilization method for waste residues |
| CN105567987B (en) * | 2016-01-08 | 2017-07-21 | 石棉县亿欣钙业有限责任公司 | It is a kind of to extract vanadium, the method for tellurium simultaneously from waste residue |
| CN108728641A (en) * | 2018-06-22 | 2018-11-02 | 汉能新材料科技有限公司 | A kind of recovery method of GaAs waste material |
| CN111321427A (en) * | 2020-03-05 | 2020-06-23 | 惠州大亚湾艾利荣化工科技有限公司 | Method for low-temperature and low-pressure electrolysis of aluminum by using ionic liquid electrolyte |
| CN111321427B (en) * | 2020-03-05 | 2021-05-28 | 惠州大亚湾艾利荣化工科技有限公司 | Method for low-temperature and low-pressure electrolysis of aluminum by using ionic liquid electrolyte |
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Application publication date: 20130410 |