CN103046081A - Method for preparing silver by utilizing ionic liquid through electrodeposition at low temperature - Google Patents
Method for preparing silver by utilizing ionic liquid through electrodeposition at low temperature Download PDFInfo
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- CN103046081A CN103046081A CN2012105636300A CN201210563630A CN103046081A CN 103046081 A CN103046081 A CN 103046081A CN 2012105636300 A CN2012105636300 A CN 2012105636300A CN 201210563630 A CN201210563630 A CN 201210563630A CN 103046081 A CN103046081 A CN 103046081A
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Abstract
The invention relates to a method for preparing silver by utilizing ionic liquid through electrodeposition at low temperature. The method is characterized by comprising the following steps: anhydrous silver chloride is taken as raw material, ionic liquid is taken as electrolyte, the silver chloride is dissolved in the ionic liquid completely, then a direct current supply is adopted for performing electrodeposition, and during electrodeposition, the bath voltage is higher than the decomposition voltage of the silver chloride and lower than the electrochemical window of the ionic liquid, so that silver is produced at the cathode, and chlorine gas is produced at the anode. The invention provides the method for producing metal silver by utilizing ionic liquid through electrodeposition at low temperature. According to the method, silver chloride (AgCl) is taken as raw material and is dissolved in ionic liquid, so that ionic liquid-AgCl electrolyte is prepared for electrodeposition. During the electrodeposition process, the bath voltage is higher than the decomposition voltage of the silver chloride and lower than the electrochemical window of the ionic liquid, so that silver is produced at the cathode, and chlorine gas is produced at the anode.
Description
Technical field
The present invention relates to a kind of method of utilizing ionic liquid low temp. electric depositing silver.
Background technology
Nano material is because its unique physics, chemical property and wide application prospect have become the focus that people study.Metal nano material has significant physics and chemistry characteristic at aspects such as electricity, magnetics, mechanics, is with a wide range of applications.Nanometer silver has been widely used in many fields such as stupalith, environment-friendly materials and coating as important functional materials.Although at present the multiple method for preparing nanoparticle has been arranged, along with the raising of people's Environmental awareness, the proposition of Green Chemistry concept, the preparation method who studies the nanoparticle pollution-free, that energy consumption is low, method is easy still is the target that people pursue.Recently, the method for preparing nano material in Room Temperature Ionic Liquid begins that reported in literature is arranged.Studies show that, ionic liquid can reuse in preparations of nanomaterials, can reduce preparation cost, is expected to realize the Green Chemistry preparation.
Ionic liquid is that a kind of room temperature that is made of ion is fully melted salt, usually is comprised of 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 is high, toxicity is little, electrochemical window is wide.Ionic liquid at room temperature can obtain the metal that the ability galvanic deposit obtains in high-temperature molten salt, but does not have again the such severe corrosive of high-temperature molten salt.
Summary of the invention
The purpose of this invention is to provide that a kind of service temperature is low, less energy consumption, the method for utilizing ionic liquid low temp. electric depositing silver little to equipment corrosion.
A kind of method of utilizing ionic liquid low temp. electric depositing silver, its special feature is, comprise the steps: take anhydrous chlorides of rase silver as raw material, ionic liquid is ionogen, first silver chloride is dissolved in wherein fully, adopts direct supply to carry out galvanic deposit again, bath voltage is higher than the silver chloride decomposition voltage and is lower than the electrochemical window of ionic liquid during galvanic deposit, thereby produce silver at negative electrode, emit chlorine on the anode.
Wherein ionic liquid is as positively charged ion, and with Cl with 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 and the optional one of fluoro-alkyl season phosphonium salt
-, AlCl
4 -, BF
4 -, PF
6 -, NO
3 -, N (CF
3SO
2)
-And CF
3SO
3 -Between optional one as negatively charged ion, a kind of pure ionic liquid of composition or two kinds and above mixed ionic liquid.
Wherein the dc electrodeposition mode is adopted in galvanic deposit, is anode with high purity graphite or metallic copper, and Solid Silver is negative electrode, and cathode current density is controlled at 5～100A/m
2, bath voltage is controlled at 1.0～3V, and pole span is controlled at 15～60mm, and electrolysis temperature is controlled at 25～150 ℃.
Wherein negative electrode and positive electrode is arranged vertically in the electrolyzer, and electrode surface is parallel to each other, and is provided with at least one group of electrode of arranging with anode, negative electrode, anode mode in cell body.
Wherein the consumption of silver chloride and ionic liquid is for making silver chloride be dissolved in any proportioning in the ionic liquid fully.
The invention provides a kind of method of utilizing ionic liquid low temp. electric deposition to produce argent.The method is dissolved into AgCl in the ionic liquid take silver chloride (AgCl) as raw material, is mixed with ionic liquid-AgCl electrolytic solution, carries out galvanic deposit.In the electrodeposition process, bath voltage will be higher than the decomposition voltage of silver chloride, and is lower than the electrochemical window of ionic liquid, produces silver on the negative electrode, emits chlorine on the anode.The ionic liquid quality is light, nontoxic, non-volatility, without flammable, electroconductibility is good, thermostability is high, fusing point is low, boiling point is high, electrochemical window is wide, can slow down the corrosion to electrode materials and slot liner, and reusable edible.
Embodiment
Method of the present invention is to deposit for present industrial electro to produce some problems that silver exists, and the problems such as such as high energy consumption,, etching apparatus unfriendly to environment, cost is large, contaminate environment propose a kind of ionic liquid that utilizes and carry out galvanic deposit production silver.The method service temperature is low, less energy consumption, little to equipment corrosion, will greatly reduce production costs.
A kind of method of utilizing ionic liquid low temp. electric deposition to produce argent, the method is dissolved into AgCl in the ionic liquid take silver chloride AgCl as raw material, and gained solution is that electrolytic solution carries out dc electrodeposition.Groove is pressed and is higher than the decomposition voltage of silver chloride, and is lower than the electrochemical window of ionic liquid.Produce silver on the negative electrode, emit chlorine on the anode.The selected ionic liquid of method is mainly considered two problems, the one, silver chloride there is good solubility, and the 2nd, have wider electrochemical window and higher specific conductivity.The positively charged ion of common ion liquid has the positively charged ions such as alkyl imidazole salt, Fixanol, alkyl pyrroles salt, alkyl quaternary ammonium salts, alkyl quaternary phosphonium salt, can also carry out the fluoro processing to it in order to improve its electrochemical stability.Negatively charged ion commonly used also has BF except chlorion
4 -PF
6 -, NO
3 -AlCl
4 -, CF
3SO
3 -, N (CF
3SO
2)
2 -Deng negatively charged ion.The ionic liquid that adopts in addition can be a kind of pure ionic liquid, also can be two or more mixed ionic liquids.Adopt dc electrolysis, groove is pressed and will be higher than the decomposition voltage that closes silver chloride and the electrochemical window that is lower than ionic liquid produced silver on the negative electrode, emits chlorine on the anode.
Embodiment 1:
Take by weighing the choline chloride 60 ChCl of 50g, be that 1:2 adds ethylene glycol in ChCl according to mol ratio, obtain colourless transparent solution 80 ℃ of lower heating, and then add the 3g silver chloride, and 60 ℃ of constant temperature oil bath heating, magnetic agitation to silver chloride dissolves fully, again take two parallel high-purity (purity gets final product greater than 66.6%) graphite as anode, the centre is solid silver strip negative electrode, and pole span 15mm is at 50A/m
2Current density under constant-current electrolysis 0.5h, anode produces chlorine, separates out Solid Silver on the negative electrode.
What electrolysis mode adopted is the continuous current galvanic deposit, and bath voltage is controlled at 1.2V, and electrolysis temperature is controlled at 60 ℃.
Embodiment 2:
Take by weighing the choline chloride 60 ChCl of 50g, be that 1:2 adds urea in choline chloride 60 ChCl according to mol ratio, obtain colourless transparent solution 120 ℃ of heating, then add the 1g silver chloride, 60 ℃ of heating of constant temperature oil bath, magnetic agitation to silver chloride dissolves fully, again take two parallel high purity graphites as anode, the centre is solid silver strip negative electrode, and pole span 15mm is at 80A/m
2Current density under constant-current electrolysis 0.5h, anode produces chlorine, separates out Solid Silver on the negative electrode.
What electrolysis mode adopted is the continuous current galvanic deposit, and bath voltage is controlled at 1.2V, and electrolysis temperature is controlled at 60 ℃.
Claims (5)
1. method of utilizing ionic liquid low temp. electric depositing silver, it is characterized in that, comprise the steps: take anhydrous chlorides of rase silver as raw material, ionic liquid is ionogen, first silver chloride is dissolved in wherein fully, adopts direct supply to carry out galvanic deposit again, bath voltage is higher than the silver chloride decomposition voltage and is lower than the electrochemical window of ionic liquid during galvanic deposit, thereby produce silver at negative electrode, emit chlorine on the anode.
2. a kind of method of utilizing ionic liquid low temp. electric depositing silver as claimed in claim 1, it is characterized in that: wherein ionic liquid is as positively charged ion, and with Cl with 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 and the optional one of fluoro-alkyl season phosphonium salt
-, AlCl
4 -, BF
4 -, PF
6 -, NO
3 -, N (CF
3SO
2)
-And CF
3SO
3 -Between optional one as negatively charged ion, a kind of pure ionic liquid of composition or two kinds and above mixed ionic liquid.
3. a kind of method of utilizing ionic liquid low temp. electric depositing silver as claimed in claim 1, it is characterized in that: wherein the dc electrodeposition mode is adopted in galvanic deposit, be anode with high purity graphite or metallic copper, Solid Silver is negative electrode, and cathode current density is controlled at 5～100A/m
2, bath voltage is controlled at 1.0～3V, and pole span is controlled at 15～60mm, and electrolysis temperature is controlled at 25～150 ℃.
4. a kind of method of utilizing ionic liquid low temp. electric depositing silver as claimed in claim 3, it is characterized in that: wherein negative electrode and positive electrode is arranged vertically in the electrolyzer, electrode surface is parallel to each other, and is provided with at least one group of electrode of arranging with anode, negative electrode, anode mode in cell body.
5. a kind of method of utilizing ionic liquid low temp. electric depositing silver as claimed in claim 1 is characterized in that: wherein the consumption of silver chloride and ionic liquid is for making silver chloride be dissolved in any proportioning in the ionic liquid fully.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103590089A (en) * | 2013-11-20 | 2014-02-19 | 上海应用技术学院 | Preparation method of graphene/silver composite material |
| CN105413717A (en) * | 2015-11-05 | 2016-03-23 | 长安大学 | Method for preparing Ag/AgCl nano catalysts and application thereof |
| CN106661753A (en) * | 2014-04-15 | 2017-05-10 | 尼奥工业有限责任公司 | Ionic liquid electrolyte and method to electrodeposit metals |
| CN107190283A (en) * | 2017-05-19 | 2017-09-22 | 东北大学 | A kind of method that nearly room temperature is co-deposited magnesium neodymium foundry alloy |
| CN110029370A (en) * | 2019-04-17 | 2019-07-19 | 上海大学 | By the method for low value cupro-nickel composite ore electro-deposition preparation high level ternary alloy three-partalloy |
| CN111620365A (en) * | 2019-02-28 | 2020-09-04 | 中国科学院化学研究所 | High-concentration silver halide solution, preparation method thereof and regeneration method of silver halide |
| CN114032581A (en) * | 2021-08-31 | 2022-02-11 | 中国科学院过程工程研究所 | Method for electrochemically reconstructing metal surface by ionic liquid medium to electro-catalytically reduce carbon dioxide |
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| CN102517608A (en) * | 2011-12-23 | 2012-06-27 | 彩虹集团公司 | Method for electrodepositing zinc and zinc alloy at low temperature by ionic liquor |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103590089A (en) * | 2013-11-20 | 2014-02-19 | 上海应用技术学院 | Preparation method of graphene/silver composite material |
| CN103590089B (en) * | 2013-11-20 | 2016-06-01 | 上海应用技术学院 | The preparation method of a kind of graphene/silver composite material |
| CN106661753A (en) * | 2014-04-15 | 2017-05-10 | 尼奥工业有限责任公司 | Ionic liquid electrolyte and method to electrodeposit metals |
| US11105013B2 (en) | 2014-04-15 | 2021-08-31 | Neo Industries Llc | Ionic liquid electrolyte and method to electrodeposit metals |
| CN105413717A (en) * | 2015-11-05 | 2016-03-23 | 长安大学 | Method for preparing Ag/AgCl nano catalysts and application thereof |
| CN107190283A (en) * | 2017-05-19 | 2017-09-22 | 东北大学 | A kind of method that nearly room temperature is co-deposited magnesium neodymium foundry alloy |
| CN107190283B (en) * | 2017-05-19 | 2018-10-26 | 东北大学 | A kind of method that nearly room temperature is co-deposited magnesium neodymium master alloy |
| CN111620365A (en) * | 2019-02-28 | 2020-09-04 | 中国科学院化学研究所 | High-concentration silver halide solution, preparation method thereof and regeneration method of silver halide |
| CN110029370A (en) * | 2019-04-17 | 2019-07-19 | 上海大学 | By the method for low value cupro-nickel composite ore electro-deposition preparation high level ternary alloy three-partalloy |
| CN114032581A (en) * | 2021-08-31 | 2022-02-11 | 中国科学院过程工程研究所 | Method for electrochemically reconstructing metal surface by ionic liquid medium to electro-catalytically reduce carbon dioxide |
| CN114032581B (en) * | 2021-08-31 | 2023-03-07 | 中国科学院过程工程研究所 | Method for electrochemically reconstructing metal surface by ionic liquid medium to electro-catalytically reduce carbon dioxide |
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Application publication date: 20130417 |