CN103820827A - Method for electrodepositing palladium from ionic liquid - Google Patents
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- CN103820827A CN103820827A CN201410061799.5A CN201410061799A CN103820827A CN 103820827 A CN103820827 A CN 103820827A CN 201410061799 A CN201410061799 A CN 201410061799A CN 103820827 A CN103820827 A CN 103820827A
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Abstract
The invention relates to a method for electrodepositing palladium from an ionic liquid. The method is characterized in that an ionic liquid containing PdCl2 is utilized as an electrolyte, and a palladium element is directly obtained on a cathode in a constant current electrodeposition mode at a low temperature (25-70DEG C). The cation of the ionic liquid used in the invention is a 1,3-dialkyl substituted imidazole ionic liquid, and concretely is a 1-ethyl-3-methylimidazolium cation [EMIm]<+> having a low viscosity and a good conductivity at normal temperature, and the anion of the ionic liquid is trifluoroacetate (CF3COO<->), trifluoromethanesulfonate (CF3SO3<->), dicyanamide (DCA<->), ethylsulfate (C2H5SO4<->) and hexafluorophosphate (PF6<->). The cation is combined with one or more anions to form a substance, and the substance can be used as a PdCl2 solvent and an electrolyte. The method has the advantages of simple operation and low apparatus cost, and the electrolytic medium ionic liquid has the advantages of wide electrochemical window, good thermal stability, wide difference between a solidifying point and a boiling point and the like, so environment pollution caused by the inflammableness and the volatility of a common organic solvent is avoided.
Description
Technical field
The present invention relates to a kind of from ionic liquid the method for galvanic deposit palladium, utilize the non-aluminum chloride type of imidazoles ionic liquid that under normal temperature, viscosity ethyl low, good conductivity replaces as solvent and electrolytic solution, be a kind of electrochemical techniques of efficient, environmental protection.
Background technology
Palladium is a kind of precious metal with silvery white metalluster, good erosion resistance, ductility, wear-resisting, high temperature resistant and higher catalytic activity and high economic worth.The fields such as automobile, processing of ornament, industry and investment are widely used at present.
Traditional electrolysis system has water solution system and high-temperature molten salt, but the electrochemical window relative narrower of the aqueous solution, and liberation of hydrogen side reaction is serious, cause Hydrogen Brittleness Phenomena to produce, it is reported that spongy or pulverous palladium can absorb the hydrogen of 900 times of its volumes, has a strong impact on current efficiency and product quality.High-temperature molten salt rule fusing point is too high, and corrodibility is strong, and easily volatilize oxidation, burning and current consumption large equipment cost of electrolyte ingredient is high.Comparatively speaking, ionic liquid is due to wider electrochemical window, higher specific conductivity and mobility of ions, and wider liquid journey, volatilization hardly, toxicity are little etc., and advantage makes it have high using value and development prospect in electrochemical field.
So-called ionic liquid be in room temperature or approach under room temperature (lower than 100 ℃), be liquid state conventionally combine by relatively large, the asymmetric organic cation of volume and the relatively little organic or inorganic negatively charged ion of volume the material forming completely.Conventionally also referred to as ionic liquid at room temperature (Room Temperature Ionic Liquids) or room temperature fused salt.
The positively charged ion of composition ionic liquid mainly can be divided into four classes: alkyl quaternary ammonium ion [NR
xh
4-x]
+, alkyl quaternary phosphine ion [PR
xh
4-x]
+, N-alkyl substituted pyridines ion [RPy]
+, 1,3-dialkyl group substituted imidazole ion, or claim N, N '-dialkyl group substituted imidazole ion [RR ' im]
+.Negatively charged ion can be divided into the adjustable aluminum chloride type ionic liquid of composition, and composition structure is halide salt+AlCl
3(Cl can replace with other haloid elements such as Br), its performance can be with AlCl
3molar fraction N variation and change, in the time of 0.33<N<0.5, be lewis base property, in the time of 0.5<N<0.67, be acid, in the time of N=0.5, be neutrality.Early, advantage is that performance is adjustable in this class ionic liquid research, and shortcoming is extremely responsive to moisture, is unfavorable for application.In addition it is fixing that ionic liquid also can be divided into composition, and the stable novel ion liquid of large multipair water and air is as BF
4 -, PF
6 -, CF
3cOO
-, CF
3sO
3 -deng.
The special composition of ionic liquid makes it have the performance advantage that is different from ordinary organic solvents uniqueness, as lower fusing point, because positively charged ion and negatively charged ion huge in ionic liquid have height asymmetry, due to steric restriction, make yin, yang ion on microcosmic, be difficult to close-packed, thereby hinder its crystallization, and making the melting point depression of this ionic compound, at lower temperature, can exist with liquid form.In addition, ionic liquid does not almost have vapour pressure, good solubility, solubilized organic or inorganic compound, wide electrochemical window, those can be studied to some electrochemical process water sensitive or that should not carry out in the aqueous solution, and the ionic liquid of different performance can be obtained by changing the combination of positively charged ion and negatively charged ion.
The above-mentioned advantage of ionic liquid is that its entirety is for the aqueous solution and the common organic reagent, with regard to ionic liquid self, because its composition, structure difference also exist certain difference.The people such as M.Jayakumar carry out the electrochemical research of palladium from nitric acid medium and simulated high-level radioactive waste by extraction-electro-deposition method, its ionic liquid adopting is methyl tricapryl ammonium chloride (TOMAC), changed into the form of methyl trioctylphosphine ammonium nitrate (TOMAN) by nitrification, method novelty, but TOMAC at normal temperatures viscosity is larger, in nitrification and extraction process, add respectively toxic substance benzene and chloroform as thinner, be unfavorable for operator's safety and popularization.Y.Katayama etc. have studied palladium halogen complex compound [PdBr
4]
2-[PdCl
4]
2-electrochemical behavior in the two fluoroform sulfimides (BMPTFSI) of hydrophobic ionic liquid 1-butyl-3-methylpyrrole, and prepare the palladium of nano-scale.Although testing used pair of fluoroform sulfimide (TFSI-) anionic ionic liquid not only can stable existence, and not miscible with water, its cost is relatively high, and electrodeposition time is also grown (42h) increases energy consumption.M.Jayakumar etc. have studied the electrochemical behavior of fission platinum metals in ionic liquid chlorination 1-butyl-3-Methylimidazole (bmimCl), but bmimCl with respect to other substituting group chain lengths shorter (as ethyl replace) ionic liquid fusing point higher approximately 70 ℃, need be heated to the above temperature of fusing point and could dissolve PdCl
2.
Although ionic liquid has been obtained certain progress in electrochemical field, for Electrodeposition of Noble Metal palladium, also need continuation some good combination properties of searching and cost relatively cheap, the ionic liquid of convenient operation and popularization is used as electrolytic medium.
Summary of the invention
For seeking the electrolytic solution that can be used for Electrodeposition of Noble Metal palladium of a kind of good combination property, environmental protection, the invention provides a kind of from ionic liquid the method for galvanic deposit palladium.
A method for galvanic deposit palladium from ionic liquid, its feature comprises the following steps:
(1) configuration electrolytic solution: add oversaturated Palladous chloride to obtain mixed system in ionic liquid; Described ionic liquid is the glyoxaline ion liquid that ethyl replaces, and positively charged ion is 1-ethyl-3-methylimidazole [EMIm]
+, negatively charged ion is non-aluminum chloride type;
(2) mixed system in (1) is carried out to cyclic voltammetry curve test, obtain the reduction peak of palladium ion, corresponding palladium ion is reduced to the electric current of simple substance palladium, calculates current density;
(3) according to the current density in (2), adopt current constant mode galvanic deposit palladium by direct supply, negative electrode is stainless steel plate, Ti plate, graphite or platinum carbon noble electrode, and anode is Pd sheet; The parallel electrolyzer that is placed in of two lateral electrodes, two interpole gap 19～35mm, electrolysis time 10～24h, 25～70 ℃ of electrolysis temperatures;
(4) collect the product of gained in (3), the product obtaining is separated by centrifugation with ionic liquid, product is used ethanol, hydrochloric acid, washed with de-ionized water successively, removing residual organic phase, have neither part nor lot in the PdCl of reaction
2, then dry;
Above step is carried out under inert atmosphere.Generally can use argon gas.
Further, negatively charged ion is trifluoroacetate, fluoroform sulphonate, Dyhard RU 100 salt, sulfovinic acid salt or hexafluorophosphate.
Ionic liquid after separating in step (4) can reuse.
Concrete steps are as follows:
(1) configuration electrolytic solution: first take the ionic liquid at room temperature of 0.05mol, then add therein oversaturated PdCl
2, object is to avoid in Constant Electric Current deposition process, owing to constantly consuming Pd
2+, make Pd
2+can not be diffused into around negative electrode in time, and cause concentration polarization degree to increase, maintain current constant simultaneously.
(2) mixed system in (1) is carried out to cyclic voltammetry curve test, obtain the reduction peak of palladium ion, corresponding palladium ion is reduced to the electric current of simple substance palladium, calculates current density.
(3) according to the current density in (2), adopt current constant mode galvanic deposit palladium by direct supply, negative electrode is stainless steel plate, Ti plate, graphite, platinum carbon noble electrode, and anode is Pd sheet.The parallel electrolyzer that is placed in of two lateral electrodes, two interpole gap 19～35mm, electrolysis time 10～24h, 25～70 ℃ of electrolysis temperatures.
(4) product of gained in collection (3), the galvanic deposit product obtaining is separated by centrifugation with ionic liquid, wherein ionic liquid sealed storage is waited to reuse, and product is used ethanol, hydrochloric acid, washed with de-ionized water successively, removing residual organic phase, have neither part nor lot in the PdCl of reaction
2, then dry.
The present invention has following advantage technically:
(1) selected ionic liquid is the novel ion liquid of the non-aluminum chloride type to water and air good stability, and positively charged ion is that normal temperature viscosity is low, and the glyoxaline cation that the ethyl of good conductivity replaces is 1-ethyl-3-methylimidazole positively charged ion [EMIm]
+, negatively charged ion is trifluoroacetate (CF
3cOO
-), fluoroform sulphonate (CF
3sO
3 -), Dyhard RU 100 salt (DCA
-), sulfovinic acid salt (C
2h
5sO
4 -), hexafluorophosphate (PF
6 -), ionic liquid used is that the mode of above-mentioned positively charged ion and one or more negatively charged ion combination is as PdCl
2solvent and electrolytic solution, do not need to add extra thinner.
(2) can realize cold operation, avoid too much energy consumption.
(3) equipment cost is cheap, and electrolyzer is conventional DC power supply, and operating process is simple.
(4) ionic liquid is soluble in ethanol as organic phase, can be collected and be obtained clean product by the mode that adds ethanol to clean after centrifugation.
Accompanying drawing explanation
Fig. 1 be 35 ℃ from ionic liquid EMIMCF
3sO
3the SEM figure of middle galvanic deposit palladium product:
As can be seen from the figure, products therefrom surface topography is even.
Fig. 2 is the XRD figure of above-mentioned product:
From figure, see to draw that the palladium in galvanic deposit product is to exist with a kind of form of palladium simple substance really.
Embodiment
Below in conjunction with example, the invention will be further described
Embodiment mono-:
(1) take the 1-ethyl-3-methylimidazole trifluoroacetate (EMIMCF of 0.05mol
3cOO) ionic liquid.
(2) to EMIMCF
3in COO, add 0.2gPdCl
2, at 25 ℃, through temperature constant magnetic stirring 30min, make PdCl
2reach hypersaturated state, object is to avoid in Constant Electric Current deposition process, owing to constantly consuming Pd
2+, make Pd
2+can not be diffused into around negative electrode in time, and cause concentration polarization degree to increase, maintain current constant simultaneously.
(3) mixed system is carried out to cyclic voltammetry curve test, obtain the reduction peak of palladium ion, corresponding palladium ion is reduced to the electric current of simple substance palladium, and calculating current density is 0.02mA/mm
2.
(4) during according to the current density in (3) and galvanic deposit, the surface-area of negative electrode used calculates the size of current of electrodeposition process, carries out the galvanic deposit of palladium under this electric current.Wherein negative electrode is Ti plate (15mm × 5mm), and anode is Pd sheet (6mm × 4mm), and the parallel placement of two electrodes and two interelectrode distances are 19mm.
(5) electrodeposition temperature is 25 ℃, controls by thermostatical oil bath, and electrodeposition time is 24h.
(6) galvanic deposit product and ionic liquid are carried out to centrifugation, ionic liquid stores to be waited to reuse, and galvanic deposit product cleans through ethanol, removes residual organic phase, then uses hydrochloric acid cleaning, to dissolve unreacted PdCl
2, finally use washed with de-ionized water, dry, obtain palladium simple substance.
Embodiment bis-:
(1) take 0.05mol1-ethyl-3-methylimidazole fluoroform sulphonate (EMIMCF
3sO
3) ionic liquid.
(2) to EMIMCF
3sO
3in add 0.2gPdCl
2, at 35 ℃, through temperature constant magnetic stirring 30min, make PdCl
2reach hypersaturated state, object is to avoid in Constant Electric Current deposition process, owing to constantly consuming Pd
2+, make Pd
2+can not be diffused into around negative electrode in time, and cause concentration polarization degree to increase, maintain current constant simultaneously.
(3) mixed system is carried out to cyclic voltammetry curve test, obtain the reduction peak of palladium ion, corresponding palladium ion is reduced to the electric current of simple substance palladium, and calculating current density is 0.016mA/mm
2.
(4) during according to the current density in (3) and galvanic deposit, the surface-area of negative electrode used calculates the size of current of electrodeposition process, carries out the galvanic deposit of palladium under this electric current.Wherein negative electrode is stainless steel plate (15mm × 5mm), and anode is Pd sheet (6mm × 4mm), and the parallel placement of two electrodes and two interelectrode distances are 27mm.
(5) electrodeposition temperature is 35 ℃, controls by thermostatical oil bath, and electrodeposition time is 20h.
(6) galvanic deposit product and ionic liquid are carried out to centrifugation, ionic liquid stores to be waited to reuse, and galvanic deposit product cleans through ethanol, removes residual organic phase, then uses hydrochloric acid cleaning, to dissolve unreacted PdCl
2, finally use washed with de-ionized water, dry, obtain palladium simple substance.
Embodiment tri-:
(1) take 0.05mol1-ethyl-3-methylimidazole hexafluorophosphate (EMIMPF
6) ionic liquid.
(2) be warming up to 70 ℃, now EMIMPF
6be fused into liquid state completely, then add wherein 0.2gPdCl
2, at 70 ℃, through temperature constant magnetic stirring 1h, make PdCl
2reach hypersaturated state, object is to avoid in Constant Electric Current deposition process, owing to constantly consuming Pd
2+, make Pd
2+can not be diffused into around negative electrode in time, and cause concentration polarization degree to increase, maintain current constant simultaneously.
(3) mixed system is carried out to cyclic voltammetry curve test, obtain the reduction peak of palladium ion, corresponding palladium ion is reduced to the electric current of simple substance palladium, and calculating current density is 0.03mA/mm
2.
(4) during according to the current density in (3) and galvanic deposit, cathodic surface area used is calculated the size of current of electrodeposition process, carries out the galvanic deposit of palladium under this electric current.Wherein negative electrode is Graphite Electrodes (Φ 7mm), and anode is Pd sheet (6mm × 4mm), and the parallel placement of two electrodes and two interelectrode distances are 35mm.
(5) electrodeposition temperature is 70 ℃, controls by thermostatical oil bath, and electrodeposition time is 15h.
(6) galvanic deposit product and ionic liquid are carried out to centrifugation, ionic liquid stores to be waited to reuse, and galvanic deposit product cleans through ethanol, removes residual organic phase, then uses hydrochloric acid cleaning, to dissolve unreacted PdCl
2, finally use washed with de-ionized water, dry, obtain palladium simple substance.
Above operating process is all carried out under argon gas atmosphere.
Claims (3)
1. a method for galvanic deposit palladium from ionic liquid, its feature comprises the following steps:
(1) configuration electrolytic solution: add oversaturated Palladous chloride to obtain mixed system in ionic liquid; Described ionic liquid is the glyoxaline ion liquid that ethyl replaces, and positively charged ion is 1-ethyl-3-methylimidazole [EMIm]
+, negatively charged ion is non-aluminum chloride type;
(2) mixed system in (1) is carried out to cyclic voltammetry curve test, obtain the reduction peak of palladium ion, corresponding palladium ion is reduced to the electric current of simple substance palladium, calculates current density;
(3) according to the current density in (2), adopt current constant mode galvanic deposit palladium by direct supply, negative electrode is stainless steel plate, Ti plate, graphite or platinum carbon noble electrode, and anode is Pd sheet; The parallel electrolyzer that is placed in of two lateral electrodes, two interpole gap 19～35mm, electrolysis time 10～24h, 25～70 ℃ of electrolysis temperatures;
(4) collect the product of gained in (3), the product obtaining is separated by centrifugation with ionic liquid, product is used ethanol, hydrochloric acid, washed with de-ionized water successively, removing residual organic phase, have neither part nor lot in the PdCl of reaction
2, then dry;
Above step is carried out under inert atmosphere.
As claimed in claim 1 a kind of from ionic liquid the method for galvanic deposit palladium, it is characterized in that: negatively charged ion is trifluoroacetate, fluoroform sulphonate, Dyhard RU 100 salt, sulfovinic acid salt or hexafluorophosphate.
As claimed in claim 1 a kind of from ionic liquid the method for galvanic deposit palladium, it is characterized in that: the ionic liquid recycling after separating in step (4).
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105063665A (en) * | 2015-08-05 | 2015-11-18 | 北京工业大学 | Method for electrically depositing nanometer platinum powder from ionic liquid |
| CN107447208A (en) * | 2017-06-23 | 2017-12-08 | 安庆师范大学 | A kind of method for preparing Pd Ni Fe P alloy films using chemical plating displacement |
| CN108251871A (en) * | 2018-02-12 | 2018-07-06 | 东北大学 | A kind of method of electro-deposition Al-Pt alloys in imidazole type ion liquid |
| CN108359809A (en) * | 2018-04-27 | 2018-08-03 | 连云港笃翔化工有限公司 | A method of recycling palladium bichloride from waste and old palladium catalyst |
| CN112080765A (en) * | 2020-08-07 | 2020-12-15 | 江苏理工学院 | Method for recovering palladium chloride in waste colloidal palladium activation solution |
| CN113215400A (en) * | 2021-05-11 | 2021-08-06 | 苏州科技大学 | Method for extracting metal ions by using ionic liquid compound |
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Cited By (10)
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|---|---|---|---|---|
| CN105063665A (en) * | 2015-08-05 | 2015-11-18 | 北京工业大学 | Method for electrically depositing nanometer platinum powder from ionic liquid |
| CN105063665B (en) * | 2015-08-05 | 2017-07-11 | 北京工业大学 | A kind of method of the nanometer of the electro-deposition from ionic liquid platinum powder |
| CN107447208A (en) * | 2017-06-23 | 2017-12-08 | 安庆师范大学 | A kind of method for preparing Pd Ni Fe P alloy films using chemical plating displacement |
| CN107447208B (en) * | 2017-06-23 | 2020-04-10 | 安庆师范大学 | Method for preparing Pd-Ni-Fe-P alloy film by chemical plating-displacement |
| CN108251871A (en) * | 2018-02-12 | 2018-07-06 | 东北大学 | A kind of method of electro-deposition Al-Pt alloys in imidazole type ion liquid |
| CN108359809A (en) * | 2018-04-27 | 2018-08-03 | 连云港笃翔化工有限公司 | A method of recycling palladium bichloride from waste and old palladium catalyst |
| CN112080765A (en) * | 2020-08-07 | 2020-12-15 | 江苏理工学院 | Method for recovering palladium chloride in waste colloidal palladium activation solution |
| CN112080765B (en) * | 2020-08-07 | 2021-10-19 | 江苏理工学院 | Method for recovering palladium chloride in waste colloidal palladium activation solution |
| CN113215400A (en) * | 2021-05-11 | 2021-08-06 | 苏州科技大学 | Method for extracting metal ions by using ionic liquid compound |
| CN113215400B (en) * | 2021-05-11 | 2022-04-15 | 苏州科技大学 | Method for extracting metal ions by using ionic liquid compound |
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Inventor after: Xi Xiaoli Inventor after: Song Panpan Inventor after: Nie Zuoren Inventor after: Sun Xiaokai Inventor after: Ma Liwen Inventor after: Zhang Liwen Inventor before: Xi Xiaoli Inventor before: Nie Zuoren Inventor before: Song Panpan Inventor before: Sun Xiaokai Inventor before: Ma Liwen Inventor before: Zhang Liwen |
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Free format text: CORRECT: INVENTOR; FROM: XI XIAOLI NIE ZUOREN SONG SHANSHAN SUN XIAOKAI MA LIWEN ZHANG LIWEN TO: XI XIAOLI SONG SHANSHAN NIE ZUOREN SUN XIAOKAI MA LIWEN ZHANG LIWEN |
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Application publication date: 20140528 |
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| RJ01 | Rejection of invention patent application after publication |