CN103540974B - A kind of method that dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal - Google Patents
A kind of method that dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal Download PDFInfo
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Abstract
The present invention relates to a kind of method that dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, belong to metallurgical and technical field of material.First ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid;Then lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, makees negative electrode, graphite or inert anode with platinized platinum and makees anode, and in the ionic liquid electroplate liquid that above-mentioned steps prepares, electro-deposition 1~3h, can prepare lanthanoid metal at cathode surface.This method is relatively low because of electrolysis temperature, has that energy consumption is low, current efficiency is high, production procedure is short, pollute the advantages such as little, technique is simple, added value of product is high.
Description
Technical field
The present invention relates to a kind of method that dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, belong to metallurgical and technical field of material.
Background technology
Rare earth lanthanum is widely used in preparing the functional materials such as thermoelectricity, magnetic, nickel-hydrogen battery electrode because of its special character.The production of metal current lanthanum is mainly fused salt electrolysis process.Molten-salt electrolysis can realize stable, the large-scale production of lanthanoid metal, but the method exists the series of problems such as electrolysis temperature is high, energy consumption is huge, efficiency is low, discharge amount of exhaust gas is high, equipment corrosion is serious.Energy shortage, greenhouse effect aggravation severe situation under, how to realize energy-saving and emission-reduction prepared by lanthanoid metal and green production be key issue urgently to be resolved hurrily.Although fused salt electrolysis process has some technological improvements, the energy consumption of commercial production lanthanum to decrease in recent years, but years of researches and energy consumption can not be made significantly to decline it was verified that existing technique carries out improvement.Therefore, the low-temperature electrolytic novel preparation method of research and development lanthanoid metal, to its energy consumption being greatly lowered on source, reducing discharge, cause the extensive concern of researcher.
Ionic liquid is that a kind of room temperature being made up of ion completely melts salt, is generally made up of the asymmetric organic cation of geometry and inorganic or organic anion.With other solvent phase ratio, ionic liquid shows the physicochemical properties of uniqueness and distinctive function, has the characteristic such as light weight, nontoxic, non-combustible, steam forces down, chemical heat stability high, good, the electrochemical window width (generally higher than 4V) of heat-conductivity conducting.Ionic liquid is a kind of preferably room temperature liquid electrolyte, the advantage that it has merged high-temperature molten salt and aqueous solution: there is wider electrochemical window, the most i.e. can get ability electro-deposition obtains in high-temperature molten salt metal and alloy, and there is no severe corrosive as high-temperature molten salt.Utilize ionic liquid to prepare lanthanoid metal and electrolysis temperature can be controlled below 100 DEG C, thus solve the series of problems such as conventional high-temperature fused salt electrolysis process temperature is high, energy consumption is huge, discharge amount of exhaust gas is high, equipment corrosion is serious, it is achieved energy-saving and emission-reduction prepared by lanthanoid metal and green production.
Document (Rare Metals Materials and engineering, 2012,41,599-602) reports employing 1-ethyl-3-methylimidazole tetrafluoroborate (BMIMBF4) ionic liquid is that solvent electrolyte can prepare lanthanoid metal.This report is important to note that, as one typical neutral ion liquid, BMIMBF4The lowest to the dissolubility of metal halide, therefore add anhydrous LiCl to improve electrolyte system to lanthanum salt precursor body (LaCl3) dissolubility most important for the electrolytic deposition of lanthanoid metal.But the LiCl salt itself that the method uses also belongs to metal halide, limited in one's ability in terms of improving system dissolubility, and anhydrous LiCl cost intensive.
Apply for a patent (number of patent application 201110435737.2) and disclose a kind of method of electrodepositing metal lanthanum in ionic liquid, using 1-methyl-3-ethyl imidazol(e) two (trimethyl fluoride sulfonyl) imines as electrolyte, anhydrous LaCl3For lanthanum salt precursor body, copper sheet, as negative electrode, prepares lanthanoid metal using platinum, graphite or titanium-based oxide as anode, galvanostatic deposition.This application patent uses 1-methyl-3-ethyl imidazol(e) two (trimethyl fluoride sulfonyl) imines neutral ion liquid as electrolyte, equally exists the problem that the above-mentioned metal halide dissolubility mentioned is the lowest.This key issue is not illustrated by this patent, and its gained cathode product is not carried out material phase analysis yet, causes and cannot determine that its product is lanthanoid metal.
Summary of the invention
The problem existed for above-mentioned prior art and deficiency, the present invention provides a kind of method that dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal.When verifying 25 DEG C due to experiment, anhydrous LaCl3Saturation solubility in dicyandiamide type ionic liquid MDCA is not less than 2.5g/100g, therefore uses dissolved with LaCl3Dicyandiamide ionic liquid prepare lanthanoid metal as electroplate liquid electro-deposition, the present invention is achieved through the following technical solutions.
A kind of method that dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, it specifically comprises the following steps that
(1) ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid, the wherein volume of dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Mass ratio be 100:(1~5) ml/g;
(2) lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, makees negative electrode, graphite or inert anode with platinized platinum and makees anode, electrolysis temperature be 25~60 DEG C, stir speed (S.S.) be 100~300r/min, and to use controlling potential be (-0.80~-1.15V
vs.Ag/Ag+), groove pressure is 2.80~3.20V or electric current is 2~8mA cm-2Under the conditions of and electro-deposition 1~3h in the ionic liquid electroplate liquid that step (1) prepares, lanthanoid metal can be prepared at cathode surface.
M in described dicyandiamide type ionic liquid MDCA is ionic liquid cation, such as 1-ethyl-3-methylimidazole, 1-butyl-3-Methylimidazole., 1-ethyl-1-methylpyrrole, 1-butyl-1-methylpyrrole, 1-ethyl-3-picoline, 1-butyl-3-picoline, tetramethyl ammonium, tetraethyl ammonium salt or 4-butyl ammonium.
Above-mentioned dicyandiamide type ionic liquid MDCA purity is 99%, containing 1% moisture and other impurity.
The invention has the beneficial effects as follows: this method is relatively low because of electrolysis temperature have that energy consumption is low, current efficiency is high, production procedure is short, pollute the advantages such as little, technique is simple, added value of product is high.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the lanthanoid metal of the embodiment of the present invention 1 preparation;
Fig. 2 is the XRD figure of the lanthanoid metal of the embodiment of the present invention 1 preparation;
Fig. 3 is the SEM figure of the lanthanoid metal of the embodiment of the present invention 2 preparation;
Fig. 4 is the XRD figure of the lanthanoid metal of the embodiment of the present invention 2 preparation.
Detailed description of the invention
Below in conjunction with the accompanying drawings and detailed description of the invention, the invention will be further described.
Embodiment 1
The method that this dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, it specifically comprises the following steps that
(1) ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid, the wherein volume of dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Mass ratio be 100:2.5ml/g, M in dicyandiamide type ionic liquid MDCA is 1-butyl-3-Methylimidazole. ionic liquid cation, this dicyandiamide type ionic liquid is 1-butyl-3-Methylimidazole. dicyandiamide salt (BMIMDCA), and the purity of BMIMDCA is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, make negative electrode with platinized platinum (1.0cm × 1.0cm × 0.2cm), graphite makees anode, to keep die opening be 1cm, electrolysis temperature is 25 DEG C, stir speed (S.S.) is 100r/min, and to use controlling potential be (-1.00V vs.Ag/Ag+Electro-deposition 2h under the conditions of) and in the ionic liquid electroplate liquid that step (1) prepares, can prepare lanthanoid metal at cathode surface, and gained lanthanum sedimentary average grain size is 100nm, as illustrated in fig. 1 and 2.
Embodiment 2
The method that this dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, it specifically comprises the following steps that
(1) ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid, the wherein volume of dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Mass ratio be 100:5ml/g, M in dicyandiamide type ionic liquid MDCA is 1-butyl-1-methylpyrrole ionic liquid cation, this dicyandiamide type ionic liquid is 1-butyl-1-crassitude dintrile amine salt (BMPDCA), and BMPDCA purity is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, negative electrode is made with platinized platinum (1.0cm × 1.0cm × 0.2cm), graphite makees anode, to keep die opening be 1cm, electrolysis temperature is 40 DEG C, stir speed (S.S.) is 300r/min, and use control flume pressure for electro-deposition 1h under the conditions of 3.00V and in the ionic liquid electroplate liquid that step (1) prepares, can prepare lanthanoid metal at cathode surface, gained lanthanum sedimentary average grain size is 100nm, as shown in Figures 3 and 4.
Embodiment 3
The method that this dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, it specifically comprises the following steps that
(1) ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid, the wherein volume of dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Mass ratio be 100:1ml/g, M in dicyandiamide type ionic liquid MDCA is 1-ethyl-3-methylimidazole ionic liquid cation, this dicyandiamide type ionic liquid is 1-ethyl-3-methylimidazole dicyandiamide salt, and 1-ethyl-3-methylimidazole dicyandiamide purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, makees negative electrode with platinized platinum, and anode made by platinized platinum, electrolysis temperature be 60 DEG C, stir speed (S.S.) be 200r/min, and to use controlling potential be (-0.80V vs.Ag/Ag+Electro-deposition 3h under the conditions of) and in the ionic liquid electroplate liquid that step (1) prepares, can prepare lanthanoid metal at cathode surface.
Embodiment 4
The method that this dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, it specifically comprises the following steps that
(1) ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid, the wherein volume of dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Mass ratio be 100:3ml/g, M in dicyandiamide type ionic liquid MDCA is 1-ethyl-1-methylpyrrole ionic liquid cation, this dicyandiamide type ionic liquid is 1-ethyl-3-methylpyrrole dicyandiamide salt, and 1-ethyl-3-methylpyrrole dicyandiamide purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, makees negative electrode with platinized platinum, and inert anode makees anode, electrolysis temperature be 50 DEG C, stir speed (S.S.) be 150r/min, and to use controlling potential be (-1.15V vs.Ag/Ag+Electro-deposition 1h under the conditions of) and in the ionic liquid electroplate liquid that step (1) prepares, can prepare lanthanoid metal at cathode surface.
Embodiment 5
The method that this dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, it specifically comprises the following steps that
(1) ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid, the wherein volume of dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Mass ratio be 100:2ml/g, M in dicyandiamide type ionic liquid MDCA is 1-butyl-3-methylpyrrole ionic liquid cation, this dicyandiamide type ionic liquid is 1-butyl-3-methylpyrrole dicyandiamide salt, and 1-butyl-3-methylpyrrole dicyandiamide purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, negative electrode is made with platinized platinum, graphite makees anode, electrolysis temperature be 45 DEG C, stir speed (S.S.) be 220r/min, and to use controlling potential be groove pressure for electro-deposition 1h under the conditions of 2.80V and in the ionic liquid electroplate liquid that step (1) prepares, lanthanoid metal can be prepared at cathode surface.
Embodiment 6
The method that this dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, it specifically comprises the following steps that
(1) ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid, the wherein volume of dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Mass ratio be 100:4ml/g, M in dicyandiamide type ionic liquid MDCA is 1-ethyl-3-picoline ionic liquid cation, this dicyandiamide type ionic liquid is 1-ethyl-3-picoline dicyandiamide salt, and 1-ethyl-3-picoline dicyandiamide purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, negative electrode is made with platinized platinum, graphite makees anode, electrolysis temperature be 30 DEG C, stir speed (S.S.) be 100r/min, and use control flume pressure for electro-deposition 1h under the conditions of 3.20V and in the ionic liquid electroplate liquid that step (1) prepares, lanthanoid metal can be prepared at cathode surface.
Embodiment 7
The method that this dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, it specifically comprises the following steps that
(1) ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid, the wherein volume of dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Mass ratio be 100:4ml/g, M in dicyandiamide type ionic liquid MDCA is 1-butyl-3-picoline ionic liquid cation, this dicyandiamide type ionic liquid is 1-butyl-3-picoline dicyandiamide salt, and 1-butyl-3-picoline dicyandiamide purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, makees negative electrode with platinized platinum (1.0cm × 1.0cm × 0.2cm), and graphite makees anode, electrolysis temperature be 40 DEG C, stir speed (S.S.) is 180r/min, and uses that to control electric current be 2mA cm-2Under the conditions of and in the ionic liquid electroplate liquid that step (1) prepares electro-deposition 1h, lanthanoid metal can be prepared at cathode surface.
Embodiment 8
The method that this dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, it specifically comprises the following steps that
(1) ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid, the wherein volume of dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Mass ratio be 100:2ml/g, the M in dicyandiamide type ionic liquid MDCA is tetramethyl ammonium ionic liquid cation, and this dicyandiamide type ionic liquid is tetramethyl-ammonium dicyandiamide salt, and tetramethyl-ammonium dicyandiamide purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, makees negative electrode with platinized platinum (1.0cm × 1.0cm × 0.2cm), and graphite makees anode, electrolysis temperature be 45 DEG C, stir speed (S.S.) is 280r/min, and uses that to control electric current be 8mA cm-2Under the conditions of and in the ionic liquid electroplate liquid that step (1) prepares electro-deposition 3h, lanthanoid metal can be prepared at cathode surface.
Embodiment 9
The method that this dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, it specifically comprises the following steps that
(1) ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid, the wherein volume of dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Mass ratio be 100:4ml/g, the M in dicyandiamide type ionic liquid MDCA is tetraethyl ammonium ionic liquid cation, and this dicyandiamide type ionic liquid is tetraethyl ammonium dicyandiamide salt, and tetraethyl ammonium dicyandiamide purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, makees negative electrode with platinized platinum (1.0cm × 1.0cm × 0.2cm), and graphite makees anode, electrolysis temperature be 40 DEG C, stir speed (S.S.) is 250r/min, and uses that to control electric current be 5mA cm-2Under the conditions of and in the ionic liquid electroplate liquid that step (1) prepares electro-deposition 1.5h, lanthanoid metal can be prepared at cathode surface.
Embodiment 10
The method that this dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, it specifically comprises the following steps that
(1) ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid, the wherein volume of dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Mass ratio be 100:3ml/g, the M in dicyandiamide type ionic liquid MDCA is 4-butyl ammonium ionic liquid cation, and this dicyandiamide type ionic liquid is TBuA dicyandiamide salt, and TBuA dicyandiamide purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, makees negative electrode with platinized platinum (1.0cm × 1.0cm × 0.2cm), and graphite makees anode, electrolysis temperature be 50 DEG C, stir speed (S.S.) is 100r/min, and uses that to control electric current be 7mA cm-2Under the conditions of and in the ionic liquid electroplate liquid that step (1) prepares electro-deposition 3h, lanthanoid metal can be prepared at cathode surface.
Claims (3)
1. the method that a dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal, it is characterised in that specifically comprise the following steps that
(1) ionic liquid electroplate liquid is prepared: under an inert atmosphere, by dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Dissolve mix homogeneously and form ionic liquid electroplate liquid, the wherein volume of dicyandiamide type ionic liquid MDCA and anhydrous LaCl3Mass ratio be 100:(1~5) ml/g;
(2) lanthanoid metal is prepared in electro-deposition: under an inert atmosphere, makees negative electrode, graphite or inert anode with platinized platinum and makees anode, electrolysis temperature be 25~60 DEG C, stir speed (S.S.) be 100~300r/min, and to use controlling potential be-0.80~-1.15V(vs.Ag/Ag+) or groove pressure be 2.80~3.20V under the conditions of and electro-deposition 1~3h in the ionic liquid electroplate liquid that step (1) prepares, lanthanoid metal can be prepared at cathode surface.
The method that dicyandiamide ionic liquid low-temperature electro-deposition the most according to claim 1 prepares lanthanoid metal, it is characterised in that: the M in described dicyandiamide type ionic liquid MDCA is ionic liquid cation.
The method that dicyandiamide ionic liquid low-temperature electro-deposition the most according to claim 2 prepares lanthanoid metal, it is characterised in that: described ionic liquid cation is 1-ethyl-3-methylimidazole, 1-butyl-3-Methylimidazole., 1-ethyl-1-methylpyrrole, 1-butyl-1-methylpyrrole, 1-ethyl-3-picoline, 1-butyl-3-picoline, tetramethyl ammonium, tetraethyl ammonium salt or 4-butyl ammonium.
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