CN103540974A - Method for preparing metal lanthanum through dicyandiamide ionic liquid low-temperature electro-deposition - Google Patents
Method for preparing metal lanthanum through dicyandiamide ionic liquid low-temperature electro-deposition Download PDFInfo
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- CN103540974A CN103540974A CN201310477746.7A CN201310477746A CN103540974A CN 103540974 A CN103540974 A CN 103540974A CN 201310477746 A CN201310477746 A CN 201310477746A CN 103540974 A CN103540974 A CN 103540974A
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- 239000002608 ionic liquid Substances 0.000 title claims abstract description 124
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 65
- 239000002184 metal Substances 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims abstract description 29
- 229910052746 lanthanum Inorganic materials 0.000 title abstract description 10
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 title abstract description 10
- 238000004070 electrodeposition Methods 0.000 title abstract 4
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 title abstract 3
- 239000007788 liquid Substances 0.000 claims abstract description 43
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 20
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 12
- 239000010439 graphite Substances 0.000 claims abstract description 12
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 54
- 150000002602 lanthanoids Chemical class 0.000 claims description 54
- 230000008021 deposition Effects 0.000 claims description 18
- 150000002500 ions Chemical class 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical compound CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 claims description 6
- QQAJQOSQIHCXPL-UHFFFAOYSA-N 1-butyl-3-methyl-2h-pyridine Chemical compound CCCCN1CC(C)=CC=C1 QQAJQOSQIHCXPL-UHFFFAOYSA-N 0.000 claims description 5
- ITIABACYRWQDBU-UHFFFAOYSA-N C(C)N1CC(=CC=C1)C Chemical compound C(C)N1CC(=CC=C1)C ITIABACYRWQDBU-UHFFFAOYSA-N 0.000 claims description 5
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 claims description 5
- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical compound CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 claims description 4
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical class CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 claims description 4
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 238000009713 electroplating Methods 0.000 abstract 3
- 229910002249 LaCl3 Inorganic materials 0.000 abstract 1
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 description 25
- 239000012535 impurity Substances 0.000 description 11
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 5
- FVBSUVNLJBVTLB-UHFFFAOYSA-N 1-butyl-3-methylpyrrole Chemical compound CCCCN1C=CC(C)=C1 FVBSUVNLJBVTLB-UHFFFAOYSA-N 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- LPRJTTSNPNSAEB-UHFFFAOYSA-N 1-ethyl-3-methylpyrrole Chemical compound CCN1C=CC(C)=C1 LPRJTTSNPNSAEB-UHFFFAOYSA-N 0.000 description 2
- -1 amine salt Chemical class 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002466 imines Chemical class 0.000 description 2
- 150000002603 lanthanum Chemical class 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001449 anionic compounds Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002891 organic anions Chemical class 0.000 description 1
- 150000002892 organic cations Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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Abstract
The invention relates to a method for preparing metal lanthanum through dicyandiamide ionic liquid low-temperature electro-deposition, and belongs to the technical field of metallurgy and material preparation. According to the invention, first, an ionic liquid electroplating liquid is prepared, wherein under an inert atmosphere, dicyandiamide ionic liquid MDCA and anhydrous LaCl3 are dissolved and uniformly mixed for form the ionic liquid electroplating liquid; and metal lanthanum is prepared through electro-deposition, wherein under an inert atmosphere, a platinum sheet is adopted as a cathode and graphite or an inert anode is adopted as an anode; and electro-deposition is carried out for 1-3h in the ionic liquid electroplating liquid prepared in the previous step, such that metal lanthanum can be obtained on the surface of the cathode. Because of low electrolysis temperature, the method has the advantages of low energy consumption, high current efficiency, short production process, low pollution, simple process, high product added value, and the like.
Description
Technical field
The present invention relates to a kind of Dyhard RU 100 ionic liquid low temp. electric deposition and prepare the method for lanthanoid metal, belong to metallurgy and technical field of material.
Background technology
Rare earth lanthanum is widely used in preparing the functional materialss 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.Fused 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.Under the severe situation of energy shortage, Greenhouse effect aggravation, how realizing energy-saving and emission-reduction and green production prepared by lanthanoid metal is key issue urgently to be resolved hurrily.Although fused salt electrolysis process has some technological improvements in recent years, the energy consumption of industrial production lanthanum decreases, and years of researches and facts have proved are improved and can not be made energy consumption significantly decline existing technique.Therefore, the low-temperature electrolytic novel preparation method of research and development lanthanoid metal, to significantly reducing its production energy consumption from source, reducing discharge, has caused the extensive concern of researcher.
Ionic liquid is that a kind of room temperature consisting of ion is completely melted salt, conventionally the asymmetric organic cation of geometry and inorganic or organic anion, consists of.With other solvent phase ratio, ionic liquid shows unique physicochemical property and distinctive function, has the characteristics such as quality is light, nontoxic, non-combustible, steam forces down, chemical heat stability is high, heat-conductivity conducting is good, electrochemical window wide (being generally greater than 4V).Ionic liquid is a kind of desirable room temperature liquid electrolyte, it has merged the advantage of high-temperature molten salt and the aqueous solution: have wider electrochemical window, at room temperature can obtain ability galvanic deposit obtains in high-temperature molten salt metal and alloy, and there is no the such severe corrosive of high-temperature molten salt.Utilizing ionic liquid to prepare lanthanoid metal can be controlled at electrolysis temperature below 100 ℃, thereby 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, realize energy-saving and emission-reduction and green production prepared by lanthanoid metal.
Document (Rare Metals Materials and engineering, 2012,41,599-602) reported employing 1-ethyl-3-methylimidazole a tetrafluoro borate (BMIMBF
4) ionic liquid is that solvent ionogen can be prepared lanthanoid metal.This report emphasis is pointed out, as a kind of typical neutral ion liquid, BMIMBF
4very low to the solubleness of metal halogen, therefore add anhydrous LiCl to improve electrolyte system to lanthanum salt precursor body (LaCl
3) solubleness most important for the electrolytic deposition of lanthanoid metal.But the LiCl salt itself that the method adopts also belongs to metal halogen, limited in one's ability aspect raising system solubleness, and anhydrous LiCl cost is expensive.
Apply for a patent (number of patent application 201110435737.2) disclose a kind of in ionic liquid the method for electrodepositing metal lanthanum, using 1-methyl-3-ethyl imidazol(e) two (trimethyl fluoride sulfonyl) imines as ionogen, anhydrous LaCl
3for lanthanum salt precursor body, copper sheet, as negative electrode, is usingd platinum, graphite or titanium-based oxide as anode, and galvanostatic deposition is prepared lanthanoid metal.This application patent adopts 1-methyl-3-ethyl imidazol(e) two (trimethyl fluoride sulfonyl) imines neutral ion liquid as ionogen, has equally the above-mentioned very low problem of metal halogen solubleness of mentioning.This patent is not set forth this key issue, and its gained cathode product is not carried out to material phase analysis yet, causes and cannot determine that its product is lanthanoid metal.
Summary of the invention
The problem and the deficiency that for above-mentioned prior art, exist, the invention provides a kind of method that Dyhard RU 100 ionic liquid low temp. electric deposition is prepared lanthanoid metal.While verifying 25 ℃ due to experiment, anhydrous LaCl
3saturation solubility in Dyhard RU 100 type ionic liquid MDCA is not less than 2.5g/100g, therefore adopts and is dissolved with LaCl
3 dyhard RU 100 ionic liquid as electroplate liquid galvanic deposit prepare lanthanoid metal, the present invention is achieved through the following technical solutions.
Dyhard RU 100 ionic liquid low temp. electric deposition is prepared a method for lanthanoid metal, and its concrete steps are as follows:
(1) prepare ionic liquid electroplate liquid: under inert atmosphere, by Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3dissolving mixes and forms ionic liquid electroplate liquid, the wherein volume of Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3mass ratio be 100:(1～5) ml/g;
(2) lanthanoid metal is prepared in galvanic deposit: under inert atmosphere, with platinized platinum, make negative electrode, graphite or inert anode are made anode, at electrolysis temperature, is that 25～60 ℃, stir speed (S.S.) are 100～300r/min, and adopts that to control current potential be (0.80～-1.15V
Vs.Ag/Ag
+), groove is pressed is that 2.80～3.20V or electric current are 2～8mA ﹒ cm
-2galvanic deposit 1～3h under condition and in the ionic liquid electroplate liquid preparing in step (1), can prepare lanthanoid metal at cathode surface.
M in described Dyhard RU 100 type ionic liquid MDCA is ionic liquid positively charged ion, 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 Dyhard RU 100 type ionic liquid MDCA purity is 99%, containing 1% moisture and other impurity.
The invention has the beneficial effects as follows: present method is because electrolysis temperature is lower to have that energy consumption is low, current efficiency is high, Production Flow Chart 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 preparations;
Fig. 4 is the XRD figure of the lanthanoid metal of the embodiment of the present invention 2 preparations.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
This Dyhard RU 100 ionic liquid low temp. electric deposition is prepared the method for lanthanoid metal, and its concrete steps are as follows:
(1) prepare ionic liquid electroplate liquid: under inert atmosphere, by Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3dissolving mixes and forms ionic liquid electroplate liquid, the wherein volume of Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3mass ratio be 100:2.5ml/g, M in Dyhard RU 100 type ionic liquid MDCA is 1-butyl-3-Methylimidazole ionic liquid positively charged ion, this Dyhard RU 100 type ionic liquid is 1-butyl-3-Methylimidazole Dyhard RU 100 salt (BMIMDCA), and the purity of BMIMDCA is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in galvanic deposit: under inert atmosphere, with platinized platinum (1.0cm * 1.0cm * 0.2cm) make negative electrode, graphite is made anode, keeping interpole gap, be that 1cm, electrolysis temperature are that 25 ℃, stir speed (S.S.) are 100r/min, and adopt that to control current potential be (1.00V vs.Ag/Ag
+) galvanic deposit 2h under condition and in the ionic liquid electroplate liquid preparing in step (1), can prepare lanthanoid metal at cathode surface, gained lanthanum settled layer average grain size is 100nm, as illustrated in fig. 1 and 2.
Embodiment 2
This Dyhard RU 100 ionic liquid low temp. electric deposition is prepared the method for lanthanoid metal, and its concrete steps are as follows:
(1) prepare ionic liquid electroplate liquid: under inert atmosphere, by Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3dissolving mixes and forms ionic liquid electroplate liquid, the wherein volume of Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3mass ratio be 100:5ml/g, M in Dyhard RU 100 type ionic liquid MDCA is 1-butyl-1-methylpyrrole ionic liquid positively charged ion, this Dyhard RU 100 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 galvanic deposit: under inert atmosphere, with platinized platinum (1.0cm * 1.0cm * 0.2cm), make negative electrode, graphite is made anode, keeping interpole gap, be that 1cm, electrolysis temperature are that 40 ℃, stir speed (S.S.) are 300r/min, and adopt control flume to press as galvanic deposit 1h under 3.00V condition and in the ionic liquid electroplate liquid preparing in step (1), can prepare lanthanoid metal at cathode surface, gained lanthanum settled layer average grain size is 100nm, as shown in Figures 3 and 4.
Embodiment 3
This Dyhard RU 100 ionic liquid low temp. electric deposition is prepared the method for lanthanoid metal, and its concrete steps are as follows:
(1) prepare ionic liquid electroplate liquid: under inert atmosphere, by Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3dissolving mixes and forms ionic liquid electroplate liquid, the wherein volume of Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3mass ratio be 100:1ml/g, M in Dyhard RU 100 type ionic liquid MDCA is 1-ethyl-3-methylimidazole ionic liquid positively charged ion, this Dyhard RU 100 type ionic liquid is 1-ethyl-3-methylimidazole Dyhard RU 100 salt, 1-ethyl-3-methylimidazole Dyhard RU 100 purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in galvanic deposit: under inert atmosphere, with platinized platinum, make negative electrode, platinized platinum is made anode, at electrolysis temperature, is that 60 ℃, stir speed (S.S.) are 200r/min, and adopts that to control current potential be (0.80V vs.Ag/Ag
+) galvanic deposit 3h under condition and in the ionic liquid electroplate liquid preparing in step (1), can prepare lanthanoid metal at cathode surface.
Embodiment 4
This Dyhard RU 100 ionic liquid low temp. electric deposition is prepared the method for lanthanoid metal, and its concrete steps are as follows:
(1) prepare ionic liquid electroplate liquid: under inert atmosphere, by Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3dissolving mixes and forms ionic liquid electroplate liquid, the wherein volume of Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3mass ratio be 100:3ml/g, M in Dyhard RU 100 type ionic liquid MDCA is 1-ethyl-1-methylpyrrole ionic liquid positively charged ion, this Dyhard RU 100 type ionic liquid is 1-ethyl-3-methylpyrrole Dyhard RU 100 salt, 1-ethyl-3-methylpyrrole Dyhard RU 100 purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in galvanic deposit: under inert atmosphere, with platinized platinum, make negative electrode, inert anode is made anode, at electrolysis temperature, is that 50 ℃, stir speed (S.S.) are 150r/min, and adopts that to control current potential be (1.15V vs.Ag/Ag
+) galvanic deposit 1h under condition and in the ionic liquid electroplate liquid preparing in step (1), can prepare lanthanoid metal at cathode surface.
Embodiment 5
This Dyhard RU 100 ionic liquid low temp. electric deposition is prepared the method for lanthanoid metal, and its concrete steps are as follows:
(1) prepare ionic liquid electroplate liquid: under inert atmosphere, by Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3dissolving mixes and forms ionic liquid electroplate liquid, the wherein volume of Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3mass ratio be 100:2ml/g, M in Dyhard RU 100 type ionic liquid MDCA is 1-butyl-3-methylpyrrole ionic liquid positively charged ion, this Dyhard RU 100 type ionic liquid is 1-butyl-3-methylpyrrole Dyhard RU 100 salt, 1-butyl-3-methylpyrrole Dyhard RU 100 purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in galvanic deposit: under inert atmosphere, with platinized platinum, make negative electrode, graphite is made anode, at electrolysis temperature, be that 45 ℃, stir speed (S.S.) are 220r/min, and adopt to control current potential and be groove and press as galvanic deposit 1h under 2.80V condition and in the ionic liquid electroplate liquid preparing in step (1), can prepare lanthanoid metal at cathode surface.
Embodiment 6
This Dyhard RU 100 ionic liquid low temp. electric deposition is prepared the method for lanthanoid metal, and its concrete steps are as follows:
(1) prepare ionic liquid electroplate liquid: under inert atmosphere, by Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3dissolving mixes and forms ionic liquid electroplate liquid, the wherein volume of Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3mass ratio be 100:4ml/g, M in Dyhard RU 100 type ionic liquid MDCA is 1-ethyl-3-picoline ionic liquid positively charged ion, this Dyhard RU 100 type ionic liquid is 1-ethyl-3-picoline Dyhard RU 100 salt, 1-ethyl-3-picoline Dyhard RU 100 purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in galvanic deposit: under inert atmosphere, with platinized platinum, make negative electrode, graphite is made anode, at electrolysis temperature, be that 30 ℃, stir speed (S.S.) are 100r/min, and adopt control flume to press as galvanic deposit 1h under 3.20V condition and in the ionic liquid electroplate liquid preparing in step (1), can prepare lanthanoid metal at cathode surface.
Embodiment 7
This Dyhard RU 100 ionic liquid low temp. electric deposition is prepared the method for lanthanoid metal, and its concrete steps are as follows:
(1) prepare ionic liquid electroplate liquid: under inert atmosphere, by Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3dissolving mixes and forms ionic liquid electroplate liquid, the wherein volume of Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3mass ratio be 100:4ml/g, M in Dyhard RU 100 type ionic liquid MDCA is 1-butyl-3-picoline ionic liquid positively charged ion, this Dyhard RU 100 type ionic liquid is 1-butyl-3-picoline Dyhard RU 100 salt, 1-butyl-3-picoline Dyhard RU 100 purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in galvanic deposit: under inert atmosphere, with platinized platinum (1.0cm * 1.0cm * 0.2cm), make negative electrode, graphite is made anode, at electrolysis temperature, is that 40 ℃, stir speed (S.S.) are 180r/min, and adopts that to control electric current be 2mA ﹒ cm
-2galvanic deposit 1h under condition and in the ionic liquid electroplate liquid preparing in step (1), can prepare lanthanoid metal at cathode surface.
Embodiment 8
This Dyhard RU 100 ionic liquid low temp. electric deposition is prepared the method for lanthanoid metal, and its concrete steps are as follows:
(1) prepare ionic liquid electroplate liquid: under inert atmosphere, by Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3dissolving mixes and forms ionic liquid electroplate liquid, the wherein volume of Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3mass ratio be 100:2ml/g, the M in Dyhard RU 100 type ionic liquid MDCA is tetramethyl ammonium ionic liquid positively charged ion, this Dyhard RU 100 type ionic liquid is tetramethyl-ammonium Dyhard RU 100 salt, tetramethyl-ammonium Dyhard RU 100 purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in galvanic deposit: under inert atmosphere, with platinized platinum (1.0cm * 1.0cm * 0.2cm), make negative electrode, graphite is made anode, at electrolysis temperature, is that 45 ℃, stir speed (S.S.) are 280r/min, and adopts that to control electric current be 8mA ﹒ cm
-2galvanic deposit 3h under condition and in the ionic liquid electroplate liquid preparing in step (1), can prepare lanthanoid metal at cathode surface.
Embodiment 9
This Dyhard RU 100 ionic liquid low temp. electric deposition is prepared the method for lanthanoid metal, and its concrete steps are as follows:
(1) prepare ionic liquid electroplate liquid: under inert atmosphere, by Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3dissolving mixes and forms ionic liquid electroplate liquid, the wherein volume of Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3mass ratio be 100:4ml/g, the M in Dyhard RU 100 type ionic liquid MDCA is tetraethyl ammonium salt ion liquid cation, this Dyhard RU 100 type ionic liquid is tetraethyl ammonium Dyhard RU 100 salt, tetraethyl ammonium Dyhard RU 100 purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in galvanic deposit: under inert atmosphere, with platinized platinum (1.0cm * 1.0cm * 0.2cm), make negative electrode, graphite is made anode, at electrolysis temperature, is that 40 ℃, stir speed (S.S.) are 250r/min, and adopts that to control electric current be 5mA ﹒ cm
-2galvanic deposit 1.5h under condition and in the ionic liquid electroplate liquid preparing in step (1), can prepare lanthanoid metal at cathode surface.
Embodiment 10
This Dyhard RU 100 ionic liquid low temp. electric deposition is prepared the method for lanthanoid metal, and its concrete steps are as follows:
(1) prepare ionic liquid electroplate liquid: under inert atmosphere, by Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3dissolving mixes and forms ionic liquid electroplate liquid, the wherein volume of Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3mass ratio be 100:3ml/g, the M in Dyhard RU 100 type ionic liquid MDCA is 4-butyl ammonium ionic liquid positively charged ion, this Dyhard RU 100 type ionic liquid is TBuA Dyhard RU 100 salt, TBuA Dyhard RU 100 purity salt is 99%, containing 1% moisture and other impurity;
(2) lanthanoid metal is prepared in galvanic deposit: under inert atmosphere, with platinized platinum (1.0cm * 1.0cm * 0.2cm), make negative electrode, graphite is made anode, at electrolysis temperature, is that 50 ℃, stir speed (S.S.) are 100r/min, and adopts that to control electric current be 7mA ﹒ cm
-2galvanic deposit 3h under condition and in the ionic liquid electroplate liquid preparing in step (1), can prepare lanthanoid metal at cathode surface.
Claims (2)
1. Dyhard RU 100 ionic liquid low temp. electric deposition is prepared a method for lanthanoid metal, it is characterized in that concrete steps are as follows:
(1) prepare ionic liquid electroplate liquid: under inert atmosphere, by Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3dissolving mixes and forms ionic liquid electroplate liquid, the wherein volume of Dyhard RU 100 type ionic liquid MDCA and anhydrous LaCl
3mass ratio be 100:(1～5) ml/g;
(2) lanthanoid metal is prepared in galvanic deposit: under inert atmosphere, with platinized platinum, make negative electrode, graphite or inert anode are made anode, at electrolysis temperature, is that 25～60 ℃, stir speed (S.S.) are 100～300r/min, and adopts that to control current potential be (0.80～-1.15V
Vs.Ag/Ag
+), groove is pressed is that 2.80～3.20V or electric current are 2～8mA ﹒ cm
-2galvanic deposit 1～3h under condition and in the ionic liquid electroplate liquid preparing in step (1), can prepare lanthanoid metal at cathode surface.
2. Dyhard RU 100 ionic liquid low temp. electric deposition according to claim 1 is prepared the method for lanthanoid metal, it is characterized in that: the M in described Dyhard RU 100 type ionic liquid MDCA is ionic liquid positively charged ion, 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310477746.7A CN103540974B (en) | 2013-10-14 | 2013-10-14 | A kind of method that dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310477746.7A CN103540974B (en) | 2013-10-14 | 2013-10-14 | A kind of method that dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanoid metal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103540974A true CN103540974A (en) | 2014-01-29 |
| CN103540974B CN103540974B (en) | 2016-10-19 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480492A (en) * | 2014-11-13 | 2015-04-01 | 昆明理工大学 | Method for preparing Ni-La alloy through ionic liquid electro-deposition |
| CN105803484A (en) * | 2014-12-31 | 2016-07-27 | 有研稀土新材料股份有限公司 | Preparation method of rare earth metal |
| CN106757215A (en) * | 2016-12-14 | 2017-05-31 | 昆明理工大学 | A kind of method that dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanum nickel alloy film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102433575A (en) * | 2011-12-22 | 2012-05-02 | 哈尔滨工业大学 | Method for electrodepositing metal lanthanum in ionic liquid |
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| CN102433575A (en) * | 2011-12-22 | 2012-05-02 | 哈尔滨工业大学 | Method for electrodepositing metal lanthanum in ionic liquid |
Non-Patent Citations (1)
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| MING-JAY DENG: "Electrodeposition of Nanostructured Sn in 1-ethyl-3-methylimidazolium Dicyanamide Room Temperature Ionic Liquid", <<ELECTROCHEMISTY>>, 8 June 2009 (2009-06-08) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480492A (en) * | 2014-11-13 | 2015-04-01 | 昆明理工大学 | Method for preparing Ni-La alloy through ionic liquid electro-deposition |
| CN105803484A (en) * | 2014-12-31 | 2016-07-27 | 有研稀土新材料股份有限公司 | Preparation method of rare earth metal |
| CN105803484B (en) * | 2014-12-31 | 2019-05-31 | 有研稀土新材料股份有限公司 | The preparation method of rare earth metal |
| CN106757215A (en) * | 2016-12-14 | 2017-05-31 | 昆明理工大学 | A kind of method that dicyandiamide ionic liquid low-temperature electro-deposition prepares lanthanum nickel alloy film |
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