CN116536711A - Method for preparing metal lithium magnesium alloy by using organic solvent electrodeposition - Google Patents
Method for preparing metal lithium magnesium alloy by using organic solvent electrodeposition Download PDFInfo
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- CN116536711A CN116536711A CN202310817619.0A CN202310817619A CN116536711A CN 116536711 A CN116536711 A CN 116536711A CN 202310817619 A CN202310817619 A CN 202310817619A CN 116536711 A CN116536711 A CN 116536711A
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- Prior art keywords
- dmi
- imidazolidinone
- dimethyl
- lithium
- lithium chloride
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- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 43
- 239000003960 organic solvent Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 11
- 239000002184 metal Substances 0.000 title claims abstract description 11
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 216
- CYSGHNMQYZDMIA-UHFFFAOYSA-N 1,3-Dimethyl-2-imidazolidinon Chemical compound CN1CCN(C)C1=O CYSGHNMQYZDMIA-UHFFFAOYSA-N 0.000 claims abstract description 117
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910052802 copper Inorganic materials 0.000 claims abstract description 78
- 239000010949 copper Substances 0.000 claims abstract description 78
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 61
- 238000003756 stirring Methods 0.000 claims abstract description 51
- 239000003792 electrolyte Substances 0.000 claims abstract description 40
- 159000000003 magnesium salts Chemical class 0.000 claims abstract description 33
- 238000004140 cleaning Methods 0.000 claims abstract description 26
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 55
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 26
- 239000008151 electrolyte solution Substances 0.000 claims description 15
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract 1
- 239000001989 lithium alloy Substances 0.000 description 10
- 229910000733 Li alloy Inorganic materials 0.000 description 9
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 238000003723 Smelting Methods 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- OTCKOJUMXQWKQG-UHFFFAOYSA-L magnesium bromide Chemical compound [Mg+2].[Br-].[Br-] OTCKOJUMXQWKQG-UHFFFAOYSA-L 0.000 description 2
- 229910001623 magnesium bromide Inorganic materials 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910001148 Al-Li alloy Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 229910001234 light alloy Inorganic materials 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/24—Alloys obtained by cathodic reduction of all their ions
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to the field of metallurgy, and particularly relates to a method for preparing a metal lithium magnesium alloy by using organic solvent electrodeposition, which comprises the following steps: s1, dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, putting a 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with lithium chloride into an electrolytic tank, adding magnesium salt into the electrolyte, and continuously stirring until uniform electrolyte with good fluidity is obtained; s2, using a copper sheet as a cathode, controlling the temperature of a system to be 25-100 ℃, controlling the electrolytic voltage range to be-2.5 to-3.5V vs Ag, and electrolyzing in the electrolyte for 1-4 h in the S1; and S3, taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode. The invention uses the organic solvent to carry out electrodeposition, can reduce the production energy consumption, reduce the corrosion to equipment and is easy to operate.
Description
Technical Field
One or more embodiments of the present specification relate to the field of metallurgical technology, and more particularly, to a method for preparing a metallic lithium magnesium alloy using organic solvent electrodeposition.
Background
The magnesium-lithium alloy is the lightest alloy structural material in the world at present, and has the density of 0.95 g/cm 3 ~1.65g/cm 3 Also known as ultra-light alloys. The magnesium-lithium alloy has extremely high specific rigidity, specific strength, excellent anti-seismic performance and high-energy particle penetration resistance, and in addition, the density of the magnesium-lithium alloy is far smaller than that of an aviation material aluminum-lithium alloy, so that after the magnesium-lithium alloy is developed, the magnesium-lithium alloy is widely applied to the fields of automobiles, electronic industry, medical equipment, weapon industry, nuclear industry, aviation, aerospace and the like and becomes one of structural materials with great application potential. Meanwhile, the preparation of the magnesium-lithium alloy is difficult, firstly, raw materials are easy to oxidize and burn, and danger occurs; secondly, the difference of melting points of magnesium and lithium is large, and the melting point of lithium is only 180 ℃. Because of the difficulty in smelting the magnesium-lithium alloy, the process is complex, the application range of mechanical properties is not clear, and research on the magnesium-lithium alloy is started in China from the 90 th century.
At present, common methods for preparing magnesium-lithium alloy are as follows: flux-shielded smelting (e.g., licl+lif shielding), gas-shielded smelting (e.g., ar, SF) 6 +CO 2 Protection), vacuum induction-resistance furnace smelting (vacuumizing first, then introducing Ar), molten salt electrolysis method and the like. The smelting method has higher requirement on metal purity, high cost and common protective atmosphere SF 6 And CO 2 Is a greenhouse gas, is not environment-friendly enough, and the higher operation temperature of molten salt electrolysis requires larger energy consumption in the preparation process, and is complex to operate. Many researchers have focused on producing metals and their alloys at or near room temperature. The standard electrode potential of lithium is-3.02V, the standard electrode potential of magnesium is-2.38V, which is negative than the potential of hydrogen, if deposited in aqueous solution, hydrogen gas will be separated out, severely interfering with the deposition of lithium magnesium alloy, so electrodeposition of lithium (magnesium) coating can only be performed in nonaqueous electrolyte systems.
In view of the foregoing, the present application now proposes a method for preparing a metallic lithium magnesium alloy using organic solvent electrodeposition to solve the above-mentioned problems.
Disclosure of Invention
The present invention is directed to solving the problems occurring in the prior art, and one or more embodiments of the present specification are directed to a method for preparing a lithium magnesium alloy by low-temperature electrolysis using 1, 3-dimethyl-2-imidazolidinone (DMI) (purity greater than 99.0%) as an organic solvent, which has a good prospect in the electrodeposition field of metals and alloys thereof, with anhydrous lithium chloride (purity greater than 99.0%), anhydrous magnesium chloride (purity greater than 99.0%) and magnesium bromide (purity greater than 98.0%) as raw materials.
In view of the above objects, one or more embodiments of the present specification provide a method for preparing a metallic lithium magnesium alloy using organic solvent electrodeposition, including the steps of:
s1, dissolving anhydrous lithium chloride in an organic solvent 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.02-1 mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium salt into the electrolytic solution, and continuously stirring until the uniform and good-fluidity electrolytic solution is obtained, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.01-0.5 mol/L;
s2, using a copper sheet as a cathode, controlling the temperature of a system to be 25-100 ℃, controlling the electrolytic voltage range to be-2.5-3.5V vs Ag, and electrolyzing in the electrolyte for 1-4 h in the S1;
and S3, taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
In the method for preparing the metal lithium magnesium alloy by using the organic solvent electrodeposition provided by the embodiment of the invention, in the step S1, the magnesium salt is magnesium chloride.
In the method for preparing the metal lithium magnesium alloy by using the organic solvent electrodeposition, in the step S1, the molar concentration of lithium chloride is 0.01-1 mol/L.
In the method for preparing the metal lithium magnesium alloy by using the organic solvent electrodeposition, in the step S1, the molar concentration of the magnesium salt is 0.01-0.5 mol/L.
In the embodiment of the invention, the reaction occurring on the cathode in the electrolytic process is that
According to the above, the invention has the following beneficial effects:
compared with high-temperature molten salt electrolysis, the invention can reduce the production energy consumption, reduce the corrosion to equipment and is easy to operate. In addition, the raw materials used in the scheme of the invention are relatively cheap, and compared with the existing preparation process of the lithium magnesium alloy, the method can improve the yield of the alloy and reduce the production cost.
Drawings
For a clearer description of one or more embodiments of the present description or of the solutions of the prior art, the drawings that are necessary for the description of the embodiments or of the prior art will be briefly described, it being apparent that the drawings in the description below are only one or more embodiments of the present description, from which other drawings can be obtained, without inventive effort, for a person skilled in the art.
FIG. 1 shows DMI-0.02mol/L LiCl-0.01mol/L MgCl 2 Electrolyzing 2h by-3.1V vs. Ag at 80 ℃ in the system to obtain an SEM image of the product;
FIG. 2 shows DMI-0.1mol/L LiCl-0.05mol/L MgCl 2 Electrolyzing the silver powder at 80 ℃ with-3.1V vs. Ag for 2 hours to obtain an SEM image of a product;
FIG. 3 shows DMI-0.2mol/L LiCl-0.1mol/L MgCl 2 Electrolyzing the silver powder at 80 ℃ with-3.1V vs. Ag for 2 hours to obtain an SEM image of a product;
FIG. 4 shows DMI-0.4mol/L LiCl-0.2mol/L MgCl 2 Electrolyzing the silver powder at 80 ℃ with-3.1V vs. Ag for 2 hours to obtain an SEM image of a product;
FIG. 5 shows DMI-0.6mol/L LiCl-0.3mol/L MgCl 2 Electrolyzing the silver powder at 80 ℃ with-3.1V vs. Ag for 2 hours to obtain an SEM image of a product;
FIG. 6 shows DMI-0.8mol/L LiCl-0.4mol/L MgCl 2 The SEM image of the product is obtained by electrolyzing the-3.1V vs. Ag for 2 hours at 80 ℃ in the system.
Detailed Description
For the purposes of promoting an understanding of the principles and advantages of the disclosure, reference will now be made in detail to the following specific examples.
The experimental methods described in the following examples, unless otherwise specified, are all conventional: the reagents and materials, unless otherwise specified, are commercially available.
The purity of 1, 3-dimethyl-2-imidazolidinone (DMI) adopted in the embodiment of the invention is 99.0%, the purity of lithium chloride is 99.0%, the purity of magnesium chloride is 99.0%, and the purity of magnesium bromide is 98.0%.
In the embodiment of the invention, an Shanghai Chenhua electrochemical workstation is used as an electrolysis power supply.
In the embodiment of the invention, a Czech Quanta 250FEG microscope is adopted to analyze the morphology and the components of the lithium magnesium alloy.
Example 1
Referring to fig. 1-6, at room temperature, dissolving anhydrous lithium chloride in an organic solvent 1, 3-dimethyl-2-imidazolidinone (DMI), wherein the molar concentration of lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.02mol/L, placing the DMI solution added with lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuing stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.01 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 80 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 2
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.1mol/L, placing the DMI solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolytic solution, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.05 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 80 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 3
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.2mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.1 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 80 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 4
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4mol/L, placing the DMI solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolytic solution, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.2 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 80 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 5
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.6mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.3 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 80 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 6
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, placing the DMI solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolytic solution, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; using a copper sheet as a cathode, controlling the temperature of a system to be 80 ℃ and the voltage to be-3.1V vs Ag for electrolysis for 2 hours; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 7
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, placing the DMI solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolytic solution, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; using a copper sheet as a cathode, controlling the temperature of a system to be 80 ℃ and the voltage to be-3.1V vs Ag for electrolysis for 2 hours; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 8
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 25 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 9
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, placing the DMI solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolytic solution, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 30 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 10
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, placing the DMI solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolytic solution, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 40 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 11
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 50 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 12
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the DMI is 0.8mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolytic solution, and continuously stirring to obtain an electrolytic solution with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 60 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 13
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 70 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 14
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 90 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 15
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, placing the DMI solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolytic solution, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 100 ℃, and the voltage is-3.1V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 16
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, placing the DMI solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolytic solution, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 80 ℃, and the voltage is-2.5V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 17
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 80 ℃, and the voltage is-2.7V vs Ag electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 18
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 80 ℃, and the voltage is-2.9V vs Ag for electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 19
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 80 ℃, and the voltage is-3.3V vs Ag for electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 20
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the DMI is 0.8mol/L, placing the DMI solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 80 ℃, and the voltage is-3.5V vs Ag for electrolysis 2h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using DMI to obtain the lithium magnesium alloy deposited on the surface of the cathode.
Example 21
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 80 ℃, and the voltage is-3.1V vs Ag electrolysis 1 h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 22
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, placing the DMI solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolytic solution, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; using a copper sheet as a cathode, controlling the temperature of a system to be 80 ℃ and the voltage to be-3.1V vs Ag for electrolysis 3 h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
Example 23
Dissolving anhydrous lithium chloride in an organic solvent of 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.8mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium chloride into the electrolyte, and continuously stirring to obtain an electrolyte with good uniform fluidity, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.4 mol/L; copper sheet is used as a cathode, the temperature of the system is controlled to be 80 ℃, and the voltage is-3.1V vs Ag electrolysis 4h; and taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
The present disclosure is intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Any omissions, modifications, equivalents, improvements, and the like, which are within the spirit and principles of the one or more embodiments of the disclosure, are therefore intended to be included within the scope of the disclosure.
Table 1 shows the molar concentration of lithium chloride in 1, 3-dimethyl-2-imidazolidinone (DMI), the molar concentration of magnesium salt, the current efficiency of the electrolysis, the temperature of the electrolysis, the voltage and the electrolysis time in examples 1-23. As can be seen from the results in table 1, the current efficiency increases and decreases with increasing concentration, and the current efficiency of example 6 is 80% at the highest; the electrolysis temperature is preferably 80℃and the time is preferably 2 hours.
TABLE 1 Effect of electrolytic process variations on Current efficiency results
| Lithium chloride in DMI Molar concentration mol/L | Magnesium chloride in DMI Molar concentration mol/L | Electrolysis voltage V （vs Ag） | Electrolysis temperature Degree (. Degree. C.) | During electrolysis Interval (h) | Electric current effect Rate η (%) | Magnesium content At（%） | Lithium content At（%） | |
| Implementation of the embodiments Example 1 | 0.02 | 0.01 | -3.1 | 80 | 2 | 10 | 96.5 | 3.5 |
| Implementation of the embodiments Example 2 | 0.1 | 0.05 | -3.1 | 80 | 2 | 20 | 95.8 | 4.2 |
| Implementation of the embodiments Example 3 | 0.2 | 0.1 | -3.1 | 80 | 2 | 30 | 93.3 | 6.7 |
| Implementation of the embodiments Example 4 | 0.4 | 0.2 | -3.1 | 80 | 2 | 60 | 90.6 | 9.4 |
| Implementation of the embodiments Example 5 | 0.6 | 0.3 | -3.1 | 80 | 2 | 70 | 86.7 | 13.3 |
| Implementation of the embodiments Example 6 | 0.8 | 0.4 | -3.1 | 80 | 2 | 80 | 80.5 | 19.5 |
| Implementation of the embodiments Example 7 | 1.0 | 0.5 | -3.1 | 80 | 2 | 65 | 87.2 | 12.8 |
| Implementation of the embodiments Example 8 | 0.8 | 0.4 | -3.1 | 25 | 2 | 60 | 94.6 | 5.4 |
| Implementation of the embodiments Example 9 | 0.8 | 0.4 | -3.1 | 30 | 2 | 65 | 94.1 | 5.9 |
| Implementation of the embodiments Example 10 | 0.8 | 0.4 | -3.1 | 40 | 2 | 66 | 92.7 | 7.3 |
| Implementation of the embodiments Example 11 | 0.8 | 0.4 | -3.1 | 50 | 2 | 68 | 91.5 | 8.5 |
| Implementation of the embodiments Example 12 | 0.8 | 0.4 | -3.1 | 60 | 2 | 69 | 90.3 | 9.7 |
| Implementation of the embodiments Example 13 | 0.8 | 0.4 | -3.1 | 70 | 2 | 72 | 89.8 | 10.2 |
| Implementation of the embodiments Example 14 | 0.8 | 0.4 | -3.1 | 90 | 2 | 78 | 88.5 | 11.5 |
| Implementation of the embodiments Example 15 | 0.8 | 0.4 | -3.1 | 100 | 2 | 77 | 88.1 | 11.9 |
| Implementation of the embodiments Example 16 | 0.8 | 0.4 | -2.5 | 80 | 2 | 74 | 93.5 | 6.5 |
| Implementation of the embodiments Example 17 | 0.8 | 0.4 | -2.7 | 80 | 2 | 75 | 92.5 | 7.5 |
| Implementation of the embodiments Example 18 | 0.8 | 0.4 | -2.9 | 80 | 2 | 77 | 90.6 | 9.4 |
| Implementation of the embodiments Example 19 | 0.8 | 0.4 | -3.3 | 80 | 2 | 78 | 87.1 | 12.9 |
| Implementation of the embodiments Example 20 | 0.8 | 0.4 | -3.5 | 80 | 2 | 77 | 83.2 | 16.8 |
| Implementation of the embodiments Example 21 | 0.8 | 0.4 | -3.1 | 80 | 1 | 70 | 91.3 | 8.7 |
| Implementation of the embodiments Example 22 | 0.8 | 0.4 | -3.1 | 80 | 3 | 76 | 85.4 | 14.6 |
| Implementation of the embodiments Example 23 | 0.8 | 0.4 | -3.1 | 80 | 4 | 73 | 82.2 | 17.8 |
Claims (4)
1. A method for preparing a metallic lithium magnesium alloy by using organic solvent electrodeposition, which is characterized by comprising the following steps:
s1, dissolving anhydrous lithium chloride in an organic solvent 1, 3-dimethyl-2-imidazolidinone (DMI) at room temperature, wherein the molar concentration of the lithium chloride in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.02-1 mol/L, putting the 1, 3-dimethyl-2-imidazolidinone (DMI) solution added with the lithium chloride into an electrolytic tank, stirring until the lithium chloride is completely dissolved, adding magnesium salt into the electrolytic solution, and continuously stirring until the uniform and good-fluidity electrolytic solution is obtained, wherein the molar concentration of the magnesium salt in the 1, 3-dimethyl-2-imidazolidinone (DMI) is 0.01-0.5 mol/L;
s2, using a copper sheet as a cathode, controlling the temperature of a system to be 25-100 ℃, controlling the electrolytic voltage range to be-2.5-3.5V vs Ag, and electrolyzing 1-4 h in the electrolyte in S1;
and S3, taking out the copper sheet after the electrolysis is finished, and cleaning the copper sheet by using 1, 3-dimethyl-2-imidazolidinone (DMI) to obtain the lithium-magnesium alloy deposited on the surface of the cathode.
2. The method for preparing a lithium magnesium alloy according to claim 1, wherein the magnesium salt used in the step S1 is magnesium chloride.
3. The method for preparing a metal lithium magnesium alloy by using organic solvent electrodeposition according to claim 1, wherein in the step S1, the molar concentration of lithium chloride is 0.01-1 mol/L.
4. The method for preparing a metal lithium magnesium alloy by using organic solvent electrodeposition according to claim 1, wherein in the step S1, the molar concentration of magnesium salt is 0.01-0.5 mol/L.
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