CN113279015A - Method for preparing high-purity lithium by using double-chamber molten salt electrolytic cell based on solid electrolyte - Google Patents
Method for preparing high-purity lithium by using double-chamber molten salt electrolytic cell based on solid electrolyte Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/02—Electrolytic production, recovery or refining of metals by electrolysis of melts of alkali or alkaline earth metals
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/04—Diaphragms; Spacing elements
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
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Abstract
The invention belongs to the technical field of lithium metallurgy, and particularly relates to a method for preparing high-purity lithium by a double-chamber molten salt electrolytic cell based on solid electrolyte. The method specifically comprises the following steps: uniformly mixing dry LiCl and KCl in proportion, and adding into an anode chamber of a double-chamber molten salt electrolytic cell; adding a proper amount of metal lithium into the cathode chamber, heating the cathode chamber in an electrolytic cell until molten salt and the metal lithium are completely molten, maintaining the temperature of the electrolytic cell at 420-500 ℃, introducing direct current to start electrolysis, and starting a chlorine recovery system; the cathode plate of the cathode chamber obtains high-purity lithium, the invention utilizes the single lithium ion conductivity of the solid electrolyte to realize the automatic separation and outflow of the metal lithium and the fused salt, thereby avoiding impurity elements from entering the cathode chamber and greatly improving the product purity; the production process does not need manual lithium discharge, the sealing performance of the electrolytic cell is improved, continuous production can be realized, and the production efficiency is greatly improved.
Description
Technical Field
The invention relates to the technical field of lithium metallurgy, in particular to a method for preparing high-purity lithium by a double-chamber molten salt electrolytic cell based on solid electrolyte.
Background
Lithium is the lightest metal element in nature and has high activity. The lithium compound is widely applied to industries such as heat-resistant glass, ceramics, lithium lubricants and the like. Metallic lithium is attracting attention in the field of energy, and due to its excellent nuclear properties and thermal conductivity, it can be used for preparing tritium as a raw material for nuclear reactions, and also as a coolant for nuclear reactors; and the extremely high specific capacity and the low potential make the metallic lithium an ideal negative electrode material for a high-energy-density battery system. Therefore, lithium is known as "energy metal of the 21 st century". With the continuous development of new energy industry, people increasingly demand lithium metal.
Because of its active property, lithium exists in brine or rock mineral only in a compound state in nature, and the LiCl-KCl molten salt electrolysis method is mainly adopted to prepare metallic lithium industrially at present. The industrial lithium electrolytic cell adopts a graphite anode and a low-carbon steel cathode, under the action of direct current, chlorine gas floats upwards from the anode to leave molten salt, molten lithium floats above the molten salt through cathode precipitation, and a diaphragm is used in the middle of the electrolytic cell to separate the anode from the molten salt, so that secondary reaction is avoided. The lithium electrolytic cells currently used are mainly of the three types french, american and german. The French type electrolytic cell needs to manually discharge lithium from the lithium collecting cell, the American type electrolytic cell adopts a non-partition design, and also needs to periodically scoop the metal lithium out of the lithium collecting region by using a metal strainer, the German type electrolytic cell uses a porous diaphragm to separate the metal lithium from chlorine, and the metal lithium overflows through a riserAnd feeding the lithium alloy into a lithium storage tank. These cells all suffer from certain drawbacks: (1) the liquid metal lithium needs to be scooped out manually. Impurities are easy to be carried in the process of scooping lithium, and the operation requirement is high; lithium is easily oxidized or nitrided in the lithium discharging process; the operating environment of workers is severe. (2) The produced lithium metal is easily contaminated by Na. Since the decomposition potential of NaCl is lower than that of LiCl, Na that is not removed from the raw material during electrolysis+Will precede Li+And the product is separated out and enters the product, so that the requirement of molten salt electrolysis on the purification process of LiCl and KCl serving as raw materials is extremely high. Patent CN105624752A discloses a lithium electrolysis trough structure adds in traditional electrolysis trough and can dismantle board and store up the lithium groove temporarily, avoids the direct contact of workman with lithium to a certain extent, nevertheless need control the electrolysis trough slope when going out lithium, has increased the operation degree of difficulty, unable continuous production. Patent CN101760759A utilizes the buoyancy of electrolyte to metallic lithium, exports lithium outside the groove automatically, has solved the artifical problem of going out lithium, has promoted product purity, nevertheless can't avoid the pollution of Na to the metallic lithium product.
With the development of high energy density batteries and controllable nuclear fusion technology, the demand for high purity lithium metal is increasingly strong, so that the improvement of the traditional lithium electrolysis process is needed.
Disclosure of Invention
Aiming at the defects of the existing metal lithium molten salt electrolytic cell, the invention aims to provide a high-purity metal lithium prepared by electrolysis in an efficient and clean mode. The method comprises the steps of electrolyzing LiCl-KCl molten salt through a double-chamber molten salt electrolytic cell, arranging a lithium ion conductor ceramic diaphragm between a cathode chamber and an anode chamber of the electrolytic cell, placing the molten salt in an anode chamber, reducing Cl & lt- & gt at an anode, introducing generated chlorine into a chlorine recovery system through a gas collecting hood, and feeding Li into a chlorine recovery system through a Li collecting hood+Passes through a solid electrolyte ceramic membrane to enter a cathode chamber and is reduced into metallic lithium. The whole process is continuous electrolysis, and high automation can be realized.
In order to achieve the above object, the embodiment of the present invention provides a method for preparing high purity lithium by a solid electrolyte-based dual-chamber molten salt electrolyzer, which comprises an electrolyzer shell, an anode plate, an anode chamber, a cathode plate, a cathode chamber and a solid electrolyte ceramic diaphragm, wherein the anode chamber and the cathode chamber are separated by the solid electrolyte ceramic diaphragm;
the method for preparing high-purity lithium specifically comprises the following steps:
uniformly mixing dry LiCl and KCl, adding the mixture into an anode chamber of a double-chamber molten salt electrolytic cell, and adding metal lithium into a cathode chamber;
heating the double-chamber molten salt electrolytic cell until the salt in the anode chamber and the lithium in the cathode chamber are completely melted and preserving heat, so that the double-chamber molten salt electrolytic cell forms a continuous passage;
and (3) electrifying direct current to the double-chamber molten salt electrolytic bath forming the continuous passage for electrolysis, recovering gas generated in the anode chamber, and obtaining high-purity metal lithium from the cathode chamber.
Further, the double-chamber molten salt electrolytic cell also comprises a gas collecting hood; the gas-collecting hood is arranged above the inside of the anode chamber, and a fan and a chlorine recovery system are connected to the outside of the gas-collecting hood;
and the gas-collecting hood is used for absorbing and recycling gas generated by the anode chamber.
Further, the double-chamber molten salt electrolytic cell also comprises a lithium outlet pipe and an oxygen-free working box;
the lithium outlet pipe is arranged on the side face of the cathode chamber, and the other end of the lithium outlet pipe is connected with an oxygen-free working box and used for collecting the metal lithium melt and cooling the metal lithium melt into a lithium ingot.
Furthermore, the double-chamber molten salt electrolytic cell also comprises a feed inlet, wherein the feed inlet is arranged on the side surface of the anode chamber and is used for adding LiCl, so that the electrolytic process reaches dynamic balance, and the continuous preparation of lithium is realized.
Further, the ratio of LiCl in the mixture of LiCl and KCl is 40-60 wt%.
Further, the temperature is 420-.
Furthermore, the anode plate is a high-temperature-resistant and corrosion-resistant anode plate and is provided with a graphite electrode; the cathode plate is a low-carbon steel electrode.
Further, the solid electrolyte ceramic diaphragm is a lithium ion conductor material, including but not limited to NASICON type oxidesSolid electrolyte, LISICON-type oxide solid electrolyte, garnet-type oxide solid electrolyte, perovskite-type oxide solid electrolyte, anti-perovskite-type oxide solid electrolyte, Thio-LISICON-type sulfide solid electrolyte, Li(11-x)M(2-x)P(1+x)S12A sulfide solid electrolyte (wherein M is at least one of Ge, Sn and Si, and x is more than or equal to 0 and less than or equal to 1), a silviganite sulfide solid electrolyte and a halide solid electrolyte; a preferred ceramic separator material is a garnet-type oxide solid electrolyte.
Furthermore, the chlorine gas recovery system absorbs Cl through alkali liquor2A hypochlorite solution is generated.
Has the advantages that:
(1) the invention utilizes a solid electrolyte ceramic diaphragm to divide the electrolytic cell into an anode chamber and a cathode chamber, molten salt is positioned in the anode chamber, and the ceramic diaphragm only allows Li+The lithium ion battery anode has the advantages that the lithium ion battery anode can penetrate through the cathode chamber and is reduced into high-purity metal lithium, automatic separation of molten salt and the metal lithium can be achieved, dispersion and dissolution of the metal lithium in the molten salt are avoided, meanwhile, the metal lithium is completely isolated from chlorine generated by the anode, secondary reaction is avoided, and product yield and production efficiency are improved.
(2) The solid electrolyte membrane can prevent Na not removed from raw materials+And the lithium metal enters the cathode chamber, so that the purity of the lithium metal product is greatly improved, the requirement on the purity of the raw material is reduced, and the production cost is reduced.
(3) According to the invention, the metal lithium in the cathode chamber of the electrolytic cell can automatically flow out of the electrolytic cell to cool and cast ingots without manual lithium discharge, so that the automation degree is improved. The production process can be completely sealed, the pollution of air to the lithium metal is avoided, the product quality is effectively improved, the chlorine gas is prevented from escaping to the outside, and the production environment is improved.
Drawings
FIG. 1 is a schematic structural diagram of a double-chamber molten salt electrolyzer provided by an embodiment of the invention.
[ Mark Specification ]:
1-an anode plate; 2-an anode chamber; 3-a solid electrolyte ceramic separator; 4-a cathode chamber; 5-a cathode plate; 6-oxygen-free work box; 7-a lithium outlet pipe; 8-a gas-collecting hood; 9-feeding port.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to specific embodiments, but the scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
As shown in FIG. 1, the embodiment of the invention provides a structural schematic diagram of a double-chamber molten salt electrolyzer, which comprises an electrolyzer shell, wherein a solid electrolyte ceramic diaphragm 3 is vertically arranged in the electrolyzer, and the solid electrolyte ceramic diaphragm 3 comprises, but is not limited to, NASICON type oxide solid electrolyte, LISICON type oxide solid electrolyte, garnet type oxide solid electrolyte, perovskite type oxide solid electrolyte, anti-perovskite type oxide solid electrolyte, Thio-LISICON type sulfide solid electrolyte, Li(11-x)M(2-x)P(1+x)S12A sulfide solid electrolyte (wherein M is at least one of Ge, Sn and Si, and x is more than or equal to 0 and less than or equal to 1), a silviganite sulfide solid electrolyte and a halide solid electrolyte; the preferred ceramic separator material is a garnet-type oxide solid electrolyte; the electrolytic cell is divided into an anode chamber 2 and a cathode chamber 4, wherein an anode plate 1 and a cathode plate 5 are respectively arranged in the anode chamber 2 and the cathode chamber 4 and are used for being connected with an external circuit to carry out electrolysis; the upper side in the anode chamber is provided with a gas collecting hood 8 for absorbing chlorine generated in the electrolysis process, the gas collecting hood is connected with a fan and a filter recovery system for absorbing the chlorine through alkali liquor, the side surface of the anode chamber is provided with a feed inlet 9 for adding LiCl,so that the electrolytic process reaches dynamic balance and the continuous preparation of lithium is realized; and a lithium outlet pipe 7 is arranged on the side surface of the cathode chamber 4, and the other end of the lithium outlet pipe 7 is connected with an oxygen-free working tank 6 for collecting the molten lithium metal and cooling the molten lithium metal into a lithium ingot.
Examples
(1) Drying KCl and LiCl at 400 deg.C and 500 deg.C for 1 hr respectively;
(2) and uniformly mixing the dried KCl and LiCl according to the mass ratio of 1: 1, adding the mixture into an anode chamber of an electrolytic cell, and adding a proper amount of metal lithium into a cathode chamber protected by inert gas. The temperature of the electrolytic cell begins to rise until the KCl-LiCl molten salt and the metal lithium are completely melted;
(3) the temperature of the electrolytic cell is kept at 450 ℃, 1600A direct current is introduced to start electrolysis, and meanwhile, a fan and a chlorine recovery system are started, and LiCl is automatically supplemented through a feed inlet of an anode chamber to keep the proportion constant.
(4) After electrolysis for a period of time, when the liquid level of liquid metal lithium in the cathode chamber reaches the position of a lithium outlet, opening a metal valve to enable the metal lithium liquid to flow into a casting mold in an oxygen-free working box protected by argon through a guide pipe to cool an ingot; chlorine generated by the anode chamber enters a chlorine recovery system through the gas-collecting hood and the exhaust pipe to generate sodium hypochlorite solution.
Through calculation, the current efficiency is 85.1%, the electric energy efficiency is 32.6%, and the purity of the prepared metal lithium is 99%.
The above-mentioned embodiments are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical scope of the present invention, and equivalents and modifications of the technical solutions and concepts of the present invention should be covered by the scope of the present invention.
Claims (9)
1. A method for preparing high-purity lithium by a double-chamber molten salt electrolytic cell based on solid electrolyte is characterized in that the double-chamber molten salt electrolytic cell comprises an electrolytic cell shell, an anode plate, an anode chamber, a cathode plate, a cathode chamber and a solid electrolyte ceramic diaphragm, wherein the anode chamber and the cathode chamber are separated by the solid electrolyte ceramic diaphragm;
the method for preparing high-purity lithium specifically comprises the following steps:
uniformly mixing dry LiCl and KCl, adding the mixture into an anode chamber of a double-chamber molten salt electrolytic cell, and adding metal lithium into a cathode chamber;
heating the double-chamber molten salt electrolytic cell until the salt in the anode chamber and the lithium in the cathode chamber are completely melted and preserving heat, so that the double-chamber molten salt electrolytic cell forms a continuous passage;
and (3) electrifying direct current to the double-chamber molten salt electrolytic bath forming the continuous passage for electrolysis, recovering gas generated in the anode chamber, and obtaining high-purity metal lithium from the cathode chamber.
2. The solid electrolyte-based dual-chamber molten salt electrolyzer cell for the production of high purity lithium in claim 1, wherein the dual-chamber molten salt electrolyzer cell further comprises a gas-collecting hood; the gas-collecting hood is arranged above the inside of the anode chamber, and a fan and a chlorine recovery system are connected to the outside of the gas-collecting hood;
and the gas-collecting hood is used for absorbing and recycling gas generated by the anode chamber.
3. The solid electrolyte-based dual-chamber molten salt electrolyzer cell for the production of high purity lithium in claim 1, characterized in that the dual-chamber molten salt electrolyzer cell further comprises a lithium outlet tube and an oxygen-free working chamber;
the lithium outlet pipe is arranged on the side face of the cathode chamber, and the other end of the lithium outlet pipe is connected with an oxygen-free working box and used for collecting the metal lithium melt and cooling the metal lithium melt into a lithium ingot.
4. The method for preparing high-purity lithium by using the solid-state electrolyte-based double-chamber molten salt electrolytic cell according to claim 1, wherein the double-chamber molten salt electrolytic cell further comprises a feed inlet which is arranged on the side of the anode chamber and is used for adding LiCl, so that the electrolytic process is dynamically balanced, and the continuous preparation of lithium is realized.
5. The method for preparing high-purity lithium by using the solid-state electrolyte-based double-chamber molten salt electrolyzer of claim 1 is characterized in that the ratio of LiCl in the mixture of LiCl and KCl is 40-60 wt%.
6. The method for preparing high-purity lithium by the solid-state electrolyte-based double-chamber molten salt electrolytic cell according to claim 1, wherein the heat preservation temperature is 420-500 ℃.
7. The method for preparing high-purity lithium by using the solid-state electrolyte-based double-chamber molten salt electrolytic cell according to claim 1, wherein the anode plate is a high-temperature-resistant and corrosion-resistant anode plate and is a graphite electrode; the cathode plate is a low-carbon steel electrode.
8. The solid electrolyte-based dual-compartment molten salt electrolyzer cell for the production of high purity lithium in accordance with claim 1 wherein the solid electrolyte ceramic membrane is a lithium ion conductor material including, but not limited to, NASICON type oxide solid electrolyte, LISICON type oxide solid electrolyte, garnet type oxide solid electrolyte, perovskite type oxide solid electrolyte, anti-perovskite type oxide solid electrolyte, Thio-LISICON type sulfide solid electrolyte, Li(11-x)M(2-x)P(1+x)S12Type sulfide solid electrolytes, thiogenitic type sulfide solid electrolytes, and halide solid electrolytes.
9. The method for preparing high-purity lithium by the double-chamber solid electrolyte-based molten salt electrolysis cell according to claim 2, wherein the chlorine gas recovery system is Cl absorption by lye2A hypochlorite solution is generated.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116695185A (en) * | 2023-08-04 | 2023-09-05 | 四川澳晟新材料科技有限责任公司 | Simulation test device for parameters of metal lithium molten salt electrolysis process |
| CN116837419A (en) * | 2023-08-28 | 2023-10-03 | 上海阿波罗机械股份有限公司 | Method for extracting lithium from salt lake |
| WO2024061312A1 (en) * | 2022-09-22 | 2024-03-28 | Beijing Yeeneng New Energy Technology Co., Ltd | A method and device for preparing high-purity lithium chloride based on lithium-ion solid electrolyte |
| WO2024078526A1 (en) * | 2022-10-11 | 2024-04-18 | Beijing Yeeneng New Energy Technology Co., Ltd. | A method and apparatus for preparing high-purity metallic lithium based on lithium-ion solid-liquid dual electrolyte |
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Application publication date: 20210820 |