CN111719166B - Metal lithium electrolytic bath and preparation method of metal lithium - Google Patents
Metal lithium electrolytic bath and preparation method of metal lithium Download PDFInfo
- Publication number
- CN111719166B CN111719166B CN202010685411.4A CN202010685411A CN111719166B CN 111719166 B CN111719166 B CN 111719166B CN 202010685411 A CN202010685411 A CN 202010685411A CN 111719166 B CN111719166 B CN 111719166B
- Authority
- CN
- China
- Prior art keywords
- lithium
- electrolytic cell
- diaphragm
- graphite anode
- cathode
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- 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
-
- 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
- C25C7/005—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells of cells for the electrolysis of melts
-
- 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
- C25C7/02—Electrodes; Connections thereof
- C25C7/025—Electrodes; Connections thereof used in cells for the electrolysis of melts
-
- 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
-
- 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
- C25C7/06—Operating or servicing
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
Abstract
The invention belongs to the technical field of metal lithium preparation by fused salt electrolysis, and provides a metal lithium electrolytic bath and a preparation method of metal lithium.A graphite anode is inserted from the top of the electrolytic bath and is arranged in the middle of a cathode, so that the uniform distribution of current is facilitated; the graphite anode and the cathode are separated by the diaphragm, the chlorine gas delivery pipe is arranged between the graphite anode and the diaphragm, the lithium delivery pipe is arranged between the diaphragm and the cathode, and the generated chlorine gas is pumped out from the chlorine gas delivery pipe in the electrolytic reaction process, and the metal lithium enters the lithium collection chamber through the lithium delivery pipe, so that the chlorine gas is separated from the metal lithium, the metal lithium is prevented from carrying out secondary reaction with the chlorine gas to regenerate lithium chloride, the current efficiency is improved, and the power consumption is reduced; furthermore, the metal lithium electrolytic cell provided by the invention is provided with the baffle which can be opened at the bottom of the charging bin, and during charging, lithium chloride can be preheated and then added into the electrolytic cell, so that the phenomenon that the temperature of molten salt fluctuates too much after charging is avoided.
Description
Technical Field
The invention belongs to the technical field of metal lithium preparation through molten salt electrolysis, and particularly relates to a metal lithium electrolytic bath and a preparation method of metal lithium.
Background
The preparation of metallic lithium by lithium chloride molten salt electrolysis is the main technical method for industrially preparing metallic lithium at present, and about 90 percent of metallic lithium is prepared by the method. There are many kinds of designs in the fused salt electrolysis trough at home and abroad, insert formula steel negative pole and side and insert formula graphite anode under adopting generally, separate the negative and positive pole product with the steel baffle, use pottery or graphite to make the groove lining, adopt the manual mode of scooping up lithium to get lithium, metal lithium easily reacts with oxygen in the air, nitrogen, reduce product purity to chlorine easily reacts with metal lithium secondary and regenerates the lithium chloride among the electrolysis process, leads to the electrolytic efficiency low.
Disclosure of Invention
In view of the above, the present invention provides a metal lithium electrolytic bath and a method for preparing metal lithium. The metal lithium electrolytic cell provided by the invention has high electrolytic efficiency and high product purity.
In order to achieve the above object, the present invention provides the following technical solutions:
a metal lithium electrolytic cell comprises a cavity; the interior of the cavity is divided into an electrolysis chamber and a lithium collecting chamber;
a graphite anode disposed in the center of the electrolytic cell;
a separator surrounding the outside of the graphite anode;
a cathode surrounding an outer side of the separator;
a chlorine gas delivery pipe is arranged between the graphite anode and the diaphragm;
a lithium guide pipe is arranged between the diaphragm and the cathode and is communicated with the lithium collecting chamber;
the top of the cavity is provided with a cavity cover, and the cavity cover is provided with a feeding bin and an observation hole; the top end of the graphite anode extends out of the top of the cavity cover;
the outer surface of the cavity is also sequentially provided with a heating resistance plate, a refractory insulating brick and an outer protective shell.
Preferably, the metallic lithium electrolytic cell further comprises an anode clamp; the anode clamp is clamped to the portion of the graphite anode that protrudes from the top of the chamber cover.
Preferably, the feed inlet of the feeding bin is an inclined opening; the bottom of the feeding bin is provided with an openable baffle.
Preferably, a lithium extraction pipe is further arranged in the lithium collection chamber.
Preferably, the distance between the graphite anode and the diaphragm is 20-40 mm; the distance between the diaphragm and the cathode is 50-80 mm.
Preferably, the length of the part of the graphite anode extending out of the top of the cavity cover is 150-200 mm.
Preferably, the surface of the diaphragm is provided with small holes, the aperture ratio of the diaphragm is 5-9%, and the aperture of each small hole is 0.07-1 mm.
The invention also provides a method for preparing the metal lithium by using the metal lithium electrolytic bath, which comprises the following steps:
(1) adding a mixture of lithium chloride and potassium chloride into a metal lithium electrolytic bath, and starting a heating resistance plate to melt the lithium chloride and the potassium chloride to form a molten salt;
(2) the electrolytic cell is electrified to carry out electrolysis, chlorine generated by electrolysis is extracted through the chlorine delivery pipe, and lithium metal generated by electrolysis enters the lithium collection chamber from the lithium delivery pipe.
Preferably, the electrolysis temperature is 400-440 ℃, and the current is 600-1000A.
Preferably, in the electrolysis process, lithium chloride is supplemented into the electrolytic cell from the feeding bin, the lithium chloride is preheated in the feeding bin, and then the preheated lithium chloride is added into the electrolytic cell by opening the baffle.
The invention provides a metal lithium electrolytic cell, wherein a graphite anode is designed into a top-inserted type, is inserted from the top of the electrolytic cell and is arranged in the middle of a cathode, so that the uniform distribution of current is facilitated; in addition, the graphite anode and the graphite cathode are separated by the diaphragm, the chlorine gas delivery pipe is arranged between the anode and the diaphragm, the lithium delivery pipe is arranged between the diaphragm and the cathode, the generated chlorine gas is pumped out from the chlorine gas delivery pipe in the electrolytic reaction process, and the metal lithium enters the lithium collection chamber through the lithium delivery pipe; and the lithium metal is pumped out by the lithium pumping pipe after entering the lithium collecting chamber, so that the reaction of the lithium metal and oxygen and nitrogen in the air can be avoided, and the product purity is improved.
In addition, in the field, the lithium chloride raw material is generally directly added into the electrolytic cell in the electrolytic process of the metal lithium, and the temperature difference between the added lithium chloride raw material and the molten salt in the electrolytic cell is large, so that the temperature fluctuation of the molten salt in the electrolytic cell is large, the molten salt is locally hardened, and the electrolysis is influenced.
The results of the examples show that the current efficiency of electrolysis can reach 85.31% and the purity of the metallic lithium can reach 98.57% when the metallic lithium electrolytic cell of the invention is used for preparing the metallic lithium.
Drawings
FIG. 1 is a schematic structural diagram of a metallic lithium electrolytic cell;
FIG. 2 is a top view of a metallic lithium electrolytic cell;
in FIGS. 1 to 2: 1-graphite anode, 2-anode clamp, 3-cavity cover, 4-diaphragm, 5-cathode, 6-cavity, 7-heating resistance plate, 8-outer protective shell, 9-chlorine gas outlet pipe, 10-lithium guide pipe, 11-fire-resistant insulating brick, 12-lithium extraction pipe, 13-lithium collection chamber, 14-electrolysis chamber, 15-baffle, 16-observation hole, 17-feeding bin and 18-cathode hanger.
Detailed Description
The invention provides a metal lithium electrolytic cell, which is shown in a schematic structural diagram of fig. 1, a top view of the metal lithium electrolytic cell is shown in fig. 2, and in fig. 1-2: 1-graphite anode, 2-anode clamp, 3-cavity cover, 4-diaphragm, 5-cathode, 6-cavity, 7-heating resistance plate, 8-outer protective shell, 9-chlorine gas outlet pipe, 10-lithium guide pipe, 11-fire-resistant insulating brick, 12-lithium extraction pipe, 13-lithium collection chamber, 14-electrolysis chamber, 15-baffle, 16-observation hole, 17-feeding bin and 18-cathode hanger.
The following description will be made with reference to FIGS. 1 to 2.
The metal lithium electrolytic cell provided by the invention comprises a cavity. In the invention, the cavity is divided into an electrolytic chamber and a lithium collecting chamber; the sizes of the electrolytic chamber and the lithium collecting chamber are not particularly limited and can be set according to actual requirements; in the embodiment of the present invention, the lithium collecting chamber is preferably disposed at one side of the cavity, the lithium collecting chamber and the electrolytic chamber are separated by a separator, the volume of the lithium collecting chamber is preferably 9% of the volume of the cavity, and the rest is the electrolytic chamber. In the invention, a lithium extraction pipe is preferably further arranged in the lithium collection chamber, one end of the lithium extraction pipe extends into the bottom of the lithium collection chamber, the other end of the lithium extraction pipe extends out of the top of the chamber cover, and when the volume of lithium metal lithium in the lithium collection chamber reaches above 1/3 of the volume of the lithium collection chamber, the lithium extraction pipe is used for extracting the lithium metal.
The metal lithium electrolytic cell provided by the invention comprises a graphite anode arranged in the center of the electrolytic chamber. In the present invention, the graphite anode is preferably a solid cylinder; the size of the graphite anode is not particularly limited in the present invention, and may be set according to the size known to those skilled in the art.
The metal lithium electrolytic cell provided by the invention comprises a diaphragm surrounding the outer side of the graphite anode. In the invention, the surface of the diaphragm is preferably provided with small holes, the aperture ratio of the diaphragm is preferably 5-9%, more preferably 7%, and the aperture of the small holes is preferably 0.07-1 mm; the thickness of the diaphragm is preferably 3-5 mm; the distance between the graphite anode and the diaphragm is preferably 20-40 mm, and more preferably 30 mm.
In the invention, a chlorine gas delivery pipe is arranged between the graphite anode and the diaphragm, and is particularly arranged at the periphery of the graphite anode, one end of the chlorine gas delivery pipe is close to the graphite anode, the port of the chlorine gas delivery pipe is 15-20 mm away from the graphite anode, and the other end of the chlorine gas delivery pipe is connected with an anticorrosive induced draft fan and is used for delivering chlorine gas generated by the graphite anode; the size of the chlorine gas outlet pipe is not particularly limited in the present invention, and may be set according to the size well known to those skilled in the art.
The metal lithium electrolytic cell provided by the invention comprises a cathode surrounding the outer side of the diaphragm; in the invention, the graphite anode, the diaphragm and the cathode are superposed at the center, namely the diaphragm and the cathode are both in a circular ring shape, the graphite anode is positioned at the center of the circular diaphragm, and the outer side of the circular diaphragm is provided with the circular cathode; the distance between the diaphragm and the cathode is preferably 50-80 mm, and preferably 66 mm; the height of the cathode is the same as the length of the part of the graphite anode arranged in the cavity; the top of the cathode is preferably provided with hangers for hanging the cathode on the side wall of the cavity, and the top of the cathode is preferably symmetrically provided with 4 hangers, two of which are responsible for bearing and the other two of which are responsible for bearing and conducting.
In the invention, the graphite anode, the graphite cathode and the diaphragm are all suspended in the electrolytic chamber, namely the bottoms of the graphite anode and the graphite cathode are not in contact with the bottom of the electrolytic chamber so as to avoid short circuit, wherein the bottom ends of the graphite anode and the graphite cathode are positioned on the same plane, the bottom end of the diaphragm can be slightly higher than the bottom end of the graphite anode, the diaphragm can achieve the effect of isolating chlorine gas, and the specific height is not limited.
In the invention, a lithium guide pipe is arranged between the diaphragm and the cathode, one end of the lithium guide pipe is arranged between the diaphragm and the cathode, preferably arranged in a region between the diaphragm and the cathode and close to the top (metal lithium is suspended on the top), and the other end of the lithium guide pipe is communicated with the lithium collecting chamber, preferably communicated with the lower part of the side surface of the lithium collecting chamber; the size of the lithium guide tube is not particularly limited in the present invention, and may be set according to the size known to those skilled in the art.
In the invention, the top of the cavity is provided with a cavity cover which can be closed and covered with the cavity, and the top end of the graphite anode extends out of the top of the cavity cover; the length of the part of the graphite anode extending out of the top of the cavity cover is preferably 150-200 mm, and more preferably 160 mm. In the invention, the cavity cover is provided with a feeding bin and an observation hole; the feeding bin is arranged at the top of the electrolytic chamber; the feeding hole of the feeding bin is preferably an inclined opening so as to facilitate the feeding of raw materials; the bottom of the feeding bin is provided with a baffle which is preferably openable; when feeding, the baffle does not open earlier, waits that the raw materials preheats the back in the feed bin, opens the baffle again to it is too big to avoid reinforced back fused salt temperature fluctuation.
As an embodiment of the present invention, the metal lithium electrolytic cell further comprises an anode clip, preferably sandwiched between the graphite anode protruding from the top of the chamber cover, for fixing the anode and for connecting a power source to conduct electricity.
In the invention, the outer surface of the cavity is sequentially provided with a heating resistance plate, a refractory insulating brick and an outer protective shell, the heating resistance plate is coated on the side surface of the cavity, the refractory insulating brick is coated on the side surface of the heating resistance plate and the bottom surface of the cavity, and the outer protective shell is coated on the side surface and the bottom surface of the refractory insulating brick.
In the invention, the cavity, the cathode, the diaphragm, the lithium guide tube, the lithium extraction tube and the chlorine gas guide tube are all preferably made of lithium chloride corrosion resistant alloy, such as hastelloy alloy specifically; the materials of the cavity cover and the outer protective shell are preferably stainless steel, specifically 304 steel and 316L steel.
The invention also provides a method for preparing the metal lithium by using the metal lithium electrolytic bath, which comprises the following steps:
(1) adding a mixture of lithium chloride and potassium chloride into a metal lithium electrolytic bath, and starting a heating resistance plate to melt the lithium chloride and the potassium chloride to form a molten salt;
(2) the electrolytic cell is electrified to carry out electrolysis, chlorine generated by electrolysis is extracted through the chlorine delivery pipe, and lithium metal generated by electrolysis enters the lithium collection chamber from the lithium delivery pipe.
According to the invention, a mixture of lithium chloride and potassium chloride is added into a metal lithium electrolytic bath, and a heating resistance plate is started to melt the lithium chloride and the potassium chloride to form a molten salt. In the present invention, the mass ratio of lithium chloride to potassium chloride is preferably 1: 1; according to the invention, lithium chloride and potassium chloride are preferably uniformly mixed and then dried, and then the mixture is added into an electrolytic cell; the heating temperature of the heating resistance plate is not particularly limited, and lithium chloride and potassium chloride can be melted.
After the molten salt is formed, the electrolytic cell is electrified for electrolysis, chlorine generated by electrolysis is extracted through the chlorine gas outlet pipe, and metallic lithium generated by electrolysis enters the lithium collecting chamber from the lithium guide pipe. In the invention, a graphite anode is connected with the anode of a direct current power supply through an anode clamp, and a suspension loop of a cathode is connected with the cathode of the direct current power supply; the electrolysis temperature is preferably 400-440 ℃, more preferably 410-420 ℃, and the current is preferably 600-1000A, more preferably 700-800A; the current density of the graphite anode is preferably 0.38-0.65A/cm2(ii) a The current density of the cathode is preferably 0.25-0.43A/cm2。
The invention preferably uses an anti-corrosion induced draft fan to form micro negative pressure, and the chlorine is pumped into the chlorine absorption tower through the chlorine leading-out pipe.
In the invention, after the cathode generates the metal lithium, the metal lithium can be suspended on the surface of the molten salt in a liquid state immediately due to low melting point and low density, and is gathered in an annular interval formed by the diaphragm and the cathode, and then enters the lithium collecting chamber through the lithium guide pipe (the metal lithium floats on the surface of the molten salt, and flows into the lithium guide pipe when the liquid level of the lithium is higher than that of the lithium guide pipe), the lithium in the lithium collecting chamber is extracted by the lithium extracting pipe when the lithium in the lithium collecting chamber reaches above 1/3 of the volume of the lithium collecting chamber, specifically, negative pressure can be formed through a vacuum pump, so that the lithium is extracted from the lithium guide pipe, and the extracted lithium is preferably.
In the invention, in the electrolysis process, lithium chloride is preferably supplemented into the electrolytic cell from the feeding bin, the lithium chloride is preheated in the feeding bin, and then the preheated lithium chloride is added into the electrolytic cell by opening the baffle; the preheating time is preferably 1 h; the lithium chloride is preferably replenished every 1h, and the amount of each replenishment may be determined empirically by one skilled in the art.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
In the embodiment, molten salt electrolysis is performed by using the metal lithium electrolytic cell shown in fig. 1-2, wherein the graphite anode is a solid cylinder, the diaphragm and the cathode are both annular and sequentially surround the graphite anode, the length of the part, extending out of the top cover, of the graphite anode is 160mm, the distance between the graphite anode and the diaphragm is 30mm, the distance between the diaphragm and the cathode is 66mm, the aperture ratio of the diaphragm is 7%, and the aperture of the small hole is 1 mm.
Example 1
Uniformly mixing raw materials of lithium chloride and potassium chloride according to the mass ratio of 1:1, drying, adding the dried lithium chloride and potassium chloride into an electrolytic cell, starting a heating resistance plate of the electrolytic cell, heating to melt the lithium chloride and the potassium chloride to form molten salt. Electrolyzing at the temperature of 420 ℃ and the current of 600A, supplementing 0.81kg of lithium chloride per hour in the electrolysis process, preheating the lithium chloride in a feeding bin for 1 hour, and then adding the lithium chloride into an electrolytic cell. And after the lithium in the lithium collecting chamber reaches above 1/3 of the volume of the lithium collecting chamber, negative pressure is formed by a vacuum pump, and the lithium is pumped out through a lithium guide pipe. Chlorine generated by electrolysis is extracted through a chlorine delivery pipe. The current efficiency of electrolysis was 84.52%, and the purity of metallic lithium was 98.05%.
Example 2
Uniformly mixing raw materials of lithium chloride and potassium chloride according to the mass ratio of 1:1, drying, adding the dried lithium chloride and potassium chloride into an electrolytic cell, starting a heating resistance plate of the electrolytic cell, heating to melt the lithium chloride and the potassium chloride to form molten salt. Electrolyzing at the temperature of 420 ℃ and the current of 800A, supplementing 1.08kg of lithium chloride per hour in the electrolysis process, preheating the lithium chloride in a feeding bin for 1 hour, and then adding the lithium chloride into an electrolytic cell. And after the lithium in the lithium collecting chamber reaches above 1/3 of the volume of the lithium collecting chamber, negative pressure is formed by a vacuum pump, and the lithium is pumped out through a lithium guide pipe. Chlorine generated by electrolysis is extracted through a chlorine delivery pipe. The current efficiency of the electrolysis was 85.12% and the purity of the lithium metal was 98.57%.
Example 3
Uniformly mixing raw materials of lithium chloride and potassium chloride according to the mass ratio of 1:1, drying, adding the dried lithium chloride and potassium chloride into an electrolytic cell, starting a heating resistance plate of the electrolytic cell, heating to melt the lithium chloride and the potassium chloride to form molten salt. Electrolyzing under the conditions that the temperature of the molten salt is 420 ℃ and the current is 1000A, supplementing 1.35kg of lithium chloride per hour in the electrolysis process, preheating the lithium chloride in a feeding bin for 1 hour, and then adding the lithium chloride into an electrolytic cell. And after the lithium in the lithium collecting chamber reaches above 1/3 of the volume of the lithium collecting chamber, negative pressure is formed by a vacuum pump, and the lithium is pumped out through a lithium guide pipe. Chlorine generated by electrolysis is extracted through a chlorine delivery pipe. The current efficiency of electrolysis was 85.31%, and the purity of metallic lithium was 98.34%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. The metal lithium electrolytic cell is characterized by comprising a cavity; the interior of the cavity is divided into an electrolysis chamber and a lithium collecting chamber;
a graphite anode disposed in the center of the electrolytic cell;
a separator surrounding the outside of the graphite anode;
a cathode surrounding an outer side of the separator;
a chlorine gas delivery pipe is arranged between the graphite anode and the diaphragm; one end of the chlorine gas delivery pipe is close to the graphite anode, the port of the chlorine gas delivery pipe is 15-20 mm away from the graphite anode, and the other end of the chlorine gas delivery pipe is connected with an anti-corrosion induced draft fan and used for delivering chlorine gas generated by the graphite anode;
a lithium guide pipe is arranged between the diaphragm and the cathode and is communicated with the lithium collecting chamber; a lithium extraction pipe is also arranged in the lithium collection chamber;
the top of the cavity is provided with a cavity cover, and the cavity cover is provided with a feeding bin and an observation hole; the top end of the graphite anode extends out of the top of the cavity cover; the feed inlet of the feeding bin is an inclined opening; an openable baffle is arranged at the bottom of the feeding bin; in the electrolysis process, lithium chloride is supplemented into the electrolytic cell from the feeding bin, the lithium chloride is preheated in the feeding bin, and then the baffle is opened to add the preheated lithium chloride into the electrolytic cell;
the outer surface of the cavity is also sequentially provided with a heating resistance plate, a refractory insulating brick and an outer protective shell;
the metal lithium electrolytic cell also comprises an anode clamp; the anode clamp is clamped at the part of the graphite anode extending from the top of the cavity cover; the distance between the graphite anode and the diaphragm is 20-40 mm; the distance between the diaphragm and the cathode is 50-80 mm; the diaphragm surface is provided with small holes, the aperture ratio of the diaphragm is 5-9%, and the aperture of each small hole is 0.07-1 mm; the top of the cathode is symmetrically provided with 4 hangers, two of which are responsible for bearing, and the other two of which are responsible for bearing and conducting; the cavity, the cathode, the diaphragm, the lithium guide pipe, the lithium pumping pipe and the chlorine gas guide pipe are all made of lithium chloride corrosion resistant alloy; the cavity cover and the outer protective shell are made of stainless steel.
2. The metal lithium electrolytic cell according to claim 1, wherein the length of the part of the graphite anode protruding from the top of the chamber cover is 150-200 mm.
3. A method for preparing metallic lithium by using the metallic lithium electrolytic cell of any one of claims 1 to 2, comprising the following steps:
(1) adding a mixture of lithium chloride and potassium chloride into a metal lithium electrolytic bath, and starting a heating resistance plate to melt the lithium chloride and the potassium chloride to form a molten salt;
(2) the electrolytic cell is electrified to carry out electrolysis, chlorine generated by electrolysis is extracted through the chlorine delivery pipe, and lithium metal generated by electrolysis enters the lithium collection chamber from the lithium delivery pipe.
4. The method according to claim 3, wherein the temperature of the electrolysis is 400 to 440 ℃ and the current is 600 to 1000A.
5. The method as claimed in claim 3, wherein during the electrolysis, the electrolytic cell is replenished with lithium chloride from a feed bin, the lithium chloride is preheated in the feed bin, and then the preheated lithium chloride is fed into the electrolytic cell by opening a baffle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010685411.4A CN111719166B (en) | 2020-07-16 | 2020-07-16 | Metal lithium electrolytic bath and preparation method of metal lithium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010685411.4A CN111719166B (en) | 2020-07-16 | 2020-07-16 | Metal lithium electrolytic bath and preparation method of metal lithium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111719166A CN111719166A (en) | 2020-09-29 |
| CN111719166B true CN111719166B (en) | 2021-09-10 |
Family
ID=72572645
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010685411.4A Active CN111719166B (en) | 2020-07-16 | 2020-07-16 | Metal lithium electrolytic bath and preparation method of metal lithium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111719166B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114438549A (en) * | 2020-11-03 | 2022-05-06 | 沈阳铝镁设计研究院有限公司 | Metal lithium electrolytic bath |
| CN113279015A (en) * | 2021-05-21 | 2021-08-20 | 中南大学 | Method for preparing high-purity lithium by using double-chamber molten salt electrolytic cell based on solid electrolyte |
| CN115140732B (en) * | 2022-05-16 | 2023-05-30 | 洛阳师范学院 | Diamond preparation device and diamond preparation method thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0194979A1 (en) * | 1985-02-13 | 1986-09-17 | Hiroshi Ishizuka | Electrolytic cell for a molten salt comprising alkali- or alkaline earth metal chloride |
| JPS63183189A (en) * | 1987-01-23 | 1988-07-28 | Komatsu Denshi Kinzoku Kk | Molten-salt electrolysis method |
| CN1204700A (en) * | 1997-07-08 | 1999-01-13 | 国营建中化工总公司 | Metal lithium electrolytic bath |
| US5904821A (en) * | 1997-07-25 | 1999-05-18 | E. I. Du Pont De Nemours And Company | Fused chloride salt electrolysis cell |
| CN103205774A (en) * | 2013-05-02 | 2013-07-17 | 新疆骏强科技发展有限公司 | Method of preparing metallic lithium by one-step fusion electrolysis of lithium salt |
| CN103556181A (en) * | 2013-10-28 | 2014-02-05 | 奉新赣锋锂业有限公司 | Metallic lithium electrolytic cell |
| CN107574458A (en) * | 2017-09-20 | 2018-01-12 | 宜春赣锋锂业有限公司 | A kind of metal lithium electrolytic bath of centralized collection lithium |
| CN208933496U (en) * | 2018-11-01 | 2019-06-04 | 四川能投鼎盛锂业有限公司 | A kind of electrolytic cell for lithium metal |
| CN110791778A (en) * | 2019-08-21 | 2020-02-14 | 奉新赣锋锂业有限公司 | Metal lithium electrolytic bath |
-
2020
- 2020-07-16 CN CN202010685411.4A patent/CN111719166B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0194979A1 (en) * | 1985-02-13 | 1986-09-17 | Hiroshi Ishizuka | Electrolytic cell for a molten salt comprising alkali- or alkaline earth metal chloride |
| JPS63183189A (en) * | 1987-01-23 | 1988-07-28 | Komatsu Denshi Kinzoku Kk | Molten-salt electrolysis method |
| CN1204700A (en) * | 1997-07-08 | 1999-01-13 | 国营建中化工总公司 | Metal lithium electrolytic bath |
| US5904821A (en) * | 1997-07-25 | 1999-05-18 | E. I. Du Pont De Nemours And Company | Fused chloride salt electrolysis cell |
| CN103205774A (en) * | 2013-05-02 | 2013-07-17 | 新疆骏强科技发展有限公司 | Method of preparing metallic lithium by one-step fusion electrolysis of lithium salt |
| CN103556181A (en) * | 2013-10-28 | 2014-02-05 | 奉新赣锋锂业有限公司 | Metallic lithium electrolytic cell |
| CN107574458A (en) * | 2017-09-20 | 2018-01-12 | 宜春赣锋锂业有限公司 | A kind of metal lithium electrolytic bath of centralized collection lithium |
| CN208933496U (en) * | 2018-11-01 | 2019-06-04 | 四川能投鼎盛锂业有限公司 | A kind of electrolytic cell for lithium metal |
| CN110791778A (en) * | 2019-08-21 | 2020-02-14 | 奉新赣锋锂业有限公司 | Metal lithium electrolytic bath |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111719166A (en) | 2020-09-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111719166B (en) | Metal lithium electrolytic bath and preparation method of metal lithium | |
| US4699704A (en) | Electrolytic cell for a molten salt | |
| CN111455404A (en) | Method for recovering lead from waste lead paste by solid-phase electrolysis method | |
| CN101392387B (en) | Method for electrowinning copper nitrate solution | |
| CN112522741A (en) | Closed type rare earth chloride system electrolytic cell | |
| WO2007034645A1 (en) | PROCESS FOR PRODUCING Ti AND APPARATUS THEREFOR | |
| JPH02213492A (en) | Electrode for electrolytic cell for recovering metal from metal-containing ore or concentrate and its manufacture | |
| CN103046084B (en) | electrolytic reduction system and electrolytic reduction method | |
| CN205741227U (en) | A kind of copper refining electrolysis bath of anode auto feed | |
| US20150027881A1 (en) | Long-acting composite-basket anode combination device | |
| CN213680931U (en) | Closed type rare earth chloride system electrolytic cell | |
| CN215560566U (en) | Semi-continuous refining equipment for magnesium metal | |
| CN102925931B (en) | Negative electrode rare earth molten salt electrolytic under submergence type is inserted in side | |
| CN108004567A (en) | A kind of metal material is prepared with continuous electric level electrolytic cell | |
| CN101469373B (en) | Lithium production device | |
| CN220352255U (en) | Molten salt electrolysis metallic lithium's device | |
| CN85100748B (en) | Electrolysis tank for continuous production of nd-metal and nd-fe alloy | |
| JP2012172194A (en) | Electrolytic apparatus and electrowinning method using the same | |
| CN102925921B (en) | A kind of method strengthening Top-blown Lead Smelting | |
| CN216891256U (en) | Metallurgical ion-exchange membrane electrolytic cell | |
| CN201144272Y (en) | Lithium production device | |
| RU2453639C1 (en) | Electrolyser for obtaining lithium metal | |
| RU2418083C2 (en) | Electrolyser for refining lead in salt melt | |
| CN216688353U (en) | Isolation device | |
| CN215906290U (en) | Novel rare earth metal electrolytic bath |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 341000 No.62 Yingbin Avenue, Ganzhou economic and Technological Development Zone, Jiangxi Province Applicant after: Ganzhou Nonferrous Metallurgy Research Institute Co.,Ltd. Address before: 341000 No.62 Yingbin Avenue, Ganzhou economic and Technological Development Zone, Jiangxi Province Applicant before: GANZHOU NONFERROUS METALLURGICAL Research Institute |
|
| CB02 | Change of applicant information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |