CN112048737A - Method for improving lithium metal electrolysis current efficiency by controlling water content - Google Patents
Method for improving lithium metal electrolysis current efficiency by controlling water content Download PDFInfo
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- CN112048737A CN112048737A CN202010886363.5A CN202010886363A CN112048737A CN 112048737 A CN112048737 A CN 112048737A CN 202010886363 A CN202010886363 A CN 202010886363A CN 112048737 A CN112048737 A CN 112048737A
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- China
- Prior art keywords
- current efficiency
- humidity
- electrolysis
- electrolytic cell
- air
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 31
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 22
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 238000004378 air conditioning Methods 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 2
- 238000005192 partition Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 abstract description 3
- 238000011112 process operation Methods 0.000 abstract description 2
- 239000003570 air Substances 0.000 description 24
- 239000002994 raw material Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 4
- 229910013618 LiCl—KCl Inorganic materials 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000000087 stabilizing 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
- 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
- C25C7/06—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)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention belongs to the technical field of molten salt electrolysis, and particularly provides a method for improving the current efficiency of metal lithium electrolysis by controlling water content, which is a method for improving the current efficiency of metal lithium electrolysis in summer in a high-temperature and high-humidity area. The method is realized by the following steps: controlling air humidity of a relatively closed electrolytic plant or directly introducing relatively humid air with certain water content into the electrolytic cell, and controlling the water content in the atmosphere in the electrolytic cell to carry out electrolysis under the condition of 3.5-5 vol.%. The method is convenient and simple in process operation, is suitable for quickly and efficiently improving the summer current efficiency in high-temperature and high-humidity areas, and can improve the summer current efficiency by more than 15%.
Description
Technical Field
The invention belongs to the technical field of fused salt electrolysis, and particularly relates to a method for improving the current efficiency of metal lithium electrolysis by controlling water content, namely a method for improving the current efficiency of metal lithium electrolysis in summer in a high-temperature and high-humidity area.
Background
The molten salt electrolysis of metallic lithium is the main means for the industrial production of metallic lithium at present. The metal lithium electrolysis in high-temperature and high-humidity areas has low current efficiency in summer. The average environmental temperature in summer is 26-36 deg.C, the highest temperature in workshop is 50 deg.C, relative humidity is 20-30%, and absolute humidity of air is 15g/cm3-25g/m3The volume ratio of water vapor in the air is 2-3 vol%, and the current efficiency is 50-60%; the environmental temperature in winter is 5-25 ℃, the highest temperature in a workshop can reach 30 ℃, the relative humidity is 7-20 percent, and the absolute humidity in the air is 6g/m3-15g/m3The volume ratio of water vapor in the air is 0.8 vol.% to 2 vol.%, the current efficiency is 80% to 90%, and the method is much higher than summer. g/m3
In the current process of metal lithium electrolysis, an electrolytic cell is directly exposed in the air, so that the temperature rises to about 30-35 ℃ along with the environment in summer, and the absolute humidity is 25g/m3In the vicinity, the volume content of water vapor in the air at this time is about 3%, and the current efficiency is low, about 60%.
The present invention increases current efficiency by increasing the water content in the ambient air or in the atmosphere within the cell.
Disclosure of Invention
The invention aims to solve the problem of low summer current efficiency in a high-temperature high-humidity area in the prior art, and provides a process for improving the summer current efficiency in the high-temperature high-humidity area so as to overcome the defects of the prior art.
The purpose of the invention is realized by the following technical scheme:
a method for improving the current efficiency of lithium metal electrolysis by controlling the water content comprises the following steps:
the method comprises the following steps: the air conditioning unit with heat pump module provides temperature of 40-45 deg.c and absolute humidity of 50g/m3-60g/m3High humidity air.
The heat pump module air conditioning unit is equivalent to an industrial air conditioner, the equipment is used for providing air with required conditions, and the obtained air is led to the surface of the electrolytic bath through the vent, so that the air humidity in the electrolytic environment is changed.
Step two: an operation room is arranged outside the electrolytic cell, a hygrothermograph is respectively arranged inside and outside the workshop, and the temperature and humidity data in the working environment of the electrolytic cell are monitored and recorded at any time.
The operation room forms a closed space for building a partition plate outside the electrolysis device, and the function of the method is to reduce the leakage of low-humidity air provided by the modular air-cooled water chilling unit and reduce the influence of the environment on the method. The current production situation is that the electrolytic cell is directly placed in a factory building and is not isolated from the air.
The humiture meter is an auxiliary detection means and can be directly placed in an operation room.
Step three: introducing high-humidity air obtained in the step one into an operation workshop or the surface of the electrolytic cell, and controlling the water vapor volume ratio to be 3.5-5 vol.%, preferably 3.8-4 vol.% through reading and recording by a hygrothermograph.
The control method is to calculate the water vapor content in the air by reading the reading of the hygrothermograph. When the water vapor content is higher, the air quantity of the heat pump module air conditioning unit can be reduced to reduce the humidity; the air quantity is increased when the water vapor content is lower.
Step four: and collecting the metal lithium product every 2 hours, sampling and calculating the current efficiency, and simultaneously recording the temperature and humidity data in the environment of the electrolysis process.
The collecting operation of the lithium metal product is to utilize a porous leakage net and open the cover of the electrolytic cell to directly fish the liquid lithium metal in the electrolytic cell within the electrolysis temperature range of 400-500 ℃.
The current efficiency calculation method comprises the steps of weighing the obtained metal lithium after fishing, and determining the ratio of the obtained metal lithium to the theoretical metal lithium yield within a period of time as the current efficiency.
The process of the invention relating to the electrolysis of metallic lithium comprises the following steps: pouring a certain proportion of LiCl-KCl (preferably LiCl: KCl: 45 wt.%: 55 wt.% -50 wt.%: 50 wt.%) mixed raw materials into an electrolytic cell, introducing alternating current to heat the mixed raw materials to 400-450 ℃ to melt the raw materials, introducing 10KA-100KA direct current to electrolyze the mixed raw materials, opening a cover of the electrolytic cell after electrolyzing for a certain time (preferably 2-8h), directly fishing out lithium metal, weighing the lithium metal, and calculating the current efficiency.
The invention has the positive effects that:
the method is convenient and simple in process operation, is suitable for industrial application, and is a method for quickly and efficiently improving and stabilizing the summer current efficiency in high-temperature and high-humidity areas, and the summer current efficiency can be improved by more than 15%.
According to the invention, an isolation room device similar to a movable room is built outside the electrolytic cell, dry (humid) air is introduced into the isolation room device, and the current efficiency can reach more than 80% after the air content in the operation room is controlled to reach a certain humidity (dry or humid).
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the content of the present invention, but the content of the present invention is not limited to the following examples. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The following provides a specific embodiment of the present invention for improving the summer current efficiency in a high-temperature and high-humidity area.
The process of lithium metal electrolysis in the examples is:
pouring 50 wt.% LiCl-KCl mixed raw material into an electrolytic cell, introducing alternating current, heating to 400-450 ℃, melting the raw material to a molten state, introducing 25KA direct current for electrolysis, opening a cover of the electrolytic cell after 4 hours of electrolysis, directly fishing out lithium metal, and weighing to calculate current efficiency.
Example 1
The method comprises the following steps: the air conditioning unit with the heat pump module is utilized to provide 45 ℃ and 50g/m of absolute humidity3-60g/m360 g/m3High humidity air of (2);
step two: an operation room is arranged outside the electrolytic cell, a hygrothermograph is respectively arranged inside and outside the workshop, and the temperature and humidity data in the working environment of the electrolytic cell are monitored and recorded at any time
Step three: introducing high-humidity air obtained in the step one into an operation workshop, reading and recording through a hygrothermograph, and controlling the volume ratio of water vapor to be 4.5 vol%;
step four: and collecting the metal lithium product every 2 hours, sampling and calculating the current efficiency, and simultaneously recording the temperature and humidity data in the environment of the electrolysis process.
The current efficiency reaches 80%.
Calculating the current efficiency: the theoretical yield of electrolytic lithium metal is (0.26 is the electrochemical equivalent constant of lithium, in g/a × h):
Wtheory of the invention＝0.26*I*t
＝0.26*25000*4
＝26kg
Weighing to obtain actual yield W of lithium by fishing out lithium metalPractice ofCurrent efficiency was obtained at 20.8 kg:
η＝Wpractice of/WTheory of the invention×100％
＝20.8/26×100％
＝80％
Example 2
The method comprises the following steps: the air conditioning unit with heat pump module is utilized to provide 40 ℃ and 50g/m of absolute humidity3High humidity air of (2);
step two: the inside and the outside of the electrolytic workshop are respectively provided with a hygrothermograph for monitoring and recording the temperature and humidity data in the working environment of the electrolytic cell at any time
Step three: directly introducing the high-humidity air obtained in the step one to the surface of the electrolytic cell, reading and recording through a hygrothermograph, and controlling the volume ratio of water vapor to be 3.8 vol%;
step four: and collecting the metal lithium product every 2 hours, sampling and calculating the current efficiency, and simultaneously recording the temperature and humidity data in the environment of the electrolysis process.
The current efficiency reaches 80 percent.
The current efficiency calculation process is the same as above.
The current efficiency of the current industrial production is about 65%, and the current efficiency of the operation (introducing air with certain humidity to the surface of the electrolytic cell and increasing the humidity) can reach 80% by increasing the current efficiency.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and decorations can be made without departing from the concept of the present invention, and these modifications and decorations should also be regarded as being within the protection scope of the present invention.
Claims (5)
1. A method for increasing the current efficiency of lithium metal electrolysis by controlling the water content, comprising the steps of: the air conditioning unit with heat pump module provides temperature of 40-45 deg.c and absolute humidity of 50g/m3-60g/m3High humidity air of (2); arranging an operation room outside the electrolytic cell, respectively arranging a hygrothermograph inside and outside the workshop, and monitoring and recording temperature and humidity data in the working environment of the electrolytic cell at any time; introducing high-humidity air into operation workshop or electrolytic bath, and controlling absolute humidity at 28g/m3-40g/m3Within the range; and collecting the metal lithium product every 2 hours, sampling and calculating the current efficiency, and simultaneously recording the temperature and humidity data in the environment of the electrolysis process.
2. The method of claim 1, wherein the moisture content in the atmosphere is controlled by directly introducing humid air of 40 ℃ to 45 ℃ into the electrolysis shop or the surface of the electrolytic cell.
3. The method of claim 1, wherein the absolute humidity in the atmosphere of the electrolytic cell is controlled to be 28g/m3-40g/m3In the range of 3.5 vol.% to 5 vol.% of water vapour content.
4. A method of increasing the current efficiency of lithium metal electrolysis by controlling the water content according to claim 3 wherein the water vapour content of the atmosphere in the cell is controlled to be in the range of 3.8 vol.% to 4 vol.%.
5. The method of claim 1, wherein the operation room is a closed space for building a partition outside the electrolysis apparatus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010886363.5A CN112048737A (en) | 2020-08-28 | 2020-08-28 | Method for improving lithium metal electrolysis current efficiency by controlling water content |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010886363.5A CN112048737A (en) | 2020-08-28 | 2020-08-28 | Method for improving lithium metal electrolysis current efficiency by controlling water content |
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| CN112048737A true CN112048737A (en) | 2020-12-08 |
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| CN202010886363.5A Pending CN112048737A (en) | 2020-08-28 | 2020-08-28 | Method for improving lithium metal electrolysis current efficiency by controlling water content |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1693512A (en) * | 2005-06-16 | 2005-11-09 | 王洪 | High sodium metal lithium and its manufacturing method |
| CN101368281A (en) * | 2008-09-27 | 2009-02-18 | 东北大学 | Method for aluminum lithium alloy preparation by fused salt electrolysis process |
| CN101376992A (en) * | 2008-09-27 | 2009-03-04 | 东北大学 | Method for preparing magnesium lithium alloy by fused salt electrolysis process |
| CN101573296A (en) * | 2006-11-02 | 2009-11-04 | 株式会社三德 | Process for producing metallic lithium |
-
2020
- 2020-08-28 CN CN202010886363.5A patent/CN112048737A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1693512A (en) * | 2005-06-16 | 2005-11-09 | 王洪 | High sodium metal lithium and its manufacturing method |
| CN101573296A (en) * | 2006-11-02 | 2009-11-04 | 株式会社三德 | Process for producing metallic lithium |
| CN101368281A (en) * | 2008-09-27 | 2009-02-18 | 东北大学 | Method for aluminum lithium alloy preparation by fused salt electrolysis process |
| CN101376992A (en) * | 2008-09-27 | 2009-03-04 | 东北大学 | Method for preparing magnesium lithium alloy by fused salt electrolysis process |
Non-Patent Citations (1)
| Title |
|---|
| 张松岩等: "工艺条件对金属锂电解过程影响研究", 《有色金属（冶炼部分）》 * |
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Application publication date: 20201208 |