WO2024259611A1 - 一种提锂脱嵌槽及其应用 - Google Patents

一种提锂脱嵌槽及其应用 Download PDF

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Publication number
WO2024259611A1
WO2024259611A1 PCT/CN2023/101568 CN2023101568W WO2024259611A1 WO 2024259611 A1 WO2024259611 A1 WO 2024259611A1 CN 2023101568 W CN2023101568 W CN 2023101568W WO 2024259611 A1 WO2024259611 A1 WO 2024259611A1
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WIPO (PCT)
Prior art keywords
lithium
lithium extraction
extraction
tank
ion sieve
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Ceased
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PCT/CN2023/101568
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English (en)
French (fr)
Inventor
李爱霞
余海军
谢英豪
李长东
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Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Original Assignee
Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
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Application filed by Hunan Brunp Recycling Technology Co Ltd, Guangdong Brunp Recycling Technology Co Ltd filed Critical Hunan Brunp Recycling Technology Co Ltd
Priority to PCT/CN2023/101568 priority Critical patent/WO2024259611A1/zh
Priority to CN202380009642.5A priority patent/CN117015622B/zh
Priority to ARP240100297A priority patent/AR131817A1/es
Publication of WO2024259611A1 publication Critical patent/WO2024259611A1/zh
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present disclosure belongs to the field of electrochemistry, for example, a lithium extraction and deintercalation cell and its application.
  • Electrochemical lithium extraction technology as a new type of lithium separation and extraction technology, has the advantages of being green and efficient.
  • the device used for electrochemical deintercalation lithium extraction from salt lakes has problems such as large inter-electrode spacing, insufficient brine flow, and poor solution mass transfer, which also seriously affects the lithium extraction rate in the process of electrochemical deintercalation lithium extraction from salt lakes.
  • each lithium extraction and deintercalation tank contains up to 100 or more yin and yang deintercalation units.
  • the maximum working current peak of a single yin and yang deintercalation unit can reach 20 to 60A, and the power supply working current output requirement of the entire lithium extraction and deintercalation tank is 2000 to 6000A. With the in-depth research and development of the technology, this current will be even greater.
  • the relevant technology usually adopts a constant current-constant voltage power supply mode to ensure that the working voltage during the lithium extraction process is within the safe voltage.
  • this power supply method makes it difficult for each electrode plate to fully exert its Efficiency, it is impossible to achieve the goal of efficient lithium extraction.
  • CN115276141A discloses a power supply method and system for an electrochemical deintercalation tank power supply, which provides a constant current for each working unit in the electrochemical deintercalation working group based on a preset constant current segment sequence, and collects the working voltage of each working unit in the electrochemical deintercalation working group in real time.
  • the working voltage of any working unit reaches a preset voltage threshold, it switches to the next constant current segment, or switches to the next constant current segment when a preset delay is reached.
  • the constant current segment sequence includes multiple constant current segments, the current corresponding to each constant current segment is different, which ensures the safety of the working unit while enabling the working unit to fully exert its effectiveness.
  • the process is very cumbersome, and it is difficult to control the boundaries of the transformation of different constant current segments, making it difficult to achieve large-scale production in industry.
  • the purpose of the present disclosure is to provide a lithium extraction and deintercalation tank and its application, by arranging a partition with openings in the main tank, and the openings of adjacent partitions are staggered up and down to form a plurality of connected, "assembly line" lithium extraction tanks, so that the lithium solution to be extracted is “bent” to the plurality of lithium extraction tanks, so that the lithium ion concentration in the lithium solution to be extracted is gradually reduced along the flow direction, and lithium extraction electrodes containing different lithium ion sieve materials are correspondingly arranged according to the change in concentration, and the lithium extraction electrodes are set to different constant current sections with successively decreasing working currents and/or different constant voltage sections with successively decreasing working voltages, so as to perform electrolytic lithium extraction, thereby realizing a simple, flexible and efficient lithium extraction method.
  • the present invention adopts the following technical solutions:
  • the present disclosure provides a lithium extraction and deintercalation cell, comprising a cathode main cell, an anode main cell, and a diaphragm disposed between the cathode main cell and the anode main cell;
  • a separator is arranged in the cathode main tank, and the separator divides the cathode main tank into at least two lithium extraction tanks;
  • the lithium extraction tank is provided with lithium extraction electrodes
  • the anode main tank is provided with deintercalation electrodes corresponding to the number of the lithium extraction electrodes, and the lithium extraction electrodes are electrically connected to the deintercalation electrodes through an external power supply;
  • the separator is provided with openings, and the openings between two adjacent separators are staggered up and down along the height direction of the lithium extraction tank, so that the lithium solution to be extracted flows in the cathode main tank in a baffled manner.
  • the present invention adopts an "assembly line” type lithium extraction tank setting method, wherein a plurality of lithium extraction tanks are connected, and each two tanks are separated by a partition.
  • the first partition is provided with a hole (i.e., an opening) near the bottom or near the top for the lithium extraction solution to be tested (such as brine) to enter
  • the second partition is provided with a hole near the top or near the bottom
  • the third partition is provided with a hole near the bottom or near the top, and so on, so that the holes between the connected partitions are arranged in an alternating manner up and down along the height direction of the partition, and the lithium extraction solution to be extracted is circulated to the last lithium extraction tank in a "baffled” manner in sequence, so that the lithium extraction solution to be extracted flows more fully, thereby improving the mass transfer effect of the solution, and is particularly suitable for lithium extraction from brine with high viscosity.
  • the partition is provided in the anode main tank, dividing the anode main tank into deintercalation tanks corresponding to each lithium extraction tank, and the number of deintercalation electrodes in the deintercalation tanks is the same as the number of lithium extraction electrodes in the corresponding lithium extraction tanks.
  • a deintercalation electrode corresponding to the number of lithium extraction electrodes can be set in the anode main tank, or a separator can be used to divide the anode main tank into multiple deintercalation tanks, each deintercalation tank and the corresponding lithium extraction tank are mass-transferred through a separator, and the deintercalation electrode in each deintercalation tank corresponds to the lithium extraction electrode in the corresponding lithium extraction tank.
  • the anode separator and the cathode separator can be the same or different, and are not limited to the same separator, and even the anode does not need to be set with a separator, especially when the cathode main tank uses an independent unit or each lithium extraction tank uses an independent power supply When the anode is used as the main tank, no partition is required.
  • the first lithium extraction tank and the first deintercalation tank are both provided with a liquid inlet, and the last lithium extraction tank and the last deintercalation tank are both provided with a liquid outlet.
  • the solution at this time can be discharged to facilitate the addition of new solution from the liquid inlet.
  • This flow process can be carried out continuously by controlling the liquid inlet speed, and can support continuous large-scale lithium extraction work.
  • the number of the lithium extraction tanks is 10 to 20, for example, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19 or 20.
  • the lithium extraction tank is divided into a high concentration tank, a medium concentration tank and a low concentration tank according to the change of the lithium ion concentration in the lithium solution to be extracted in the cathode main tank.
  • the lithium ion concentration in the lithium solution to be extracted in the baffled flow continuously decreases with the flow direction. Therefore, the present disclosure divides the lithium extraction tanks, and the lithium ion sieve material on the electrode plate in each lithium extraction tank is selected according to the concentration range of the brine passing through the tank.
  • the interval segment with high lithium ion concentration in the brine adopts a lithium ion sieve material with good selectivity, high adsorption capacity and stable chemical properties
  • the interval segment with medium lithium ion concentration in the brine adopts a lithium ion sieve material with good chemical stability but higher capacity
  • the interval segment with low lithium ion concentration in the brine adopts a lithium ion sieve material with high ion diffusion coefficient but lower capacity.
  • the concentration of lithium ions in the high concentration tank is greater than 0.1g/L, such as 0.12g/L, 0.17g/L, 0.2g/L, 0.25g/L, 0.3g/L, 0.35g/L, 0.4g/L, 0.45g/L or 0.5g/L, etc.
  • the concentration of lithium ions in the medium concentration tank is 0.01 to 0.1g/L, such as 0.01g/L, 0.02g/L, 0.
  • the concentration of lithium ions in the low concentration tank is less than 0.01 g/L, for example, 0.008 g/L, 0.006 g/L, 0.004 g/L, 0.002 g/L, etc., but is not limited to the listed values. Other values not listed within the above numerical ranges are also provided. The same applies to values.
  • the number of the high-concentration slots is 2 to 8, for example, 2, 3, 4, 5, 6, 7 or 8
  • the number of the medium-concentration slots is 1 to 9, for example, 1, 2, 3, 4, 5, 6, 7, 8 or 9
  • the number of the low-concentration slots is 1 to 9, for example, 1, 2, 3, 4, 5, 6, 7, 8 or 9.
  • a first lithium ion sieve material is provided in the high concentration tank, a second lithium ion sieve material is provided in the medium concentration tank, and a third lithium ion sieve material is provided in the low concentration tank;
  • the first lithium ion sieve material is less than the second lithium ion sieve material and less than the third lithium ion sieve material.
  • the adsorption capacity of the first lithium ion sieve material is 35-38 mg/g, for example, 35 mg/g, 35.3 mg/g, 35.6 mg/g, 35.9 mg/g, 36.2 mg/g, 36.5 mg/g, 36.8 mg/g, 37.1 mg/g, 37.4 mg/g, 37.7 mg/g or 38 mg/g
  • the adsorption capacity of the second lithium ion sieve material is 30-33 mg/g, for example, 30 mg/g, 30.3 mg/g, 30.6 mg/g, 30.9 mg/g, 31.2 mg/g, 31.3 mg/g, 31.7 mg/g, 31.9 mg/g, 31.8 mg/g, 31.9 mg/g, 31.9 mg/g, 31.9 mg/g, 31.9 mg/g, 31.9 mg/g, 31.1 mg/g, 31.2 mg/g, 31.3 mg/g, 31.4 mg/g, 31.6 mg/g, 31.7 mg/g, 31.8 mg/g, 31.9 mg/g, 3
  • the ion diffusion coefficient of the first lithium ion sieve material is 10 -10 ⁇ 10 -11 cm 2 /s, for example, 10 -10 cm 2 /s, 9*10 -11 cm 2 /s, 8*10 -11 cm 2 /s, 7*10 -11 cm 2 /s, 6*10 -11 cm 2 /s, 5*10 -11 cm 2 /s, 4*10 -11 cm 2 /s, 3*10 -11 cm 2 /s, 2*10 -11 cm 2 /s or 10 -11 cm 2 /s, etc.
  • the ion diffusion coefficient of the second lithium ion sieve material is 10 -9 ⁇ 10 -10 cm 2 /s, for example, 10 -9 cm 2 /s, 9*10 -10 cm 2 /s, 8*10 -10 cm 2 /s, 7*10 -10 cm 2 /s, 6*10 -10 cm 2 /s, 5*10 -10 cm 2 /s, 4*10
  • the first lithium ion sieve material, the second lithium ion sieve material and the third lithium ion sieve material are physical adsorption materials or electrochemical adsorption materials.
  • the first lithium ion sieve material, the second lithium ion sieve material and the third lithium ion sieve material are electrochemical adsorption materials
  • the first lithium ion sieve material, the second lithium ion sieve material and the third lithium ion sieve material are respectively arranged on the lithium extraction electrodes in the corresponding lithium extraction tanks.
  • the first lithium ion sieve material, the second lithium ion sieve material and the third lithium ion sieve material are physical adsorption materials:
  • the first lithium ion sieve material includes a manganese dioxide adsorbent; the second lithium ion sieve material includes a lithium silicate adsorbent; and the third lithium ion sieve material includes an aluminum hydroxide-based adsorbent.
  • the first lithium ion sieve material, the second lithium ion sieve material and the third lithium ion sieve material are electrochemical adsorption materials:
  • the first lithium ion sieve material includes a manganese oxide lithium ion sieve, such as at least one of lithium manganate LiMn 2 O 4 , Li 1.33 Mn 1.67 O 4 or Li 1.6 Mn 1.6 O 4 ;
  • the second lithium ion sieve material includes any one of lithium cobaltate, lithium vanadate or lithium iron phosphate or a combination of at least two thereof, and typical but non-limiting examples of the combination include a combination of lithium cobaltate and lithium iron phosphate, a combination of lithium cobaltate and lithium vanadate, or a combination of lithium vanadate and iron phosphate.
  • the third lithium ion sieve material includes a titanium oxide lithium ion sieve, such as lithium titanate Li 2 TiO 3 and/or Li 4 Ti 5 O 12 .
  • the lithium ion sieve material in the present disclosure needs to be selected according to the concentration range of the brine passing through the corresponding lithium extraction tank.
  • the specific selection requirements are as described above.
  • Technical personnel in this field can make reasonable selections and adjustments based on the actual working conditions or implementation conditions.
  • This application does not limit the first, second and third lithium ion sieve materials to the specific substances listed above.
  • each of the lithium extraction cells is equipped with a current and/or voltage monitor for monitoring the corresponding lithium extraction electrode.
  • the current and/or voltage monitor is electrically connected to a host, and the electrical connection refers to connection with the host through an electrical signal transmission line, and information communication is carried out by mutually transmitting electrical signals through the line.
  • the host is used to analyze, store and display the working status and replacement information of the lithium extraction electrode.
  • the opening on the partition is arranged close to the top end or the bottom end of the partition.
  • the distance between the edge of the opening and the top or bottom of the partition is 5% to 10% of the height of the partition, for example 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5% or 10%, etc., but is not limited to the listed values, and other values not listed within the above numerical range are also applicable.
  • the radius of the opening is 3 to 8 cm, for example 3 cm, 3.5 cm, 4 cm, 4.5 cm, 5 cm, 5.5 cm, 6 cm, 6.5 cm, 7 cm, 7.5 cm or 8 cm, but is not limited to the listed values, and other values not listed within the above numerical range are also applicable.
  • the lithium solution to be extracted and hot gas are introduced into the first lithium extraction tank at the same time, and flow in a zigzag manner in the cathode main tank to perform decreasing constant current electrolysis and/or decreasing constant voltage electrolysis for lithium extraction.
  • the anode main tank may not be provided with a partition, and hot air may not be introduced.
  • the decreasing constant current electrolysis for lithium extraction includes that during the process of electrolysis for lithium extraction, the working current of the lithium extraction electrode itself in the lithium extraction tank remains unchanged, and along the flow direction of the lithium solution to be extracted, the working current of the lithium extraction electrode decreases successively or in stages.
  • the difference in working current between two adjacent lithium extraction electrodes is 0.5 to 7 A, for example 0.5 A, 1 A, 1.5 A, 2 A, 2.5 A, 3 A, 3.5 A, 4 A, 4.5 A, 5 A, 5.5 A, 6 A, 6.5 A or 7 A, but is not limited to the listed values, and other values not listed within the above numerical range are also applicable.
  • the various lithium extraction electrodes in the decreasing constant current electrolysis lithium extraction are electrically connected in parallel, or each lithium extraction electrode is individually controlled by an independent power supply to achieve constant current.
  • the decreasing constant-voltage electrolysis for lithium extraction includes that during the process of electrolysis for lithium extraction, the working voltage of the lithium extraction electrode in the lithium extraction tank remains unchanged, and along the flow direction of the lithium solution to be extracted, the working voltage of the lithium extraction electrode decreases sequentially or in stages.
  • the difference in working voltages of two adjacent lithium extraction electrodes is 0.05 to 0.15 V, for example, 0.05 V, 0.06 V, 0.07 V, 0.08 V, 0.09 V, 0.1 V, 0.11 V, 0.12 V, 0.13 V, 0.14 V or 0.15 V, etc., but is not limited to the listed values, and other values not listed within the above numerical range are also applicable.
  • One of the purposes of the present disclosure is to gradually reduce the concentration of the lithium solution to be extracted along the flow direction by dividing the lithium solution with the partition. Therefore, the working parameters of the lithium extraction electrode should be adjusted according to the actual concentration of the lithium solution to be extracted in the lithium extraction tank. Adjustment. For the case where the lithium ion concentration in the lithium extraction tank within two or three adjacent tanks or a certain interval section does not change significantly, the lithium extraction tank can also be segmented or partitioned. Taking the decreasing constant current electrolysis as an example, the working current of the lithium extraction electrode in each lithium extraction tank after segmentation is the same, and the working current of the lithium extraction electrode between adjacent sections decreases successively along the flow direction of the solution.
  • the working current in the first lithium extraction tank is determined according to the initial concentration of the lithium solution to be extracted.
  • the number of lithium extraction tanks and the amplitude of the working current change need to be adjusted according to the actual lithium extraction goals and effects, so that the lithium ion concentration in the solution in the last lithium extraction tank is reduced to below the target requirements. Therefore, the key to the present disclosure is to maintain the overall downward trend of the working current of the lithium extraction electrode along the flow direction of the solution.
  • the change in the working voltage in the decreasing constant voltage electrolysis can also be segmented.
  • the various lithium extraction electrodes in the decreasing constant voltage electrolysis lithium extraction are electrically connected in series.
  • the present disclosure provides an application of the lithium extraction and deintercalation trough as described in the first aspect for lithium extraction, and the application of the lithium extraction and deintercalation trough for lithium extraction includes: along the flow direction of the lithium solution to be extracted, the cathode main tank is divided into a front section and a rear section, the lithium extraction tank in the front section performs the decreasing constant current electrolysis lithium extraction, and the lithium extraction tank in the rear section performs the decreasing constant pressure lithium extraction.
  • the lithium extraction tank disclosed in the present invention is preferably set to different constant currents from high to low or constant current in the front section and constant voltage in the back section from the front to the back (i.e., the direction from the liquid inlet to the liquid outlet of the cathode main tank).
  • the application is more flexible and energy-saving, and avoids the tedious operation of changing the power supply method for the electrode.
  • the ratio of the number of lithium extraction tanks in the front section to the number of lithium extraction tanks in the rear section is greater than or equal to 2, for example, 2, 3, 4, 5, 6, 7 or 8, but is not limited to the listed values, and other unlisted values within the above numerical range are also applicable.
  • the lithium solution to be extracted includes brine.
  • the concentration of lithium ions in the brine is 0.2-0.8 g/L, for example 0.2 g/L, 0.25 g/L, 0.3 g/L, 0.35 g/L, 0.4 g/L, 0.45 g/L, 0.5 g/L, 0.55 g/L, 0.6 g/L, 0.65 g/L, 0.7 g/L, 0.75 g/L or 0.8 g/L, etc., but is not limited to the listed values, and other values not listed within the above numerical range are also applicable.
  • the flow rate of the lithium solution to be extracted is 1 to 5 L/h, for example, 1 L/h, 1.5 L/h, 2 L/h, 2.5 L/h, 3 L/h, 3.5 L/h, 4 L/h, 4.5 L/h or 5 L/h, but is not limited to the listed values, and other values not listed within the above numerical range are also applicable.
  • the temperature of the hot air is 35-40°C, such as 35°C, 36°C, 37°C, 38°C, 39°C or 40°C, but is not limited to the listed values, and other unlisted values within the above range are also applicable.
  • the hot gas includes air and/or an inert gas.
  • the flow ratio of the hot gas to the lithium solution to be extracted is 1:(1-2), for example 1:1, 1:1.1, 1:1.2, 1:1.3, 1:1.4, 1:1.5, 1:1.6, 1:1.7, 1:1.8, 1:1.9 or 1:2, etc., but is not limited to the listed values, and other unlisted values within the above numerical range are also applicable.
  • the application further includes introducing pure water and/or sodium chloride solution into the anode main tank while simultaneously introducing the lithium solution to be extracted and hot gas from the first lithium extraction tank.
  • the current and/or voltage of the lithium extraction electrode in the lithium extraction tank is monitored, and when it exceeds a preset value, the corresponding lithium extraction electrode is replaced.
  • the lithium extraction and deintercalation tank disclosed in the present invention is provided by connecting multiple lithium extraction tanks in an "assembly line” manner.
  • the lithium solution to be extracted in the lithium extraction tank is made to flow in a "bend flow” manner and the lithium ion concentration is distributed from high to low, so that the lithium ion sieve material of the lithium extraction electrode is set accordingly according to the different lithium ion concentrations in each lithium extraction tank, and resources are reasonably allocated, so as to reduce costs while efficiently extracting lithium;
  • the lithium extraction and deintercalation tank disclosed in the present invention is used for lithium extraction.
  • a decreasing constant current electrolysis is performed to extract lithium, or a decreasing constant current electrolysis is performed in the front stage to extract lithium, and a decreasing constant voltage electrolysis is performed in the back stage to extract lithium.
  • the setting of this scheme is more flexible and avoids the cumbersome operation of changing the power supply mode of the electrode;
  • the lithium extraction and deintercalation cell disclosed in the present invention is used for lithium extraction.
  • hot gas is also introduced.
  • the flow of the lithium solution to be extracted is sufficient, the mass transfer effect of the solution is improved, and the lithium extraction efficiency of the electrolytic cell is effectively improved.
  • FIG1 is a schematic diagram of a cathode main tank in a lithium extraction and deintercalation tank of Example 1;
  • FIG2 is a schematic diagram of the cathode main tank in the lithium extraction and deintercalation tank of Example 2;
  • FIG3 is a schematic top view of the lithium extraction and deintercalation tank of Example 1 and Example 2;
  • FIG4 is a schematic top view of the lithium extraction and deintercalation tank of Example 4.
  • 1- cathode main tank 11- liquid inlet, 12- liquid outlet, 2- partition, 21- opening, 3- diaphragm, 4- lithium extraction electrode, 5- deintercalation electrode, 6- lithium solution to be extracted, 7- external power supply, 8- anode main tank.
  • This embodiment provides a lithium extraction and deintercalation cell and its application, as shown in Figures 1 and 3:
  • the lithium extraction and deintercalation tank comprises a cathode main tank 1, an anode main tank 8, and a diaphragm 3 between the cathode main tank 1 and the anode main tank 8; a diaphragm 2 is arranged in the cathode main tank 1, and the diaphragm 2 divides the cathode main tank 1 into 15 lithium extraction tanks connected in sequence; a diaphragm 2 is also arranged in the anode main tank 8, and the diaphragm 2 divides the anode main tank 8 into 15 deintercalation tanks connected in sequence corresponding to the lithium extraction tanks; the first lithium extraction tank and the first deintercalation tank are both provided with a liquid inlet 11, and the last lithium extraction tank and the last deintercalation tank are both provided with a liquid outlet 12;
  • the lithium extraction tank is provided with a lithium extraction electrode 4, and the lithium extraction electrodes 4 are electrically connected in parallel;
  • the deintercalation tank is provided with a deintercalation electrode 5, and the deintercalation electrodes 5 are electrically connected in parallel, and the lithium extraction electrode 4 is electrically connected to the deintercalation electrode 5 through an external power supply 7;
  • the separator 2 is provided with openings 21, and the openings 21 between two adjacent separators 2 are arranged in an up-and-down staggered manner along the height direction of the lithium extraction tank or the deintercalation tank.
  • the opening 21 of the first separator 2 is arranged at a position 10 cm away from the top of the separator 2, and is a circle with a radius of 5 cm.
  • the opening 21 of the second separator 2 is arranged at a position 10 cm away from the bottom of the separator 2, and is a circle with a radius of 5 cm.
  • the opening 21 of the third separator 2 is the same as the first separator 2, and so on.
  • a total of 15 separators 2 are provided, so that the lithium solution 6 to be extracted flows in the cathode main tank 1 and the anode main tank 8 in a baffled manner;
  • the lithium extraction tank is divided into 5 high concentration tanks, 5 medium concentration tanks and 5 low concentration tanks according to the change of lithium ion concentration in the lithium extraction tank;
  • the lithium ion sieve material of the lithium extraction electrode 4 in the high concentration tank is LiMn 2 O 4 with high adsorption capacity and good selectivity;
  • the lithium ion sieve material of the lithium extraction electrode 4 is lithium iron phosphate with good chemical stability, relatively low ion diffusion coefficient and high capacity;
  • the lithium ion sieve material of the lithium extraction electrode 4 in the low concentration tank is Li 2 TiO 3 with high diffusion coefficient, good stability but low capacity;
  • a voltage monitor is installed in each of the lithium extraction tanks for monitoring the corresponding lithium extraction electrode 4 ; the voltage monitor is electrically connected to a host, and the host is used to analyze, store and display the working status and replacement information of the lithium extraction electrode 4 .
  • the lithium solution 6 to be extracted and hot air are introduced from the first lithium extraction tank at the same time, and flow in the cathode main tank 1 in a zigzag manner.
  • pure water is introduced from the first deintercalation tank and flows in the anode main tank 8 in a zigzag manner.
  • the lithium solution 6 to be extracted is brine with a lithium ion concentration of 0.5 g/L, and the flow rate of the brine is 3 L/h.
  • the hot air is hot air with a temperature of 37° C. and a flow rate of 4.5 L/h.
  • the working current of the lithium extraction electrode 4 is set according to Table 1, wherein the lithium extraction electrode 4 in the first lithium extraction tank is the first lithium extraction electrode 4, and its working current is recorded as A1, and the second lithium extraction tank is adjacent to the first lithium extraction tank in the direction close to the anode area, and its working current is recorded as A2, A1>A2, and so on, to perform decreasing constant current electrolysis to extract lithium;
  • This embodiment provides a lithium extraction and deintercalation cell and its application, as shown in Figures 2 and 3:
  • the lithium extraction and deintercalation tank comprises a cathode main tank 1, an anode main tank 8, and a diaphragm 3 between the cathode main tank 1 and the anode main tank 8; a diaphragm 2 is arranged in the cathode main tank 1, and the diaphragm 2 divides the cathode main tank 1 into 15 lithium extraction tanks connected in sequence; a diaphragm 2 is also arranged in the anode main tank 8, and the diaphragm 2 divides the anode main tank 8 into 15 deintercalation tanks connected in sequence corresponding to the lithium extraction tank; a lithium extraction electrode 4 is arranged in the lithium extraction tank, and a deintercalation electrode 5 is arranged in the deintercalation tank, and the lithium extraction electrode 4 is electrically connected to the deintercalation electrode 5 through an external power supply 7; the first lithium extraction tank and the first deintercalation tank are both provided with a liquid inlet 11, and the last lithium extraction tank and the last deintercalation tank are both
  • the separator 2 is provided with openings 21, and the openings 21 between two adjacent separators 2 are arranged in an up-and-down staggered manner along the height direction of the lithium extraction tank or the deintercalation tank.
  • the opening 21 of the first separator 2 is arranged at a position 10 cm away from the top of the separator 2, and is a circle with a radius of 5 cm.
  • the opening 21 of the second separator 2 is arranged at a position 10 cm away from the bottom of the separator 2, and is a circle with a radius of 5 cm.
  • the opening 21 of the third separator 2 is the same as the first separator 2, and so on.
  • a total of 15 separators 2 are provided, so that the lithium solution 6 to be extracted flows in the cathode main tank 1 and the anode main tank 8 in a baffled manner;
  • the lithium extraction tank is divided into 5 high-concentration tanks, 5 medium-concentration tanks and 5 low-concentration tanks according to the change of the lithium ion concentration in the lithium extraction tank;
  • the lithium ion sieve material of the lithium extraction electrode 4 in the high-concentration tank is LiMn 2 O 4 with high adsorption capacity and good selectivity;
  • the lithium ion sieve material of the lithium extraction electrode 4 in the medium-concentration tank is lithium iron phosphate with good chemical stability, relatively low ion diffusion coefficient and high capacity;
  • the lithium ion sieve material of the lithium extraction electrode 4 in the low-concentration tank is Li 2 TiO 3 with high diffusion coefficient, good stability but low capacity;
  • the lithium extraction electrode 4 in the first lithium extraction tank is the first lithium extraction electrode 4
  • the lithium extraction electrode 4 in the second lithium extraction tank is the second lithium extraction electrode 4, and so on
  • the cathode main tank 1 is divided into a front section and a rear section, the front section includes the first lithium extraction electrode 4 to the tenth lithium extraction electrode 4, and the rear section includes the eleventh lithium extraction electrode 4 to the fifteenth lithium extraction electrode 4; the lithium extraction electrodes 4 in the front section are electrically connected in parallel, and the lithium extraction electrodes 4 in the rear section are electrically connected in series;
  • a voltage monitor is installed in each of the lithium extraction tanks for monitoring the corresponding lithium extraction electrode 4 ; the voltage monitor is electrically connected to a host, and the host is used to analyze, store and display the working status and replacement information of the lithium extraction electrode 4 .
  • the lithium solution 6 to be extracted and hot air are introduced from the first lithium extraction tank at the same time, and flow in the cathode main tank 1 in a zigzag manner.
  • the sodium chloride solution is introduced from the first deintercalation tank, and flows in the anode main tank 8 in a zigzag manner.
  • the lithium solution 6 to be extracted is brine with a lithium ion concentration of 0.5 g/L, and the flow rate of the brine is 3 L/h.
  • the hot air is hot air with a temperature of 40° C. and a flow rate of 6 L/h.
  • the working current and working voltage of the lithium extraction electrode 4 are set according to Table 2, wherein the working current of the first lithium extraction electrode 4 is recorded as A1, the working current of the second lithium extraction electrode 4 is recorded as A2, A1>A2, and so on, the working voltage of the eleventh lithium extraction electrode 4 is recorded as V1, the working voltage of the twelfth lithium extraction electrode 4 is recorded as V2, and so on; the lithium extraction tank in the front section performs the said decreasing constant current electrolysis lithium extraction, and the lithium extraction tank in the said rear section performs the said decreasing constant voltage lithium extraction;
  • the voltage monitor When the real-time working voltage of the lithium extraction electrode 4 in a lithium extraction tank exceeds the set safety constant voltage of 0.8V, the voltage monitor will sound an alarm and a new lithium extraction electrode 4 will be replaced accordingly until the electrolytic lithium extraction is completed.
  • This embodiment provides a lithium extraction and deintercalation tank and its application.
  • the lithium extraction and deintercalation tank is exactly the same as that in embodiment 1.
  • the difference between the use and embodiment 1 is as follows:
  • the working voltage of the lithium extraction electrode 4 is set according to Table 3, wherein the lithium extraction electrode 4 in the first lithium extraction tank is the first lithium extraction electrode 4, and its working voltage is recorded as V1, and the lithium extraction electrode 4 in the second lithium extraction tank is the second lithium extraction electrode 4, and its working voltage is recorded as V2, V1>V2, and so on, to perform decreasing constant voltage electrolysis to extract lithium;
  • This embodiment provides a lithium extraction and deintercalation cell and its application. As shown in FIG. 4 , no separator 2 is provided in the anode main cell 8 of the lithium extraction and deintercalation cell. Apart from this, other conditions are exactly the same as those in Embodiment 1.
  • This comparative example provides a lithium extraction and deintercalation cell and its use, wherein the lithium extraction and deintercalation cell is exactly the same as that in Example 1, and the difference between the application and Example 1 is that the working current of all lithium extraction electrodes 4 is set to 25A, and other conditions are exactly the same as those in Example 1.
  • This comparative example provides a lithium extraction and deintercalation cell and its application.
  • the lithium extraction and deintercalation cell is exactly the same as that in Example 1.
  • the difference between the application and Example 1 is that the working current of all lithium extraction electrodes 4 is set to 1A, and other conditions are exactly the same as those in Example 1.
  • This comparative example provides a lithium extraction and deintercalation tank and its use.
  • the difference between the lithium extraction and deintercalation tank and Example 1 is that the openings 21 of all the partitions 2 are uniformly set to a position 10 cm close to the bottom of the partition 2, and are circular with a radius of 5 cm, so that the lithium solution 6 to be extracted is not allowed to flow in a baffled manner.
  • other conditions and application parameters of the lithium extraction and deintercalation tank are exactly the same as those of Example 1.
  • This comparative example provides a lithium extraction and deintercalation cell and its application.
  • the difference between the lithium extraction and deintercalation cell and Example 1 is that the lithium ion sieve material of all lithium extraction electrodes 4 is set to LiMn 2 O 4 .
  • other conditions and application parameters of the lithium extraction and deintercalation cell are exactly the same as those of Example 1.
  • This comparative example provides a lithium extraction and deintercalation cell and its use.
  • the lithium extraction and deintercalation cell is different from Example 1 in that the lithium ion sieve material of all lithium extraction electrodes 4 is set to Li 2 TiO 3 .
  • other conditions and application parameters of the lithium extraction and deintercalation cell are exactly the same as those of Example 1.
  • This comparative example provides a lithium extraction and deintercalation cell and its application.
  • the lithium extraction and deintercalation cell is different from Example 1 in that hot air is not used and only the lithium solution 6 to be extracted is introduced. Apart from this, other conditions and application parameters of the lithium extraction and deintercalation cell are exactly the same as those of Example 1.
  • the power supply method of the electrolytic cell of this scheme is preferably power supply at different constant current sections. It can be seen from Example 1 compared to Example 4 that whether the anode has a partition has no effect on the results of this scheme; compared to Comparative Example 1, Example 1 uses a continuous high current as the power supply method, and the electrode plate easily exceeds the safety voltage, affecting lithium extraction, and both energy consumption and cost are high; Comparative Example 2 uses a low current, and the lithium extraction efficiency is extremely low; Comparative Example 3 has openings at the bottom that will cause the brine in the lithium extraction tank to flow too fast, making it impossible to extract lithium normally; compared to Comparative Examples 4-5, Example 1 uses a lithium ion sieve with a higher capacity at low concentrations that will affect the lithium extraction efficiency, while using a lithium ion sieve with a lower capacity in high-concentration brine that will increase the number of times the lithium ion sieve is replaced, and the operation is cumbersome

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Abstract

本公开提供了一种提锂脱嵌槽及其应用，通过在主槽内设置带有开孔的隔板，且相邻隔板的开孔上下交错布置来形成多个相连的、"流水线式"的提锂槽，让待提锂溶液"折流式"地通往多个提锂槽中，使待提锂溶液中的锂离子浓度沿流动方向逐渐降低，根据浓度的变化对应设置含有不同锂离子筛材料的提锂电极，并且将提锂电极设置为工作电流依次递减的不同恒流段和/或工作电压依次递减的不同恒压段，以进行电解提锂，从而实现简单，灵活，高效的提锂方式。

Description

一种提锂脱嵌槽及其应用 技术领域
本公开属于电化学领域，例如一种提锂脱嵌槽及其应用。
背景技术
随着新能源汽车的快速发展，动力电池对锂的需求量在近几年迅速增长。锂作为重要的新能源材料和战略储备资源，被誉为“21世纪的能源金属”，其开发和利用受到全球的高度关注。据相关数据统计，全球锂资源总量达4000万吨，其中卤水(包括盐湖卤水、地下卤水、浓海水等)中的储量约占总储量的70％。由于有限的优质固体矿资源的开采受限，而卤水提锂具有成本和规模优势，因此，对卤水锂资源的开发利用成为必然趋势。
电化学提锂技术，作为一种新型的锂分离提取技术，具有绿色、高效等优点，然而，目前，针对电化学提锂装置及提锂方法的研究相对较少。由于卤水锂离子浓度低、矿化度高、黏度大等特性，导致电化学脱嵌法盐湖提锂过程中提锂速率较低。此外，用于电化学脱嵌法盐湖提锂的装置存在极间距大、卤水流动不充分、溶液传质效果不佳等问题，也严重影响了电化学脱嵌法盐湖提锂过程中的提锂速率。相关技术中，针对大规模工业化的生产的需要，每个提锂脱嵌槽含有的阴阳脱嵌单元可达100个或更多，针对不同的处理待提锂溶液，单个阴阳脱嵌单元工作最大电流峰值可达20～60A，那整个提锂脱嵌槽的电源工作电流输出要求达2000～6000A，随着技术的深入研究发展，此电流甚至会更大。对于2米长的提锂脱嵌槽，由于每对阴阳脱嵌单元之间的施加工作电压不能超过1V或更低，因此，相关技术通常采用恒流-恒压的供电模式，以保证提锂过程中的工作电压在安全电压内。但这种供电方式很难使每个电极板完全发挥其 效能，无法达到高效提锂的目的。
CN115276141A公开了一种电化学脱嵌槽电源的供电方法及系统，其基于预设的恒流段序列为电化学脱嵌工作组中各工作单元提供恒定电流，实时采集电化学脱嵌工作组中各工作单元的工作电压。在任意工作单元的工作电压达到预设电压阈值时，切换到下一恒流段，或在达到预设延时，切换到下一恒流段。由于恒流段序列中包括多个恒流段，各恒流段对应的电流不同，保证了工作单元安全的同时还可以使工作单元充分发挥效能。但其过程很繁琐，且很难控制不同恒流段变换的界限，工业上难以实现大规模生产。
因此，尚需要开发新的卤水电化学提锂的技术方案，以解决基于电化学脱嵌提锂技术存在的缺陷及问题。
发明内容
以下是对本文详细描述的主题的概述。本概述并非是为了限制权利要求的保护范围。
鉴于相关技术中存在的问题，本公开的目的在于提供一种提锂脱嵌槽及其应用，通过在主槽内设置带有开孔的隔板，且相邻隔板的开孔上下交错布置来形成多个相连的、“流水线式”的提锂槽，让待提锂溶液“折流式”地通往多个提锂槽中，使待提锂溶液中的锂离子浓度沿流动方向逐渐降低，根据浓度的变化对应设置含有不同锂离子筛材料的提锂电极，并且将提锂电极设置为工作电流依次递减的不同恒流段和/或工作电压依次递减的不同恒压段，以进行电解提锂，从而实现简单，灵活，高效的提锂方式。
为达此目的，本公开采用以下技术方案：
第一方面，本公开提供了一种提锂脱嵌槽，包括阴极主槽、阳极主槽，以及设置在阴极主槽与阳极主槽之间的隔膜；
所述阴极主槽内设置有隔板，所述隔板将所述阴极主槽划分为至少两个提锂槽；
所述提锂槽中设置有提锂电极，所述阳极主槽中设置有与所述提锂电极的数量相对应的脱嵌电极，所述提锂电极与所述脱嵌电极通过外部电源电性相连；
所述隔板上设置有开孔，相邻两个隔板之间的开孔沿所述提锂槽的高度方向上下交错排列，使待提锂溶液在所述阴极主槽内折流式流动。
本公开采用“流水线”式提锂槽设置方式，多个提锂槽相连，每两个槽之间用隔板分开，第1个隔板靠近底部或靠近顶部设置一个待测提锂溶液(如卤水)进入的孔洞(即开孔)，第2个隔板在靠近顶部或靠近底部设置孔洞，第3个隔板在靠近底部或靠近顶部设置孔洞，以此类推，使得相连隔板间的孔洞沿隔板的高度方向交错上下排布，则待提锂溶液以“折流式”依次循环到最后一个提锂槽，从而使待提锂溶液流动更加充分，提高溶液的传质效果，尤其是适用于黏度大的卤水的提锂。
以下作为本公开可选的技术方案，但不作为本公开提供的技术方案的限制，通过以下技术方案，可以更好地达到和实现本公开的技术目的和有益效果。
作为本公开可选的技术方案，所述阳极主槽内设置有所述隔板，将所述阳极主槽划分为与每个提锂槽相对应的脱嵌槽，所述脱嵌槽内的脱嵌电极的数量与对应的提锂槽内的提锂电极的数量相同。
本公开中，可以在阳极主槽内设置与提锂电极数量相对应的脱嵌电极，也可以使用隔板将阳极主槽划分成多个脱嵌槽，每个脱嵌槽与对应的提锂槽通过隔膜进行传质，且每个脱嵌槽中的脱嵌电极与对应的提锂槽中的提锂电极相对应。即，阳极隔板与阴极隔板可以相同，也可以不同，不限制同一隔板，甚至阳极无需设置隔板，尤其在阴极主槽采用独立单元或每个提锂槽采用独立电源 时，阳极主槽内可不设置隔板。
在一个实施例中，第一个提锂槽及第一个脱嵌槽均设置有进液口，最后一个提锂槽及最后一个脱嵌槽均设置有出液口。
在使用本公开所述的提锂脱嵌槽进行提锂时，待提锂流经最后一个提锂槽时，锂离子的提取率已经达到目标要求，因此，可以将此时的溶液排出，以便于从进液口补入新的溶液，此流动过程通过控制进液速度可持续不断地进行，可以支持连续大量的提锂工作。
在一个实施例中，所述提锂槽的数量为10～20个，例如10个、11个、12个、13个、14个、15个、16个、17个、18个、19个或20个。
作为本公开可选的技术方案，根据所述阴极主槽内的所述待提锂溶液中的锂离子浓度的变化，将所述提锂槽分为高浓度槽、中浓度槽及低浓度槽。
折流式流动的待提锂溶液中的锂离子浓度随着流动方向不断地降低，因此，本公开将提锂槽进行划分，各提锂槽中电极板上的锂离子筛材料根据该槽中通过的卤水的浓度的区间来进行选择，卤水中锂离子浓度高的区间段采用选择性好、吸附量高且化学性质稳定的锂离子筛材料，卤水中锂离子浓度中等的区间段采用化学稳定性较好但容量较高的锂离子筛材料，卤水中锂离子浓度较低的区间段采用离子扩散系数高但容量较低的锂离子筛材料。
作为本公开可选的技术方案，所述高浓度槽中锂离子的浓度大于0.1g/L，例如0.12g/L、0.17g/L、0.2g/L、0.25g/L、0.3g/L、0.35g/L、0.4g/L、0.45g/L或0.5g/L等，所述中浓度槽中锂离子的浓度为0.01～0.1g/L，例如0.01g/L、0.02g/L、0.03g/L、0.04g/L、0.05g/L、0.06g/L、0.07g/L、0.08g/L、0.09g/L或0.1g/L等，所述低浓度槽中锂离子的浓度为小于0.01g/L，例如0.008g/L、0.006g/L、0.004g/L或0.002g/L等，但并不仅限于所列举的数值，上述数值范围内其他未列举的数 值同样适用。
作为本公开可选的技术方案，所述高浓度槽的数量为2～8个，例如2个、3个、4个、5个、6个、7个或8个，所述中浓度槽的数量为1～9个，例如1个、2个、3个、4个、5个、6个、7个、8个或9个，所述低浓度槽的数量为1～9个，例如1个、2个、3个、4个、5个、6个、7个、8个或9个。
作为本公开可选的技术方案，所述高浓度槽中设置有第一锂离子筛材料、所述中浓度槽中设置有第二锂离子筛材料、所述低浓度槽中设置有第三锂离子筛材料；
按每单位质量的吸附容量比较，所述第一锂离子筛材料＞所述第二锂离子筛材料＞所述第三锂离子筛材料；
按每单位质量的离子扩散系数比较，所述第一锂离子筛材料＜所述第二锂离子筛材料＜所述第三锂离子筛材料。
作为本公开可选的技术方案，所述第一锂离子筛材料的吸附容量为35～38mg/g，例如35mg/g、35.3mg/g、35.6mg/g、35.9mg/g、36.2mg/g、36.5mg/g、36.8mg/g、37.1mg/g、37.4mg/g、37.7mg/g或38mg/g等，所述第二锂离子筛材料的吸附容量为30～33mg/g，例如30mg/g、30.3mg/g、30.6mg/g、30.9mg/g、31.2mg/g、31.5mg/g、31.8mg/g、32.1mg/g、32.4mg/g、32.7mg/g或33mg/g等，所述第三锂离子筛材料的吸附容量为12～15mg/g，例如12mg/g、12.3mg/g、12.6mg/g、12.9mg/g、13.2mg/g、13.5mg/g、13.8mg/g、14.1mg/g、14.4mg/g、14.7mg/g或15mg/g等，但并不仅限于所列举的数值，上述数值范围内其他未列举的数值同样适用。
作为本公开优选的技术方案，所述第一锂离子筛材料的离子扩散系数为10-10～10-11cm2/s，例如10-10cm2/s、9*10-11cm2/s、8*10-11cm2/s、7*10-11cm2/s、 6*10-11cm2/s、5*10-11cm2/s、4*10-11cm2/s、3*10-11cm2/s、2*10-11cm2/s或10-11cm2/s等，所述第二锂离子筛材料的离子扩散系数为10-9～10-10cm2/s，例如10-9cm2/s、9*10-10cm2/s、8*10-10cm2/s、7*10-10cm2/s、6*10-10cm2/s、5*10-10cm2/s、4*10-10cm2/s、3*10-10cm2/s、2*10-10cm2/s或10-10cm2/s等，所述第三锂离子筛材料的离子扩散系数为10-7～10-8cm2/s，例如10-7cm2/s、9*10-8cm2/s、8*10-8cm2/s、7*10-8cm2/s、6*10-8cm2/s、5*10-8cm2/s、4*10-8cm2/s、3*10-8cm2/s、2*10-8cm2/s或10-8cm2/s等，但并不仅限于所列举的数值，上述数值范围内其他未列举的数值同样适用。
作为本公开可选的技术方案，所述第一锂离子筛材料、所述第二锂离子筛材料及所述第三锂离子筛材料为物理吸附材料或电化学吸附材料。
在一个实施例中，当所述第一锂离子筛材料、所述第二锂离子筛材料及所述第三锂离子筛材料为电化学吸附材料时，所述第一锂离子筛材料、所述第二锂离子筛材料及所述第三锂离子筛材料分别设置于对应的提锂槽中的提锂电极上。
作为本公开可选的技术方案，当所述第一锂离子筛材料、所述第二锂离子筛材料及所述第三锂离子筛材料为物理吸附材料时：
所述第一锂离子筛材料包括二氧化锰吸附剂；所述第二锂离子筛材料包括硅酸锂吸附剂；所述第三锂离子筛材料包括氢氧化铝基吸附剂。
作为本公开可选的技术方案，当所述第一锂离子筛材料、所述第二锂离子筛材料及所述第三锂离子筛材料为电化学吸附材料时：
所述第一锂离子筛材料包括锰氧化物锂离子筛，例如锰酸锂LiMn2O4、Li1.33Mn1.67O4或Li1.6Mn1.6O4中的至少一种；所述第二锂离子筛材料包括钴酸锂、钒酸锂或磷酸铁锂中的任一种或至少两种的组合，所述组合典型但非限制性的实例包括钴酸锂与磷酸铁锂的组合、钴酸锂与钒酸锂的组合或钒酸锂与磷酸铁 锂的组合；所述第三锂离子筛材料包括钛氧化物锂离子筛，例如钛酸锂Li2TiO3和/或Li4Ti5O12。
需要说明的是，本公开中锂离子筛材需要根据对应提锂槽中通过的卤水的浓度的区间来进行选择，具体选择要求如上所述，本领域的技术人员可以根据实际面对的工况或实施条件来进行合理的选择和调整，本申请并不限定所述第一、第二及第三锂离子筛材料一定为上述所列举的具体物质。
作为本公开可选的技术方案，每个所述提锂槽中安装有电流和/或电压监测器，用于监控对应的提锂电极。
在一个实施例中，所述电流和/或电压监测器电性连接于主机，所述电性连接是指通过电信号传输线路与主机进行连接，通过线路互相传递电信号进行信息沟通，所述主机用于分析、存储并显示所述提锂电极的工作状态及更换信息。
作为本公开可选的技术方案，所述隔板上的开孔靠近所述隔板的顶端或底端设置。
在一个实施例中，沿所述隔板的高度方向，所述开孔的边缘与所述隔板顶端或底端的距离占所述隔板高度的5％～10％，例如5％、5.5％、6％、6.5％、7％、7.5％、8％、8.5％、9％、9.5％或10％等，但并不仅限于所列举的数值，上述数值范围内其他未列举的数值同样适用。
在一个实施例中，所述开孔的半径为3～8cm，例如3cm、3.5cm、4cm、4.5cm、5cm、5.5cm、6cm、6.5cm、7cm、7.5cm或8cm等，但并不仅限于所列举的数值，上述数值范围内其他未列举的数值同样适用。
作为本公开可选的技术方案，包括如下步骤：
由第1个提锂槽同时通入待提锂溶液与热气，并在所述阴极主槽内折流式流动，进行递减式恒流电解提锂和/或递减式恒压电解提锂。
新鲜待提锂溶液通入提锂槽的过程中顺带通入热的空气，既能提高提锂过程中的温度，又能搅动待提锂溶液，进一步促进待提锂溶液的流动和传质效果，有效提高提锂槽的提锂效率。需要说明的是，由于阳极主槽内的脱锂速率比阴极主槽内的提锂速率快得多，故阳极主槽内可以不设置隔板，也可以不通入热气。
作为本公开可选的技术方案，所述递减式恒流电解提锂包括，在电解提锂的过程中，提锂槽内的提锂电极自身的工作电流保持不变，沿待提锂溶液的流动方向，提锂电极的工作电流依次减小或分段式依次减小。
在一个实施例中，在所述递减式恒流电解提锂中，相邻两个提锂电极的工作电流的差值为0.5～7A，例如0.5A、1A、1.5A、2A、2.5A、3A、3.5A、4A、4.5A、5A、5.5A、6A、6.5A或7A等，但并不仅限于所列举的数值，上述数值范围内其他未列举的数值同样适用。
在一个实施例中，所述递减式恒流电解提锂中的各个提锂电极为并联式电连接，或每个提锂电极通过互相独立的电源进行单独控制实现恒流。
作为本公开可选的技术方案，所述递减式恒压电解提锂包括，在电解提锂的过程中，提锂槽内的提锂电极自身的工作电压保持不变，沿待提锂溶液的流动方向，提锂电极的工作电压依次减小或分段式依次减小。
在一个实施例中，在所述递减式恒压电解提锂中，相邻两个提锂电极的工作电压的差值为0.05～0.15V，例如0.05V、0.06V、0.07V、0.08V、0.09V、0.1V、0.11V、0.12V、0.13V、0.14V或0.15V等，但并不仅限于所列举的数值，上述数值范围内其他未列举的数值同样适用。
本公开的目的之一在于通过隔板的划分，使待提锂溶液浓度随流动方向逐渐减小，因此，提锂电极的工作参数应根据提锂槽内待提锂溶液实际的浓度进 行调整。对于相邻的两三个槽或某个区间段内的提锂槽中的锂离子浓度变化不明显的情况，也可以选择将提锂槽进行分段或分区。以递减式恒流电解为例，分段后每一段内的提锂槽内的提锂电极的工作电流相同，沿溶液流动方向，相邻段之间的提锂电极的工作电流依次减小。无论以何种方式，第一个提锂槽内的工作电流是根据待提锂溶液的初始浓度决定的，浓度越大，初始的电流值就越大，提锂槽的设置数量及工作电流变化的幅度需要根据实际的提锂目标和效果进行调整，以使得最后一个提锂槽内的溶液中的锂离子浓度降低到目标要求以下，因此，本公开关键在于保持提锂电极的工作电流沿溶液流动方向整体下降的趋势。相似地，递减式恒压电解中的工作电压的变化，也可进行分段式递减。
在一个实施例中，所述递减式恒压电解提锂中的各个提锂电极为串联式电连接。
第二方面，本公开提供一种如第一方面所述的提锂脱嵌槽用于提锂的应用，所述提锂脱嵌槽用于提锂的应用包括：沿待提锂溶液的流动方向，将阴极主槽分为前段及后段，所述前段中的提锂槽进行所述递减式恒流电解提锂，所述后段中的提锂槽进行所述递减式恒压提锂。
本公开的提锂槽从前往后(即阴极主槽进液口到出液口的方向)优选设置为从高到低的不同恒流或前段恒流后段恒压的工作方式。相较于相关技术中对一个电极先恒流再恒压，或进行分段式恒流的供电方式，所述应用更加灵活且节省能源，避免了对电极进行变换供电方式的繁琐操作。
在一个实施例中，所述前段中的提锂槽的数量与所述后段中的提锂槽的数量之比大于等于2，例如2、3、4、5、6、7或8等，但并不仅限于所列举的数值，上述数值范围内其他未列举的数值同样适用。
作为本公开可选的技术方案，所述待提锂溶液包括卤水。
在一个实施例中，所述卤水中锂离子的浓度为0.2～0.8g/L，例如0.2g/L、0.25g/L、0.3g/L、0.35g/L、0.4g/L、0.45g/L、0.5g/L、0.55g/L、0.6g/L、0.65g/L、0.7g/L、0.75g/L或0.8g/L等，但并不仅限于所列举的数值，上述数值范围内其他未列举的数值同样适用。
在一个实施例中，所述待提锂溶液的流量为1～5L/h，例如1L/h、1.5L/h、2L/h、2.5L/h、3L/h、3.5L/h、4L/h、4.5L/h或5L/h等，但并不仅限于所列举的数值，上述数值范围内其他未列举的数值同样适用。
在一个实施例中，所述热气的温度为35～40℃，例如35℃、36℃、37℃、38℃、39℃或40℃等，但并不仅限于所列举的数值，上述数值范围内其他未列举的数值同样适用。
在一个实施例中，所述热气包括空气和/或惰性气体。
在一个实施例中，所述热气与待提锂溶液的流量比为1:(1～2)，例如1:1、1:1.1、1:1.2、1:1.3、1:1.4、1:1.5、1:1.6、1:1.7、1:1.8、1:1.9或1:2等，但并不仅限于所列举的数值，上述数值范围内其他未列举的数值同样适用。
在一个实施例中，所述应用还包括，由第1个提锂槽同时通入待提锂溶液与热气时，向阳极主槽内通入纯水和/或氯化钠溶液。
当阳极主槽中也设置有隔板时，从第1个脱嵌槽的进液口通入纯水和/或氯化钠溶液。
作为本公开可选的技术方案，在电解提锂的过程中，监测提锂槽中提锂电极的电流和/或电压，当超过预设值时，更换对应的提锂电极。
本公开至少具有以下有益效果：
(1)本公开所述提锂脱嵌槽通过采用“流水线”方式设置多个提锂槽相连， 使提锂槽中待提锂溶液“折流式”流动且锂离子浓度由高到低分布，从而根据每个提锂槽中不同的锂离子浓度来对对应设置提锂电极的锂离子筛材料，合理配置资源，从而在高效提锂的同时降低成本；
(2)本公开所述提锂脱嵌槽用于提锂的应用在提锂电极匹配不同的工作电流和/或电压，进行递减式恒流电解提锂，或前段进行递减式恒流电解提锂，后段进行递减式恒压电解提锂，相较于相关技术中对一个电极进行先恒流再恒压或对一个电极进行分段式恒流供电方式，本方案的设置更灵活，而且避免了对电极进行变换供电方式的繁琐操作；
(3)本公开所述提锂脱嵌槽用于提锂的应用在通入新鲜待提锂溶液的过程中也一并通入热的气体，搭配“折流式”的流动方式，使待提锂溶液的流动充分，提高溶液的传质效果，有效提高了电解槽的提锂效率。
在阅读并理解了附图和详细描述后，可以明白其他方面。
附图说明
附图用来提供对本文技术方案的进一步理解，并且构成说明书的一部分，与本申请的实施例一起用于解释本文的技术方案，并不构成对本文技术方案的限制。
图1是实施例1的提锂脱嵌槽中的阴极主槽的示意图；
图2是实施例2的提锂脱嵌槽中的阴极主槽的示意图；
图3是实施例1及实施例2的提锂脱嵌槽的俯视示意图；
图4是实施例4的提锂脱嵌槽的俯视示意图；
图中：1-阴极主槽、11-进液口、12-出液口、2-隔板、21-开孔、3-隔膜、4-提锂电极、5-脱嵌电极、6-待提锂溶液、7-外部电源、8-阳极主槽。
具体实施方式
下面结合附图并通过具体实施方式来进一步说明本公开的技术方案。本领域技术人员应该明了，所述实施例仅仅是帮助理解本公开，不应视为对本公开的具体限制。
实施例1
本实施例提供了一种提锂脱嵌槽及其应用，如图1及图3所示：
所述提锂脱嵌槽包括阴极主槽1、阳极主槽8，以及使在阴极主槽1及阳极主槽8之间的隔膜3；所述阴极主槽1内设置有隔板2，所述隔板2将所述阴极主槽1划分为15个依次连通的提锂槽；所述阳极主槽8内也设置有隔板2，所述隔板2将所述阳极主槽8划分为与提锂槽相对应的15个依次连通的脱嵌槽；第一个提锂槽及第一个脱嵌槽均设置有进液口11，最后一个提锂槽及最后一个脱嵌槽均设置有出液口12；
所述提锂槽中设置有提锂电极4，所述提锂电极4之间并联式电连接；所述脱嵌槽中设置有脱嵌电极5，所述脱嵌电极5之间并联式电连接，所述提锂电极4与所述脱嵌电极5通过外部电源7电性相连；
所述隔板2上设置有开孔21，相邻两个隔板2之间的开孔21沿所述提锂槽或脱嵌槽的高度方向上下交错排列，第1个隔板2的开孔21设置于距离隔板2顶部10cm的位置，为半径5cm的圆形，第2个隔板2的开孔21设置于距离隔板2底部10cm的位置，为半径5cm的圆形，第3个隔板2的开孔21同第1个隔板2，以此类推共设置15个隔板2，使待提锂溶液6在所述阴极主槽1及阳极主槽8内折流式流动；
沿待提锂溶液6的流动方向，根据提锂槽中的锂离子浓度的变化将所述提锂槽分为5个高浓度槽、5个中浓度槽及5个低浓度槽；所述高浓度槽中的提锂电极4的锂离子筛材料为吸附量高且选择性较好的LiMn2O4；所述中浓度槽 中的提锂电极4的锂离子筛材料为化学稳定性较好，离子扩散系数相对较低，容量高的磷酸铁锂；所述低浓度槽中的提锂电极4的锂离子筛材料为扩散系数高，稳定性好，但容量较低的Li2TiO3；
每个所述提锂槽中安装有电压监测器，用于监控对应的提锂电极4；所述电压监测器电性连接于主机，所述主机用于分析、存储并显示所述提锂电极4的工作状态及更换信息。
本实施例中所述提锂脱嵌槽的应用包括如下步骤：
由第1个提锂槽同时通入待提锂溶液6与热气，并在所述阴极主槽1内折流式流动，同时由第1个脱嵌槽通入纯水，并在所述阳极主槽8内折流式流动，所述待提锂溶液6为锂离子浓度为0.5g/L的卤水，卤水的流量为3L/h，所述热气为温度为37℃，流量为4.5L/h的热空气；
按表1设置提锂电极4的工作电流，其中第1个提锂槽中的提锂电极4为第1个提锂电极4，其工作电流记为A1，第2个提锂槽沿靠近阳极区的方向紧邻所述第1个提锂槽，其工作电流记为A2，A1＞A2，以此类推，进行递减式恒流电解提锂；
表1
当某个提锂槽中的提锂电极4的实时工作电压超过设定的安全定压0.8V 时，电压监测器发出警报，对应更换新的提锂电极4，直至完成电解提锂。
实施例2
本实施例提供了一种提锂脱嵌槽及其应用，如图2及图3所示：
所述提锂脱嵌槽包括阴极主槽1、阳极主槽8，以及使在阴极主槽1及阳极主槽8之间的隔膜3；所述阴极主槽1内设置有隔板2，所述隔板2将所述阴极主槽1划分为15个依次连通的提锂槽；所述阳极主槽8内也设置有隔板2，所述隔板2将所述阳极主槽8划分为与提锂槽相对应的15个依次连通的脱嵌槽；所述提锂槽中设置有提锂电极4，所述脱嵌槽中设置有脱嵌电极5，所述提锂电极4与所述脱嵌电极5通过外部电源7电性相连；第一个提锂槽及第一个脱嵌槽均设置有进液口11，最后一个提锂槽及最后一个脱嵌槽均设置有出液口12；
所述隔板2上设置有开孔21，相邻两个隔板2之间的开孔21沿所述提锂槽或脱嵌槽的高度方向上下交错排列，第1个隔板2的开孔21设置于距离隔板2顶部10cm的位置，为半径5cm的圆形，第2个隔板2的开孔21设置于距离隔板2底部10cm的位置，为半径5cm的圆形，第3个隔板2的开孔21同第1个隔板2，以此类推共设置15个隔板2，使待提锂溶液6在所述阴极主槽1及阳极主槽8内折流式流动；
沿待提锂溶液6的流动方向，根据提锂槽中的锂离子浓度的变化将所述提锂槽分为5个高浓度槽、5个中浓度槽及5个低浓度槽；所述高浓度槽中的提锂电极4的锂离子筛材料为吸附量高且选择性较好的LiMn2O4；所述中浓度槽中的提锂电极4的锂离子筛材料为化学稳定性较好，离子扩散系数相对较低，容量高的磷酸铁锂；所述低浓度槽中的提锂电极4的锂离子筛材料为扩散系数高，稳定性好，但容量较低的Li2TiO3；
沿待提锂溶液6的流动方向，第1个提锂槽中的提锂电极4为第1个提锂电极4，第2个提锂槽中的提锂电极4为第2个提锂电极4，以此类推；同时将阴极主槽1分为前段及后段，前段包含第1个提锂电极4到第10个提锂电极4，后段包含第11个提锂电极4到第15个提锂电极4；前段中的提锂电极4为并联式电连接，后段中的提锂电极4为串联式电连接；
每个所述提锂槽中安装有电压监测器，用于监控对应的提锂电极4；所述电压监测器电性连接于主机，所述主机用于分析、存储并显示所述提锂电极4的工作状态及更换信息。
本实施例中所述提锂脱嵌槽的应用包括如下步骤：
由第1个提锂槽同时通入待提锂溶液6与热气，并在所述阴极主槽1内折流式流动，同时由第1个脱嵌槽通入氯化钠溶液，并在所述阳极主槽8内折流式流动，所述待提锂溶液6为锂离子浓度为0.5g/L的卤水，卤水的流量为3L/h，所述热气为温度为40℃，流量为6L/h的热空气；
按表2设置提锂电极4的工作电流及工作电压，其中第1个提锂电极4的工作电流记为A1，第2个提锂电极4的工作电流记为A2，A1＞A2，以此类推，第11个提锂电极4的工作电压记为V1，第12个提锂电极4的工作电压记为V2、以此类推；使前段中的提锂槽进行所述递减式恒流电解提锂，所述后段中的提锂槽进行所述递减式恒压提锂；
表2

当某个提锂槽中的提锂电极4的实时工作电压超过设定的安全定压0.8V时，电压监测器发出警报，对应更换新的提锂电极4，直至完成电解提锂。
实施例3
本实施例提供了一种提锂脱嵌槽及其应用，所述提锂脱嵌槽与实施例1完全相同，所述用于与实施例1的区别为：
按表3设置提锂电极4的工作电压，其中第1个提锂槽中的提锂电极4为第1个提锂电极4，其工作电压记为V1，第2个提锂槽中的提锂电极4为第2个提锂电极4，其工作电压记为V2，V1＞V2，以此类推，进行递减式恒压电解提锂；
表3
除以上外，其他条件与实施例1完全相同。
实施例4
本实施例提供了一种提锂脱嵌槽及其应用，如图4所示，所述提锂脱嵌槽的阳极主槽8中不设置隔板2，除此之外，其他条件与实施例1完全相同。
对比例1
本对比例提供了一种提锂脱嵌槽及其用于，所述提锂脱嵌槽与实施例1完全相同，所述应用与实施例1的区别为：将所有提锂电极4的工作电流设置为25A，其他条件与实施例1完全相同。
对比例2
本对比例提供了一种提锂脱嵌槽及其应用，所述提锂脱嵌槽与实施例1完全相同，所述应用与实施例1的区别为：将所有提锂电极4的工作电流设置为1A，其他条件与实施例1完全相同。
对比例3
本对比例提供了一种提锂脱嵌槽及其用于，所述提锂脱嵌槽与实施例1的区别为：将所有隔板2的开孔21统一设置为靠近隔板2底部10cm的位置，为半径5cm的圆形，不使待提锂溶液6进行折流式流动，除此之外，所述提锂脱嵌槽其他条件及应用参数与实施例1完全相同。
对比例4
本对比例提供了一种提锂脱嵌槽及其应用，所述提锂脱嵌槽与实施例1的区别为：将所有提锂电极4的锂离子筛材料均设置为LiMn2O4，除此之外，所述提锂脱嵌槽其他条件及应用参数与实施例1完全相同。
对比例5
本对比例提供了一种提锂脱嵌槽及其用于，所述提锂脱嵌槽与实施例1的区别为：将所有提锂电极4的锂离子筛材料均设置为Li2TiO3，除此之外，所述提锂脱嵌槽其他条件及应用参数与实施例1完全相同。
对比例6
本对比例提供了一种提锂脱嵌槽及其应用，所述提锂脱嵌槽与实施例1的区别为：不使用热气，仅通入待提锂溶液6，除此之外，所述提锂脱嵌槽其他条件及应用参数与实施例1完全相同。
在通入相同量的卤水提锂完成后，测试实施例及对比例溶液中最后一个提锂槽中剩余的锂离子浓度，计算提锂率，结果如表4所示。
表4
由表1可以看出：
由实施例1-3的剩余锂离子浓度可看出，本方案电解槽的供电方式优选为不同恒流段供电，实施例1相较于实施例4可看出，阳极有无隔板对本方案的结果无影响；实施例1相较于对比例1，对比例1的供电方法为持续高电流，电极板容易超过安全电压，影响提锂，耗能和成本都会较高；对比例2为低电流，提锂效率极低；对比例3开口都在底部会造成提锂槽中的卤水流动过快，无法正常提锂；实施例1相较于对比例4-5，在低浓度采用容量较高的锂离子筛会影响提锂效率，而在高浓度卤水中采用容量较低的锂离子筛则会增加更换锂离子筛的次数，操作繁琐；相较于对比例6，通入了热气提高提锂环境的温度，能更好地提高提锂效率。

Claims (17)

  1. 一种提锂脱嵌槽，包括：
    阳极主槽，所述阳极主槽内设置有脱嵌电极；
    阴极主槽，所述阴极主槽内设置有隔板，所述隔板将所述阴极主槽划分为至少两个提锂槽；所述隔板上设置有开孔，相邻两个隔板之间的开孔沿所述提锂槽的高度方向上下交错排列，使待提锂溶液在所述阴极主槽内折流式流动；所述提锂槽中设置有提锂电极，所述提锂电极的数量与所述脱嵌电极的数量相对应；所述提锂电极与所述脱嵌电极通过外部电源电性相连；
    隔膜，设置在所述阳极主槽与所述阴极主槽之间。
  2. 根据权利要求1所述的提锂脱嵌槽，其中，所述阳极主槽内设置有所述隔板，将所述阳极主槽划分为与每个所述提锂槽相对应的脱嵌槽，所述脱嵌槽内的脱嵌电极的数量与对应的提锂槽内的提锂电极的数量相同；
    可选地，第一个提锂槽及第一个脱嵌槽均设置有进液口，最后一个提锂槽及最后一个脱嵌槽均设置有出液口；
    可选地，所述提锂槽的数量为10～20个。
  3. 根据权利要求1或2所述的提锂脱嵌槽，其中，根据所述阴极主槽内的所述待提锂溶液中的锂离子浓度的变化，将所述提锂槽分为高浓度槽、中浓度槽及低浓度槽。
  4. 根据权利要求3所述的提锂脱嵌槽，其中，所述高浓度槽中锂离子的浓度大于0.1g/L；所述中浓度槽中锂离子的浓度为0.01～0.1g/L；所述低浓度槽中锂离子的浓度小于0.01g/L。
  5. 根据权利要求3或4所述的提锂脱嵌槽，其中，所述高浓度槽的数量为2～8个；所述中浓度槽的数量为1～9个；所述低浓度槽的数量为1～9个。
  6. 根据权利要求3-5任一项所述的提锂脱嵌槽，其中，所述高浓度槽中设 置有第一锂离子筛材料、所述中浓度槽中设置有第二锂离子筛材料、所述低浓度槽中设置有第三锂离子筛材料；
    按每单位质量的吸附容量比较，所述第一锂离子筛材料＞所述第二锂离子筛材料＞所述第三锂离子筛材料；
    按每单位质量的离子扩散系数比较，所述第一锂离子筛材料＜所述第二锂离子筛材料＜所述第三锂离子筛材料；
    可选地，所述第一锂离子筛材料的吸附容量为35～38mg/g；所述第二锂离子筛材料的吸附容量为30～33mg/g；所述第三锂离子筛材料的吸附容量为12～15mg/g；
    可选地，所述第一锂离子筛材料的离子扩散系数为10-10～10-11cm2/s；所述第二锂离子筛材料的离子扩散系数为10-9～10-10cm2/s；所述第三锂离子筛材料的离子扩散系数为10-7～10-8cm2/s。
  7. 根据权利要求6所述的提锂脱嵌槽，其中，所述第一锂离子筛材料、所述第二锂离子筛材料及所述第三锂离子筛材料为物理吸附材料或电化学吸附材料；
    可选地，当所述第一锂离子筛材料、所述第二锂离子筛材料及所述第三锂离子筛材料为电化学吸附材料时，所述第一锂离子筛材料、所述第二锂离子筛材料及所述第三锂离子筛材料分别设置于对应的提锂槽中的提锂电极上。
  8. 根据权利要求7所述的提锂脱嵌槽，其中，当所述第一锂离子筛材料、所述第二锂离子筛材料及所述第三锂离子筛材料为物理吸附材料时：
    所述第一锂离子筛材料包括二氧化锰吸附剂；所述第二锂离子筛材料包括硅酸锂吸附剂；所述第三锂离子筛材料包括氢氧化铝基吸附剂。
  9. 根据权利要求7所述的提锂脱嵌槽，其中，当所述第一锂离子筛材料、 所述第二锂离子筛材料及所述第三锂离子筛材料为电化学吸附材料时：
    所述第一锂离子筛材料包括锰氧化物锂离子筛；所述第二锂离子筛材料包括钴酸锂、钒酸锂或磷酸铁锂中的任一种或至少两种的组合；所述第三锂离子筛材料包括钛氧化物锂离子筛；
    可选地，所述锰氧化物锂离子筛包括LiMn2O4、Li1.33Mn1.67O4或Li1.6Mn1.6O4中的至少一种；
    可选地，所述钛氧化物锂离子筛包括Li2TiO3和/或Li4Ti5O12。
  10. 根据权利要求1-9任一项所述的提锂脱嵌槽，其中，每个所述提锂槽中安装有电流和/或电压监测器，用于监控对应的提锂电极；
    可选地，所述电流和/或电压监测器电性连接于主机，所述主机用于分析、存储并显示所述提锂电极的工作状态及更换信息。
  11. 根据权利要求1-10任一项所述的提锂脱嵌槽，其中，所述隔板上的开孔靠近所述隔板的顶端或底端设置；
    可选地，沿所述隔板的高度方向，所述开孔的边缘与所述隔板的顶端或底端的距离占所述隔板的高度的5％～10％；
    可选地，所述开孔的半径为3～8cm。
  12. 一种用权利要求1-11任一项所述的提锂脱嵌槽提锂的应用，包括如下步骤：
    由第1个提锂槽同时通入待提锂溶液与热气，并在所述阴极主槽内折流式流动，进行递减式恒流电解提锂和/或递减式恒压电解提锂。
  13. 根据权利要求12所述的应用，其中，所述递减式恒流电解提锂包括，在电解提锂的过程中，提锂槽内的提锂电极自身的工作电流保持不变，沿待提锂溶液的流动方向，提锂电极的工作电流依次减小或分段式依次减小；
    可选地，在所述递减式恒流电解提锂中，相邻两个提锂电极的工作电流的差值为0.5～7A；
    可选地，所述递减式恒流电解提锂中的各个提锂电极为并联式电连接。
  14. 根据权利要求12或13所述的应用，其中，所述递减式恒压电解提锂包括，在电解提锂的过程中，提锂槽内的提锂电极自身的工作电压保持不变，沿待提锂溶液的流动方向，提锂电极的工作电压依次减小或分段式依次减小；
    可选地，在所述递减式恒压电解提锂中，相邻两个提锂电极的工作电压的差值为0.05～0.15V；
    可选地，所述递减式恒压电解提锂中的各个提锂电极为串联式电连接。
  15. 根据权利要求12-14任一项所述的应用，其中，沿待提锂溶液的流动方向，将阴极主槽分为前段及后段，对所述前段中的提锂槽进行所述递减式恒流电解提锂，对所述后段中的提锂槽进行所述递减式恒压提锂；
    可选地，所述前段中的提锂槽的数量与所述后段中的提锂槽的数量之比大于等于2。
  16. 根据权利要求12-15任一项所述的应用，其中，所述待提锂溶液包括卤水；
    可选地，所述卤水中锂离子的浓度为0.2～0.8g/L；
    可选地，所述待提锂溶液的流量为1～5L/h；
    可选地，所述热气的温度为35～40℃；
    可选地，所述热气包括空气和/或惰性气体；
    可选地，所述热气与待提锂溶液的流量比为1:(1～2)；
    可选地，所述应用还包括，由第1个提锂槽同时通入待提锂溶液与热气时，向阳极主槽内通入纯水和/或氯化钠溶液。
  17. 根据权利要求12-16任一项所述的应用，其中，在电解提锂的过程中，监测提锂槽中提锂电极的电流和/或电压，当超过预设值时，更换对应的提锂电极。
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