CN116119741B - Preparation method of nickel-cobalt-manganese ternary positive electrode material precursor - Google Patents

Preparation method of nickel-cobalt-manganese ternary positive electrode material precursor Download PDF

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CN116119741B
CN116119741B CN202310127203.6A CN202310127203A CN116119741B CN 116119741 B CN116119741 B CN 116119741B CN 202310127203 A CN202310127203 A CN 202310127203A CN 116119741 B CN116119741 B CN 116119741B
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nickel
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CN116119741A (en
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郭孝东
刘桐李
宋扬
吴振国
万放
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Sichuan University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract

The invention discloses a preparation method of a nickel-cobalt-manganese ternary positive electrode material precursor, and belongs to the technical field of lithium batteries. The preparation method comprises the following steps: 1) Respectively injecting a mixed solution of nickel, cobalt and manganese salt and a continuous phase solution into a micro-channel reactor T1 to obtain a mixed material; 2) Respectively injecting the mixed material and the precipitant solution into a micro-channel reactor T2 for mixing reaction; 3) Sequentially separating an organic phase solution and a water phase in the mixed feed liquid containing the precursor to obtain a solid material, and drying the solid material to obtain a nickel-cobalt-manganese ternary positive electrode material precursor; the micro-channel reactor T1 and the micro-channel reactor T2 both comprise two feeding channels and one discharging channel with equal sizes, and the two feeding channels are intersected with each other at an included angle of 90 degrees and are intersected with the reaction channel. The method provided by the invention does not need to add complexing agents, and is short in time consumption, so that the production cost is greatly saved.

Description

Preparation method of nickel-cobalt-manganese ternary positive electrode material precursor
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a preparation method of a nickel-cobalt-manganese ternary positive electrode material precursor.
Background
With the continuous development of new energy automobiles to green and low carbon, the requirements on batteries are also higher and higher. The lithium nickel cobalt manganese oxide ternary lithium battery has been widely studied due to its incomparable advantages such as high energy density and power density, superior cycle performance, etc. Commercial power cells are evolving into ternary lithium cells as the main stream. The manufacturing of the ternary lithium battery anode material in the prior art disclosed at present is mainly manufactured by a two-step method: the precursor is obtained first and then calcined to obtain the positive electrode material.
At present, a coprecipitation method is generally adopted in the precursor production process, a salt solution and a precipitant solution are continuously dropwise added into a continuously stirred reaction kettle, and in order to uniformly coprecipitate a plurality of elements, a complexing agent is often added to slow down the precipitation speed. However, this method is time consuming and requires the addition of complexing agents.
Disclosure of Invention
The invention aims to provide a preparation method of a nickel-cobalt-manganese ternary positive electrode material precursor, which does not need to add a complexing agent, is short in time consumption and greatly saves production cost.
In order to achieve the above purpose, the invention provides a preparation method of a nickel-cobalt-manganese ternary positive electrode material precursor, which comprises the following steps:
1) Respectively injecting a mixed solution of nickel, cobalt and manganese salt and a continuous phase solution into a micro-channel reactor T1 to obtain a mixed material;
2) Respectively injecting the mixed material and the precipitant solution into a micro-channel reactor T2 for mixing reaction to obtain mixed feed liquid containing a precursor;
3) Sequentially separating an organic phase solution and a water phase in the mixed feed liquid containing the precursor to obtain a solid material, and drying the solid material to obtain a nickel-cobalt-manganese ternary positive electrode material precursor;
the micro-channel reactor T1 and the micro-channel reactor T2 both comprise two feeding channels and one discharging channel with equal sizes, the two feeding channels are intersected at an included angle of 90 degrees and are intersected with the reaction channel, and two different materials in the steps 1) and 2) are respectively injected from the two feeding channels.
Preferably, the discharge port of the microchannel reactor T1 is connected with the first capillary, and the discharge port of the first capillary is connected with the feed port of the microchannel reactor T2; and a discharge port of the microchannel reactor T2 is connected with a second capillary.
Preferably, the lengths of the feeding channel and the discharging channel of the micro-channel reactor T1 and the micro-channel reactor T2 are 1-100 mm, and the inner diameters are 0.1-2.5 mm.
Preferably, the lengths of the first capillary tube and the second capillary tube are respectively 100-10000 mm, and the inner diameters are respectively 0.1-2.5 mm.
Preferably, the injection speed of the mixed solution of nickel, cobalt and manganese salt in the step 1) is 0.1-5 ml/min, and the injection speed of the continuous phase solution is 0.2-10 ml/min.
Preferably, the injection rate of the precipitant solution in step 2) is 0.1-5 ml/min, and is the same as the injection rate of the mixed solution of nickel, cobalt, manganese salts.
Preferably, the temperatures of the materials in the micro-channel reactor T1, the micro-channel reactor T2 and the capillary tube are controlled between 25 ℃ and 95 ℃.
Preferably, the total cation concentration in the mixed solution of the nickel, cobalt and manganese salt is 0.1-3.0 mol/L; the concentration of anions in the precipitant solution is 0.1-6.0 mol/L; the boiling point of the continuous phase solution is 100-180 ℃, and the solubility in water is 0-15% in percentage by weight.
Preferably, the nickel element in the mixed solution of the nickel, cobalt and manganese salt is selected from one or more of nickel sulfate, nickel chloride, nickel nitrate and nickel acetate; the cobalt element is one or more selected from cobalt sulfate, cobalt chloride, cobalt nitrate and cobalt acetate; the manganese element is selected from one or more of manganese sulfate, manganese chloride, manganese nitrate and manganese acetate; and based on 1 total mole part, nickel: cobalt element: the proportion of manganese element is 0.4-0.95: 0 to 0.4:0 to 0.75.
Preferably, the precipitant solution comprises one or more of sodium carbonate, sodium bicarbonate, ammonium carbonate, ammonium bicarbonate, sodium hydroxide, potassium hydroxide, sodium oxalate, and ammonium oxalate; the molar concentration of the precipitant is 0.1-6 mol/L.
The invention has the following beneficial technical effects:
the invention greatly improves the mixing efficiency of the mixed solution of nickel, cobalt and manganese salts and the precipitant solution by forcing microscopic mixing through the microchannel reactor, and is favorable for uniform precipitation of various elements on an atomic layer. The reaction of cations in the mixed solution of nickel, cobalt and manganese salts and the anions of the precipitant belongs to quick reaction, and the reaction time is very short. If the mixing efficiency of the mixed solution of nickel, cobalt and manganese salt and the precipitant solution is low, the mixing time is long, and the mixing time of the two solutions is longer than the reaction time, element segregation is easy to occur, and the element distribution in the precursor is uneven. The conventional method selects addition of complexing agents to slow down the precipitation reaction to obtain uniform element distribution, which allows the reaction time to be prolonged to tens of hours. Therefore, the method rapidly prepares the precursor of the anode material of the lithium ion battery with uniform atomic layer element distribution under the condition of no complexing agent addition by a forced mixing feeding mode of the microchannel reactor, and solves the problem of long production time of the precursor of the anode material of the lithium ion battery.
Drawings
FIG. 1 is a schematic structural diagram of a microchannel reactor T1, wherein 1 is a mixed solution of nickel, cobalt and manganese salts, 2 is a continuous phase solution, 3 is a discharge channel, and 4 is a first capillary;
FIG. 2 is a process flow diagram of the preparation of a nickel-cobalt-manganese ternary cathode material precursor according to the present invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a preparation method of a nickel-cobalt-manganese ternary positive electrode material precursor, which comprises the following steps:
1) Respectively injecting a mixed solution of nickel, cobalt and manganese salt and a continuous phase solution into a micro-channel reactor T1 to obtain a mixed material;
2) Respectively injecting the mixed material and the precipitant solution into a micro-channel reactor T2 for mixing reaction to obtain mixed feed liquid containing a precursor;
3) Sequentially separating an organic phase solution and a water phase in the mixed feed liquid containing the precursor to obtain a solid material, and drying the solid material to obtain a nickel-cobalt-manganese ternary positive electrode material precursor;
the micro-channel reactor T1 and the micro-channel reactor T2 both comprise two feeding channels and one discharging channel with equal sizes, the two feeding channels are intersected at an included angle of 90 degrees and are intersected with the reaction channel, and two different materials in the steps 1) and 2) are respectively injected from the two feeding channels.
The mixed solution of nickel, cobalt and manganese salt and the continuous phase solution are respectively injected into a micro-channel reactor T1 to obtain a mixed material. In the invention, the total cation concentration in the mixed solution of the nickel, cobalt and manganese salts is preferably 0.1-3.0 mol/L. The nickel element in the mixed solution of the nickel, cobalt and manganese salt is preferably selected from one or more of nickel sulfate, nickel chloride, nickel nitrate and nickel acetate; the cobalt element is preferably one or more selected from cobalt sulfate, cobalt chloride, cobalt nitrate and cobalt acetate; the manganese element is preferably selected from one or more of manganese sulfate, manganese chloride, manganese nitrate and manganese acetate; and based on 1 total mole part, nickel: cobalt element: the proportion of manganese element is 0.4-0.95: 0 to 0.4:0 to 0.75. If the nickel element is 0.8 mole and the cobalt element is 0.1 mole, then the manganese element is 0.1 mole.
In the invention, the boiling point of the continuous phase solution is 100-180 ℃, and the solubility of the continuous phase in water is 0-15% in percentage by weight. In the present invention, the continuous phase is preferably selected from n-octane, isooctane or n-butanol.
In the present invention, the microchannel reactor T1 includes two feed channels and one discharge channel with equal dimensions, and the two feed channels intersect at an included angle of 90 ° and intersect with the reaction channel to form a "T" structure, as shown in fig. 1. The mixed solution of nickel, cobalt and manganese salt and the continuous phase solution are respectively injected into two feed channels of a micro-channel reactor T1, and the flow shape of liquid in the micro-channel reactor is a bullet flow; firstly, mixing a mixed solution of nickel, cobalt and manganese salt with a continuous phase solution, and shearing the mixed solution in the form of an aqueous solution by utilizing the continuous phase solution which is not mutually dissolved with the aqueous solution to form an elastic flow form which takes the continuous phase solution as a continuous phase and takes the mixed solution of nickel, cobalt and manganese salt as a disperse phase.
In the present invention, the outlet of the microchannel reactor T1 is preferably connected to the first capillary, and the outlet of the first capillary is connected to the inlet of the microchannel reactor T2. In the invention, the first capillary tube is connected between the discharge port of the microchannel reactor T1 and the feed port of the microchannel reactor T2, so that the bullet-shaped flow formed by the microchannel reactor T1 can form a stable flow state, and the bullet-shaped flow state can be still maintained after the other solution is added into the microchannel reactor T2, and the bullet-shaped flow form ensures that solid particles generated in the reaction process do not contact with the tube wall and flow out of the reaction system along with the disperse phase, thus having the advantage of being difficult to block the tube.
In the present invention, the lengths of the feed channel and the discharge channel of the microchannel reactor T1 are preferably 1 to 100mm, more preferably 10 to 50mm; the inner diameters are each preferably 0.1 to 2.5mm, more preferably 0.5 to 2mm. The length of the first capillary is preferably 100 to 10000mm, and the inner diameter is preferably 0.1 to 2.5mm, more preferably 0.5 to 2mm. In the present invention, the injection rate of the mixed solution of nickel, cobalt, and manganese salts is preferably 0.1 to 5ml/min, and the injection rate of the continuous phase solution is preferably 0.2 to 10ml/min.
After the mixed material is obtained, the mixed material and the precipitant solution are respectively injected into a micro-channel reactor T2 for mixing reaction, so as to obtain the mixed material liquid containing the precursor. In the present invention, the precipitant solution preferably includes one or more of sodium carbonate, sodium bicarbonate, ammonium carbonate, ammonium bicarbonate, sodium hydroxide, potassium hydroxide, sodium oxalate, ammonium oxalate; the molar concentration of the precipitant is preferably 0.1-6 mol/L. The concentration of anions in the precipitant solution is preferably 0.1 to 6.0mol/L. In the present invention, the injection rate of the precipitant solution is preferably 0.1 to 5ml/min, and is the same as the injection rate of the mixed solution of nickel, cobalt, and manganese salts.
In the present invention, the outlet of the microchannel reactor T2 is preferably connected to a second capillary. In the invention, the reactant can continuously flow and react in the pipeline by connecting the second capillary tube at the discharge port of the microchannel reactor T2. In the present invention, the lengths of the feed channel and the discharge channel of the microchannel reactor T2 are preferably 1 to 100mm, more preferably 10 to 50mm, and the inner diameters are preferably 0.1 to 2.5mm, more preferably 0.5 to 2mm. The length of the second capillary is preferably 100 to 10000mm, and the inner diameter is preferably 0.1 to 2.5mm, more preferably 0.5 to 2mm.
When the mixed material in the micro-channel reactor T1 is transferred into the micro-channel reactor T2 from one feeding channel of the micro-channel reactor T2, the other feeding channel of the micro-channel reactor T2 is fed with the precipitant to form an elastic flow form with the precipitant as a continuous phase and the mixed material as a disperse phase.
In the present invention, the temperatures of the materials in the microchannel reactor T1, the microchannel reactor T2 and the capillaries are preferably controlled to be 25-95 ℃.
After the mixed feed liquid containing the precursor is obtained, the organic phase solution and the water phase in the mixed feed liquid containing the precursor are sequentially separated to obtain a solid material, and the solid material is dried to obtain the nickel-cobalt-manganese ternary positive electrode material precursor. In the invention, the mixed feed liquid containing the precursor forms an organic phase, an aqueous phase and a solid material three-phase, and preferably, the organic phase is separated first, and then the aqueous phase and the solid material are separated in a centrifugal mode. The specific mode of the organic phase separation is not particularly limited, and the separation can be carried out by adopting conventional liquid separation equipment in the field. In the present invention, the drying mode is preferably vacuum drying; the temperature during vacuum drying is preferably 80-120 ℃, the vacuum degree is preferably 0.01-0.1 Mpa, and the time is preferably 8-24 h.
The particle size of the nickel, cobalt and lithium ternary anode material precursor prepared by the method provided by the invention is 50-5000 nm.
The technical solutions provided by the present invention are described in detail below in conjunction with examples for further illustrating the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
The microchannel reactor T1 comprises two feeding channels with the size of 20mm (length) multiplied by 1mm (inner diameter) and a discharging channel with the size of 20mm (length) multiplied by 1mm (inner diameter), wherein the two feeding channels are intersected at an included angle of 90 degrees and are intersected with the reaction channel to form a T-shaped structure, and a capillary with the size of 200mm (length) multiplied by 1mm (inner diameter) is connected with the discharging channel; the microchannel reactor T2 comprises two feed channels with the dimensions of 20mm (length) ×1mm (inner diameter) and a discharge channel with the dimensions of 20mm (length) ×1mm (inner diameter), wherein the two feed channels intersect at an included angle of 90 degrees and intersect in the reaction channel to form a T-shaped structure, and a capillary with the dimensions of 4000mm (length) ×1mm (inner diameter) is connected with the discharge channel.
The preparation method of the mixed solution of the nickel, cobalt and manganese salt is as follows:
31.5417g of nickel sulfate hexahydrate, 11.2441g of cobalt sulfate heptahydrate and 6.7604g of manganese sulfate monohydrate are weighed; 200g of deionized water is added for dissolution, and then the volume is fixed to 1L, so as to obtain a nickel, cobalt and manganese salt mixed solution. The stoichiometric ratio of nickel, cobalt and manganese elements in the solution is as follows: cobalt: manganese=6:2:2.
The continuous phase solution used was n-octane
A0.4 mol/L sodium carbonate solution was prepared as a precipitant solution at room temperature. The flow rate of a reciprocating type advection pump is regulated, a nickel, cobalt and manganese salt mixed solution is injected into a micro-channel reactor T1 at the speed of 0.25ml/min, a continuous phase solution is introduced into the micro-channel reactor T1 from the other inlet at the speed of 0.5ml/min, mixed and flows through a capillary tube, then the mixed solution is injected into a micro-channel reactor T2 from one feed inlet of the micro-channel reactor T2, and a precipitant solution enters from the other feed inlet of the micro-channel reactor T2 at the speed of 0.25 ml/min. Controlling the reaction temperature at 50 ℃ for 180 seconds to obtain suspension containing a precursor of the positive electrode material of the lithium ion battery, separating and recovering an upper organic phase solution through liquid-liquid separation, centrifuging (the rotating speed is 8000r/min, the time is 120 seconds) to separate a water phase solid-liquid mixture, and vacuum drying the solid material at 0.08mpa and 110 ℃ for 10 hours to obtain precursor particles of the positive electrode material of the nickel, cobalt and manganese ternary lithium ion battery, wherein the particle size is about 3 mu m.
Example 2
The microchannel reactor T1 comprises two feeding channels with the size of 20mm (length) multiplied by 1mm (inner diameter) and a discharging channel with the size of 20mm (length) multiplied by 1mm (inner diameter), wherein the two feeding channels are intersected at an included angle of 90 degrees and are intersected with the reaction channel to form a T-shaped structure, and a capillary with the size of 200mm (length) multiplied by 1mm (inner diameter) is connected with the discharging channel; the microchannel reactor T2 comprises two feed channels with the dimensions of 20mm (length) ×1mm (inner diameter) and a discharge channel with the dimensions of 20mm (length) ×1mm (inner diameter), wherein the two feed channels intersect at an included angle of 90 degrees and intersect in the reaction channel to form a T-shaped structure, and a capillary with the dimensions of 4000mm (length) ×1mm (inner diameter) is connected with the discharge channel.
The preparation method of the mixed solution of the nickel, cobalt and manganese salt is as follows:
31.5417g of nickel sulfate hexahydrate, 11.2441g of cobalt sulfate heptahydrate and 6.7604g of manganese sulfate monohydrate are weighed; 200g of deionized water is added for dissolution, and then the volume is fixed to 1L, so as to obtain a nickel, cobalt and manganese salt mixed solution. The stoichiometric ratio of nickel, cobalt and manganese elements in the solution is as follows: cobalt: manganese=6:2:2.
The continuous phase solution used was n-octane
A0.2 mol/L sodium oxalate solution was prepared as a precipitant solution at room temperature. The flow rate of a reciprocating type advection pump is regulated, a nickel, cobalt and manganese salt mixed solution is injected into a micro-channel reactor T1 at the speed of 0.25ml/min, a continuous phase solution is introduced into the micro-channel reactor T1 from the other inlet at the speed of 0.5ml/min, mixed and flows through a capillary tube, then the mixed solution is injected into a micro-channel reactor T2 from one feed inlet of the micro-channel reactor T2, and a precipitant solution enters from the other feed inlet of the micro-channel reactor T2 at the speed of 0.25 ml/min. Controlling the reaction temperature at 90 ℃ for 180 seconds to obtain suspension containing a precursor of the positive electrode material of the lithium ion battery, separating and recovering an upper organic phase solution through liquid-liquid separation, centrifuging (the rotating speed is 8000r/min, the time is 120 seconds) to separate a water phase solid-liquid mixture, and vacuum drying the solid material at 0.08mpa and 110 ℃ for 10 hours to obtain precursor particles of the positive electrode material of the nickel, cobalt and manganese ternary lithium ion battery, wherein the particle size is about 5 mu m.
Example 3
The microchannel reactor T1 comprises two feeding channels with the size of 20mm (length) ×1.5mm (inner diameter) and a discharging channel with the size of 20mm (length) ×1.5mm (inner diameter), wherein the two feeding channels intersect at an included angle of 90 degrees and are intersected with the reaction channel to form a T-shaped structure, and a capillary with the size of 200mm (length) ×1.5mm (inner diameter) is connected with the discharging channel; the microchannel reactor T2 comprises two feed channels with the dimensions of 20mm (length) ×1.5mm (inner diameter) and a discharge channel with the dimensions of 20mm (length) ×1.5mm (inner diameter), wherein the two feed channels intersect at an included angle of 90 DEG and meet in the reaction channel to form a T-shaped structure, and a capillary with the dimensions of 8000mm (length) ×1.5mm (inner diameter) is connected with the discharge channel.
The preparation method of the mixed solution of the nickel, cobalt and manganese salt is as follows:
39.8149g of nickel acetate tetrahydrate, 4.9816g of cobalt acetate tetrahydrate and 4.9018g of manganese acetate tetrahydrate are weighed; 200g of deionized water is added for dissolution, and then the volume is fixed to 1L, so as to obtain a nickel, cobalt and manganese salt mixed solution. The stoichiometric ratio of nickel, cobalt and manganese elements in the solution is as follows: cobalt: manganese=8:1:1.
The continuous phase solution used was n-octane
An oxalic acid solution of 0.2mol/L was prepared as a precipitant solution at room temperature. The flow rate of a reciprocating type advection pump is regulated, a nickel, cobalt and manganese salt mixed solution is injected into a micro-channel reactor T1 at 0.5ml/min, a continuous phase solution is introduced into the micro-channel reactor T1 from the other inlet at 1ml/min, mixed and flows through a capillary tube, then is injected into the micro-channel reactor T2 from one feed inlet of the micro-channel reactor T2, and a precipitant solution enters from the other feed inlet of the micro-channel reactor T2 at 0.5 ml/min. Controlling the reaction temperature at 90 ℃, obtaining suspension containing a precursor of the positive electrode material of the lithium ion battery after 424 seconds, separating and recovering the upper organic phase solution through liquid-liquid separation, centrifuging (the rotating speed is 8000r/min, the time is 120 seconds) to separate the aqueous phase solid-liquid mixture, and vacuum drying the solid material at 0.08Mpa and 110 ℃ for 10 hours to obtain precursor particles of the positive electrode material of the nickel, cobalt and manganese ternary lithium ion battery, wherein the particle size is about 0.5 mu m.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.

Claims (10)

1. A preparation method of a nickel-cobalt-manganese ternary positive electrode material precursor is characterized by comprising the following steps of: the method comprises the following steps:
1) Respectively injecting a mixed solution of nickel, cobalt and manganese salt and a continuous phase solution into a micro-channel reactor T1 to obtain a mixed material; the boiling point of the continuous phase solution is 100-180 ℃, and the solubility in water is 0-15% in percentage by weight;
2) Respectively injecting the mixed material and the precipitant solution into a micro-channel reactor T2 for mixing reaction to obtain mixed feed liquid containing a precursor;
3) Sequentially separating an organic phase solution and a water phase in the mixed feed liquid containing the precursor to obtain a solid material, and drying the solid material to obtain a nickel-cobalt-manganese ternary positive electrode material precursor;
the micro-channel reactor T1 and the micro-channel reactor T2 both comprise two feeding channels and one discharging channel with equal sizes, the two feeding channels are intersected at an included angle of 90 degrees and are intersected with the reaction channel, and two different materials in the steps 1) and 2) are respectively injected from the two feeding channels.
2. The preparation method according to claim 1, wherein the discharge port of the microchannel reactor T1 is connected with the first capillary, and the discharge port of the first capillary is connected with the feed port of the microchannel reactor T2; and a discharge port of the microchannel reactor T2 is connected with a second capillary.
3. The preparation method according to claim 1, wherein the lengths of the feed channel and the discharge channel of the microchannel reactor T1 and the microchannel reactor T2 are 1-100 mm, and the inner diameters are 0.1-2.5 mm.
4. The method according to claim 2, wherein the lengths of the first capillary and the second capillary are respectively 100 to 10000mm, and the inner diameters thereof are respectively 0.1 to 2.5mm.
5. The preparation method according to claim 1, wherein the injection rate of the mixed solution of nickel, cobalt and manganese salt in step 1) is 0.1 to 5ml/min, and the injection rate of the continuous phase solution is 0.2 to 10ml/min.
6. The preparation method according to claim 1, wherein the injection rate of the precipitant solution in step 2) is 0.1-5 ml/min and is the same as the injection rate of the mixed solution of nickel, cobalt, manganese salts.
7. The preparation method according to claim 1, wherein the temperatures of the materials in the microchannel reactor T1, the microchannel reactor T2 and the capillaries are controlled to be 25-95 ℃.
8. The preparation method according to claim 1, wherein the total cation concentration in the mixed solution of nickel, cobalt and manganese salt is 0.1-3.0 mol/L; the concentration of anions in the precipitant solution is 0.1-6.0 mol/L.
9. The preparation method according to claim 1, wherein the nickel element in the mixed solution of nickel, cobalt and manganese salt is selected from one or more of nickel sulfate, nickel chloride, nickel nitrate and nickel acetate; the cobalt element is one or more selected from cobalt sulfate, cobalt chloride, cobalt nitrate and cobalt acetate; the manganese element is selected from one or more of manganese sulfate, manganese chloride, manganese nitrate and manganese acetate; and based on 1 total mole part, nickel: cobalt element: the proportion of manganese element is 0.4-0.95: 0 to 0.4:0 to 0.75.
10. The method of claim 1, wherein the precipitant solution comprises one or more of sodium carbonate, sodium bicarbonate, ammonium carbonate, ammonium bicarbonate, sodium hydroxide, potassium hydroxide, sodium oxalate, ammonium oxalate; the molar concentration of the precipitant is 0.1-6 mol/L.
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