CN217699184U - Ternary precursor preparation system - Google Patents
Ternary precursor preparation system Download PDFInfo
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- CN217699184U CN217699184U CN202221648965.8U CN202221648965U CN217699184U CN 217699184 U CN217699184 U CN 217699184U CN 202221648965 U CN202221648965 U CN 202221648965U CN 217699184 U CN217699184 U CN 217699184U
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Abstract
The utility model belongs to the technical field of lithium ion battery cathode material precursor, concretely relates to ternary precursor preparation system, including reation kettle, agitating unit, transfer tank and concentrated machine, agitating unit includes the motor and sets up the stirring thick liquid in reation kettle inside, reation kettle's overflow mouth and the feed inlet pipeline intercommunication of transfer tank, the discharge gate of transfer tank and the feed inlet pipeline intercommunication of concentrated machine, the discharge gate of concentrated machine and reation kettle's first feed inlet, the feed inlet of transfer tank is respectively through first pipeline, second pipeline intercommunication, first pipeline, set up first valve and second valve on the second pipeline respectively. The utility model discloses a preparation system simple structure adopts a reation kettle can prepare the nickel cobalt manganese ternary positive electrode material precursor that obtains granularity multi-stage distribution, reduces the miropowder and produces to it is controllable to realize granularity distribution.
Description
Technical Field
The utility model belongs to the technical field of lithium ion battery cathode material precursor, a ternary precursor preparation system is related to, more specifically relates to a preparation system of nickel cobalt manganese hydroxide of wide particle size distribution.
Background
The key material of the lithium ion battery is a positive electrode material, which accounts for about 30% of the cost of the lithium ion battery, and lithium cobaltate, ternary material, lithium manganate and lithium iron phosphate are mainly applied in the current market. Wherein the ternary material, namely the lithium nickel cobalt manganese oxide material, is a novel lithiumA battery positive electrode material; compared with other anode materials, the anode material has the advantages of high mass specific capacity, low cost, good thermal stability, high energy density and the like, and is widely applied to the fields of digital electronic products, electric tools, electric bicycles and the like. The ternary material is prepared by mixing a ternary precursor and a lithium source and then sintering at a high temperature. Nickel cobalt manganese hydroxide is a widely used ternary precursor material with a chemical general formula of NixCoyMnz(OH)2Specifically, nickel salt, cobalt salt and manganese salt are used as raw materials, and the specific dosage proportion of nickel, cobalt and manganese is adjusted according to actual needs.
However, with the rapid development of the current electric vehicles, people have higher and higher requirements on the charge-discharge specific capacity, the cycle life and the stability of the lithium ion battery. At present, the nickel cobalt lithium manganate materials with single particle size or relatively narrow particle size distribution are mostly prepared, and the materials have low tap density, low compaction and capacity multiplying power and are easy to break. At present, the compaction density of the product is improved mainly by preparing large particles and small particles step by step and then mixing the large particles and the small particles, and higher capacity can be obtained in a limited volume space. The current mainstream process is to mix the large and small particles after separate sintering. However, the separate sintering and blending have the following problems: (1) Different production processes are required to be designed for the preparation and subsequent sintering of the precursors of the large and small particles, so that the production cost is greatly increased; (2) The problems of secondary spherical particle agglomeration and poor sphericity exist during the preparation of the precursor with small particle size; (3) When the small-particle-size precursor secondary spherical particles are synthesized, good crystal seeds are difficult to obtain, and the tap density is low.
SUMMERY OF THE UTILITY MODEL
The problem to prior art exists, the utility model aims at providing a ternary precursor preparation system, this production system simple structure adopts a reation kettle can prepare the nickel cobalt manganese ternary positive pole material precursor that obtains granularity multi-stage distribution, reduces the miropowder and produces to it is controllable to realize the granularity distribution.
In order to achieve the above object, the present invention provides the following specific technical solutions.
The utility model provides a ternary precursor preparation system, includes reation kettle, agitating unit, transfer tank and concentrated machine, agitating unit includes agitator motor and sets up the stirring thick liquid in reation kettle inside, reation kettle's overflow mouth and the feed inlet pipeline intercommunication of transfer tank, the discharge gate of transfer tank and the feed inlet pipeline intercommunication of concentrated machine, the discharge gate of concentrated machine and reation kettle's first feed inlet, the feed inlet of transfer tank are respectively through first pipeline, second pipeline intercommunication, set up first valve and second valve on first pipeline, the second pipeline respectively.
Preferably, the reaction kettle is provided with a metal salt solution feed inlet, an alkali liquor feed inlet and an ammonia water feed inlet; and further preferably, flow rate control valves are arranged on the metal salt solution feed inlet, the alkali liquor feed inlet and the ammonia water feed inlet.
Preferably, the reaction kettle is also provided with an air inlet; it is further preferred that an air pressure monitor is provided at the air inlet.
Preferably, the outer wall of the kettle body of the reaction kettle is provided with a heating jacket.
Preferably, a transfer pump is arranged on a pipeline for communicating the discharge hole of the transfer tank with the feed hole of the thickener.
Preferably, the preparation system further comprises an aging device for aging the materials in the reaction kettle.
Preferably, the preparation system further comprises a dehydration device for dehydrating the material in the aging device.
Preferably, the preparation system further comprises a drying device for drying the materials in the dehydration device.
Ternary precursor preparation system is particularly useful for preparing the nickel cobalt manganese hydroxide of wide particle size distribution.
Compared with the prior art, the technical scheme of the utility model obvious beneficial effect below having.
The utility model discloses a preparation system simple structure adopts a reation kettle can prepare the nickel cobalt manganese ternary positive electrode material precursor that obtains granularity multi-stage distribution, reduces the miropowder and produces to it is controllable to realize granularity distribution.
Drawings
FIG. 1 is a schematic view of the system configuration of the process of example 1.
Fig. 2 is a 5000-fold FESEM image of nickel cobalt manganese hydroxide of broad particle size distribution prepared in example 2.
Fig. 3 is a 1000-fold FESEM image of nickel-cobalt-manganese hydroxide of broad particle size distribution prepared in example 2.
Fig. 4 is a 5000-fold FESEM image of nickel cobalt manganese hydroxide of broad particle size distribution prepared in example 3.
Fig. 5 is a 1000-fold FESEM image of nickel-cobalt-manganese hydroxide of broad particle size distribution prepared in example 3.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, further description will be made below by way of examples. It should be understood that the following examples are illustrative of the present invention only and are not intended to limit the scope of the present invention. In the examples, the methods used are conventional methods unless otherwise specified, and the equipment used is commercially available.
Example 1
As shown in fig. 1, the embodiment provides a ternary precursor preparation system, specifically a preparation system of nickel, cobalt, manganese hydroxide with wide particle size distribution, the preparation system includes a reaction kettle 1, a stirring device, a transit tank 2 and a thickener 3, the stirring device includes a stirring motor 4 and a stirring paddle 5 arranged inside the reaction kettle 1, an overflow port of the reaction kettle 1 is communicated with a feed inlet pipeline of the transit tank 2, a discharge port of the transit tank 2 is communicated with a feed inlet pipeline of the thickener 3, a discharge port of the thickener 3 is communicated with a first feed inlet of the reaction kettle 1 and a feed inlet of the transit tank 2 through a first pipeline and a second pipeline respectively, and the first pipeline and the second pipeline are provided with a first valve 6 and a second valve 7 respectively; the outer wall of the kettle body of the reaction kettle 1 is provided with a heating jacket 8.
In this embodiment, the reaction kettle 1 is further provided with a metal salt solution feed port, an alkali liquor feed port and an ammonia water feed port; flow rate control valves are arranged on the metal salt solution feed port, the alkali liquor feed port and the ammonia water feed port.
In this embodiment, the reaction kettle 1 is further provided with an air inlet, and the air inlet is provided with an air pressure monitor.
In this embodiment, a transfer pump is disposed on a pipeline connecting the discharge port of the transfer tank 3 and the feed port of the thickener 3.
In this embodiment, the preparation system further includes an aging device for aging the materials in the reaction kettle, a dehydration device for dehydrating the materials in the aging device, and a drying device for drying the materials in the dehydration device.
The preparation method of the nickel-cobalt-manganese hydroxide with wide particle size distribution by using the ternary precursor preparation system of the embodiment comprises the following steps:
(1) Preparing a nickel-cobalt-manganese metal salt solution, a precipitator solution and an ammonia water solution.
(2) Adding clear water, the precipitant solution prepared in the step (1) and an ammonia water solution into a reaction kettle 1 to prepare a base solution, and adjusting the alkalinity, the temperature, the pH value and the rotating speed of a stirring paddle 5 of the base solution; and introducing nitrogen through the air inlet for protection to a certain atmospheric pressure.
(3) On the basis of the step (2), adding a nickel-cobalt-manganese metal salt solution, a precipitator solution and an ammonia water solution into the reaction kettle 1 through a metal salt solution feed port, an alkali liquor feed port and an ammonia water feed port at the same time, and controlling the flow rates of the three feed ports through a flow rate control valve to prepare a nickel-cobalt-manganese hydroxide crystal nucleus; regulating alkalinity and pH value under stirring to promote crystal nucleus growth, and tightly packing the primary particles into secondary particles; meanwhile, when the liquid level in the reaction kettle 1 reaches the discharging requirement, the thickener 3 is started to discharge, and the liquid level in the reaction kettle 1 is kept stable.
(4) When the particle size value of the reaction slurry reaches a certain value, the first valve 6 of the thickener 3 which flows back to the reaction kettle 1 is closed, the second valve 7 of the thickener 3 which flows back to the transit tank 2 is opened, so that the materials which flow back from the thickener 3 flow to the transit tank 2, and then are pumped to the thickener 3 from the transit tank 2, and in the method, the materials in the transit tank 2 and the thickener 3 form external circulation without passing through the reaction kettle 1, and the particle size of the materials does not grow any more. The particle size of the materials in the reaction kettle 1 continuously grows along with the addition of the nickel-cobalt-manganese solution, when the particle size of the materials in the reaction kettle 1 reaches a certain value, the thickener 3 is opened again to flow back to the first valve 6 of the reaction kettle 1, the thickener 3 is closed to flow back to the second valve 7 of the transfer tank 2, and the materials of the reaction kettle 1, the transfer tank 2 and the thickener 3 form circulation, so that large and small particles grow together.
(5) And stopping the reaction when the particle size of the particles in the reaction slurry meets the requirement, and conveying the reaction slurry to an aging device, a dehydration device and a drying device for aging, dehydration and drying to obtain the precursor of the nickel-cobalt-manganese ternary cathode material with mixed large and small particles.
Example 2
The embodiment discloses a preparation method for preparing nickel-cobalt-manganese hydroxide with wide particle size distribution by using the ternary precursor preparation system in embodiment 1, which comprises the following steps:
(1) 2.0mol/L of nickel cobalt manganese sulfate solution, 10mol/L of sodium hydroxide solution and 25wt% of ammonia water are prepared
(2) And (2) adding clear water, the sodium hydroxide solution prepared in the step (1) and an ammonia water solution into a reaction kettle to prepare a base solution, wherein the alkalinity of the base solution is 3.0g/L, the pH value is 11.05, the rotation speed of the reaction kettle is 50Hz, the temperature is 55 ℃, and nitrogen protection is started.
(3) On the basis of the step (2), adding a nickel-cobalt-manganese metal salt solution, a precipitator solution and an ammonia water solution into a reaction kettle at the same time, wherein the flow rate of the nickel-cobalt-manganese solution is 8L/h, the flow rate of the sodium hydroxide solution is 3.0L/h, the flow rate of the ammonia water solution is 0.3L/h, the alkalinity is adjusted to be 3.0g/L, the pH value is 11.05 under the condition of the rotation speed of 50Hz, and the temperature is controlled to be 55 ℃; preparing a nickel-cobalt-manganese hydroxide crystal nucleus; under the condition that other conditions are not changed, the pH value is reduced to 10.90, the growth of crystal nuclei is promoted, and primary particles are tightly packed into secondary particles; meanwhile, when the liquid level in the reaction kettle meets the clearing requirement, a thickener is started to begin clearing, and the liquid level in the reaction kettle is kept stable.
(4) When the particle size of the reaction slurry is 3.36 microns, closing a first valve of the thickener which flows back to the reaction kettle, opening a second valve of the thickener which flows back to the transit tank, enabling the backflow materials of the thickener to flow to the transit tank, and then pumping the backflow materials to the thickener from the transit tank. The granularity of the materials in the reaction kettle continuously grows along with the addition of the nickel-cobalt-manganese solution, when the granularity of the materials in the reaction kettle is 4.0 mu m, the first valve of the thickener which flows back to the reaction kettle is opened again, the second valve of the thickener which flows back to the transfer tank is closed, the materials of the reaction kettle, the transfer tank and the thickener form circulation, and the large particles and the small particles grow together.
(5) And when the particle size of the particles in the reaction slurry reaches 4.2 mu m, stopping the reaction, aging, dehydrating and drying to obtain the precursor of the nickel-cobalt-manganese ternary cathode material with mixed large and small particles, wherein the FESEM images of the precursor are shown in figures 2 and 3.
Example 3
The embodiment discloses a preparation method for preparing nickel-cobalt-manganese hydroxide with wide particle size distribution by using the ternary precursor preparation system in embodiment 1, which comprises the following steps:
(1) 2.2mol/L of nickel cobalt manganese sulfate solution, 10mol/L of sodium hydroxide solution and 25wt% of ammonia water are prepared
(2) And (2) adding clear water, the sodium hydroxide solution prepared in the step (1) and an ammonia water solution into a reaction kettle to prepare a base solution, wherein the alkalinity of the base solution is 5.5g/L, the pH value is 11.45, the rotation speed of the reaction kettle is 50Hz, the temperature is 55 ℃, and nitrogen protection is started.
(3) On the basis of the step (2), adding a nickel-cobalt-manganese metal salt solution, a precipitator solution and an ammonia water solution into a reaction kettle at the same time, wherein the flow rate of the nickel-cobalt-manganese solution is 9L/h, the flow rate of the sodium hydroxide solution is 3.9L/h, the flow rate of the ammonia water solution is 0.6L/h, the alkalinity is adjusted to be 5.5g/L, the pH value is 11.45 under the condition of the rotation speed of 50Hz, and the temperature is controlled to be 55 ℃; preparing a nickel-cobalt-manganese hydroxide crystal nucleus; under the condition that other conditions are not changed, the pH value is reduced to 11.20, the crystal nucleus is promoted to grow, and the primary particles are tightly packed into secondary particles; meanwhile, after the liquid level in the reaction kettle reaches the discharging requirement, the thickener is started to discharge, and the liquid level in the reaction kettle is kept stable.
(4) When the particle size of the reaction slurry is 2.7 microns, the first valve of the thickener which flows back to the reaction kettle is closed, the second valve of the thickener which flows back to the transit tank is opened, so that the material which flows back from the thickener flows to the transit tank and is pumped to the thickener from the transit tank. The granularity of the materials in the reaction kettle continuously grows along with the addition of the nickel-cobalt-manganese solution, when the granularity of the materials in the reaction kettle is 3.65 mu m, the first valve of the thickener which flows back to the reaction kettle is opened again, the second valve of the thickener which flows back to the transfer tank is closed, the materials of the reaction kettle, the transfer tank and the thickener form circulation, and the large particles and the small particles grow together.
(5) And stopping reaction when the particle size of the particles in the reaction slurry reaches 3.8 mu m, aging, dehydrating and drying to obtain a precursor of the nickel-cobalt-manganese ternary cathode material with mixed large and small particles, wherein FESEM images of the precursor are shown in figures 4 and 5.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of improvements and decorations can be made without departing from the principle of the present invention, and these improvements and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The utility model provides a ternary precursor preparation system, a serial communication port, the preparation system includes reation kettle, agitating unit, transfer tank and concentrated machine, agitating unit includes agitator motor and sets up the stirring thick liquid in reation kettle inside, reation kettle's overflow mouth and transfer tank's feed inlet pipeline intercommunication, transfer tank's discharge gate and concentrated machine's feed inlet pipeline intercommunication, concentrated machine's discharge gate and reation kettle's first feed inlet, transfer tank's feed inlet are respectively through first pipeline, second pipeline intercommunication, set up first valve and second valve on first pipeline, the second pipeline respectively.
2. The ternary precursor preparation system of claim 1, wherein the reaction kettle is further provided with a metal salt solution feed inlet, an alkali liquor feed inlet and an ammonia water feed inlet.
3. The ternary precursor preparation system of claim 2, wherein flow rate control valves are disposed on the metal salt solution feed port, the alkali solution feed port and the ammonia water feed port.
4. The ternary precursor manufacturing system of claim 1, wherein said reaction vessel is provided with an air inlet.
5. The ternary precursor preparation system of claim 4, wherein a gas pressure monitor is provided at the gas inlet.
6. The ternary precursor preparation system of claim 1, wherein a heating jacket is disposed on an outer wall of the reaction vessel.
7. The ternary precursor preparation system of claim 1, wherein a transfer pump is disposed on a conduit communicating the discharge port of the transfer tank with the feed port of the thickener.
8. The ternary precursor preparation system according to any one of claims 1 to 7, wherein the preparation system further comprises an aging device for aging materials in the reaction kettle.
9. The ternary precursor manufacturing system of claim 8, further comprising a dehydration unit that dehydrates the contents of the aging unit.
10. The ternary precursor manufacturing system of claim 9, further comprising a drying device for drying the contents of the dehydration device.
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