KR101760490B1 - Apparatus and method for manufacturing precursor - Google Patents
Apparatus and method for manufacturing precursor Download PDFInfo
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- KR101760490B1 KR101760490B1 KR1020150180840A KR20150180840A KR101760490B1 KR 101760490 B1 KR101760490 B1 KR 101760490B1 KR 1020150180840 A KR1020150180840 A KR 1020150180840A KR 20150180840 A KR20150180840 A KR 20150180840A KR 101760490 B1 KR101760490 B1 KR 101760490B1
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- aqueous solution
- storage tank
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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Abstract
A plurality of reactors for producing a precursor so that the production amount of the precursor can be effectively expanded while minimizing the structure of the equipment, a metal aqueous solution storage tank for storing the metal aqueous solution to be supplied to the reactor, A first metering pump for supplying the metering pump to at least two reactors, and a branching pipe connected between the first metering pump and each of the reactors, for separately supplying the metal aqueous solution to the respective reactors.
Description
To a precursor producing apparatus and a manufacturing method for producing a precursor having a reactor.
For example, a technique using a batch or continuous type coprecipitation reactor is known as a method for continuously producing a ternary cathode precursor among cathode materials for a secondary battery.
In order to produce precursors that cause a continuous gradient of concentration in one precursor particle, a metal aqueous solution is used as the reactor. a pH adjusting agent and the like are required in order to supply the respective raw materials.
Each storage tank connected to one reactor is provided with a metering pump for supplying a raw material to the reactor in a predetermined amount.
Generally, in order to increase the production amount of the precursor, a method of securing a reaction space by increasing the volume of the reactor or increasing the number of the reactors is used.
However, when the number of reactors is increased to increase the production amount, it is necessary to equip the necessary equipment in accordance with the number of reactors, including a metering pump for quantitatively injecting raw materials into each reactor from a storage tank. Thus, the management tasks for each reactor are increased, and the physical properties of the precursors produced in the individual reactors are not uniform.
Further, when increasing the volume of the reactor by increasing the volume of the reactor, it is difficult to sufficiently increase the production amount due to various limitations such as the stirrer and the metering pump, and additional facility expansion is required.
Provided are a precursor manufacturing apparatus and a manufacturing method that can effectively expand the production amount of a precursor while minimizing the configuration of a facility.
Also provided is a precursor manufacturing apparatus and a manufacturing method which can produce a large amount of precursors having more stable and uniform physical properties.
The precursor producing apparatus of this embodiment includes a plurality of reactors for producing a precursor, a metal aqueous solution reservoir for storing a metal aqueous solution to be supplied to the reactor, a single aqueous solution reservoir provided in the metal aqueous solution reservoir for supplying the aqueous metal solution to at least two reactors A first metering pump, and a branch pipe connected between the first metering pump and each of the reactors, for separately supplying the metal aqueous solution to the respective reactors.
The manufacturing apparatus may further include a homogenizing unit connected between the plurality of reactors to circulate the reactants between the reactors.
The homogenizing unit may include a circulation pipe connecting the one reactor and the neighboring reactor, and a circulation pump installed at one side of the circulation tube and transferring the reactants of the one reactor to the neighboring reactor.
The homogenizing unit may further include a recirculation pipe connected to a reactor which branches from one side of the circulation tube and supplies the reactants through the circulation tube to return some of the reactants.
The manufacturing apparatus includes a control agent storage tank for storing a pH control agent supplied to the reactor, a single second metering pump installed in the adjusting agent storage tank for supplying a pH adjusting agent to at least two or more reactors, And separately supplying the pH adjusting agent to each of the reactors.
The manufacturing apparatus includes a chelating agent storage tank for storing the chelating agent supplied to the reactor, a single third metering pump installed in the chelating agent storage tank for supplying the chelating agent to at least two reactors, And a branch pipe connected between the pump and each of the reactors to individually supply the chelating agent to each of the reactors.
At least one fourth metering pump installed in at least one or more of the controlled material storage tanks for supplying the composition control material to the metal aqueous solution storage tank, And a supply pipe connected between the aqueous solution storage tank and supplying the composition control material to the metal aqueous solution storage tank.
The method for producing a precursor of this embodiment includes the steps of supplying a raw material to a plurality of reactors and rotationally driving each of the reactors to produce a concentration gradient type precursor,
The step of supplying the raw material may include a step of transferring the aqueous metal solution from one metal aqueous solution storage tank storing the metal aqueous solution supplied to the reactor and branching the at least two reactors.
The step of supplying the raw material may further include feeding the pH adjusting agent from one adjusting agent storage tank, which is supplied with the pH adjusting agent supplied to the reactor, to branch at least into two or more reactors.
The step of supplying the raw material may include feeding the chelating agent from one chelating agent storage tank to which the chelating agent supplied to the reactor is transferred and branching it to at least two or more reactors.
In the step of supplying the raw material, the composition control material may be transferred from the at least one control material storage tank storing the composition control material supplied to the metal aqueous solution storage tank and supplied to the metal aqueous solution storage tank.
The manufacturing method may further include a homogenization step of circulating the reactants between the plurality of reactors.
The homogenization step may include transferring the reactants from one reactor to an adjacent reactor and circulating the reactants.
The homogenization may further include a recirculation step of returning some of the reactants circulating from one reactor to the adjacent reactor to the one reactor.
As described above, according to this embodiment, since the storage tank or the metering pump is not separately provided in each of the plurality of reactors, the production amount of the precursor can be effectively increased while minimizing the structure of the equipment.
In addition, by homogenizing the reactants produced in a plurality of reactors, a precursor having more stable and uniform physical properties can be mass-produced.
1 is a schematic view showing a precursor producing apparatus according to this embodiment.
2 is a SEM photograph of a precursor for a lithium secondary battery manufactured according to this embodiment and a comparative example.
FIG. 3 is a graph showing the results of measuring the particle size of the precursor for a lithium secondary battery according to the present invention and Comparative Example, according to reaction time.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the invention. The singular forms as used herein include plural forms as long as the phrases do not expressly express the opposite meaning thereto. Means that a particular feature, region, integer, step, operation, element and / or component is specified, and that other specific features, regions, integers, steps, operations, elements, components, and / And the like.
Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings so that those skilled in the art can easily carry out the present invention. It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention. Accordingly, the present invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
1 shows a production apparatus for producing a precursor according to this embodiment.
As shown in FIG. 1, the manufacturing apparatus 100 of the present embodiment includes a
The manufacturing apparatus may further include a control
The
In order to produce precursors that cause a continuous concentration gradient in one precursor particle, a different aqueous metal solution is required. In FIG. 1, only one metal
For example, the manufacturing apparatus can produce a cathode precursor for a cathode material of a secondary battery using a rotating flow of the
In the present embodiment, a plurality of
The manufacturing apparatus is provided with at least two
1, in the present embodiment, three
The apparatus of the present embodiment is characterized in that a plurality of
A single
The metal aqueous solution supplied from the
As described above, even when the number of reactors is increased by providing a metal aqueous
The manufacturing apparatus of this embodiment includes a
The manufacturing apparatus includes a plurality of
The
As described above, the plurality of
The manufacturing apparatus of the present embodiment includes a chelating
The manufacturing apparatus is provided in the chelating
The
As described above, the plurality of the
The manufacturing apparatus of this embodiment includes a control
The manufacturing apparatus may be configured to connect the controlled
As described above, by supplying a plurality of
Therefore, it is possible to mass-produce a large number of precursors while simplifying the structure of the equipment by branching the raw materials into a plurality of reactors by using only one metering pump for each raw material storage tank, .
The manufacturing apparatus further includes a homogenizing unit connected between the plurality of reactors (10) to circulate the reactants between the reactors (10). In the manufacturing apparatus, the reactants produced in the
1, the homogenizer includes a
The homogenizing unit further includes a
The circulation pipe (62) extends from the lower portion of the one reactor (10) to an upper portion of the adjacent reactor (10). A circulation pump (60) is installed on one side of the circulation pipe (62). When the
As described above, the
In addition to the transfer structure by the circulation pump, the reactants may overflow from one side of the reactor to the neighboring reactor and move and mix with each other. This structure is also homogenized by mixing the reactants between the reactors.
Hereinafter, a process of manufacturing the cathode precursor from the above apparatus will be described.
In the preparation of the precursor of this embodiment, a raw material containing an aqueous metal solution is supplied to a plurality of reactors, and each of the reactors is rotationally driven to produce a concentration gradient type precursor.
The feeding of the raw material may include feeding the aqueous metal solution from the metallic aqueous solution storage tank storing the metallic aqueous solution supplied to the reactor, and branching the fed aqueous solution into at least two reactors.
Thus, by branching the raw material and supplying it to a plurality of reactors, a large amount of precursors can be mass-produced from a plurality of reactors.
In this embodiment, a pH adjusting agent for adjusting the pH of the coprecipitation reaction, a chelating agent for agglomeration, or a composition controlling substance may be further supplied to the inside of the reactor.
For this purpose, the step of supplying the raw material may further include feeding the pH adjusting agent from the adjusting agent storage tank stored in the pH adjusting agent supplied to the reactor, and supplying the pH adjusting agent to at least two or more reactors.
In addition, the raw material supplying step may include feeding the chelating agent from the chelating agent storage tank, which is supplied from the chelating agent supplied to the reactor, to the at least two or more reactors.
In addition, the step of supplying the raw material may include a step of feeding the composition control material from the at least one control material storage tank storing the composition control material supplied to the reactor to the metal aqueous solution storage tank.
Each raw material is branched into a plurality of reactors in each of a single metal aqueous solution storage tank, a control agent storage tank, and a chelating agent storage tank. In each reactor, a precursor is produced through a coprecipitation reaction.
The coprecipitation reaction refers to the simultaneous precipitation of various different ions into an aqueous solution or a non-aqueous solution. For example, two or three elements are simultaneously precipitated in an aqueous solution using a neutralization reaction to obtain a precursor in the form of hydroxide or oxide, and this precursor is mixed with lithium hydroxide and fired.
The manufacturing method of the present embodiment further includes a homogenization step of circulating a reactant between a plurality of reactors in a precursor manufacturing process.
The homogenization step includes transferring and circulating the reactants from one reactor to an adjacent reactor. The homogenization may further include a recycling step of returning some of the reactants circulating from one reactor to the adjacent reactor to the one reactor.
The reactants produced in one reactor are transferred to the adjacent reactor by a circulation pump, and the reactants produced in the plurality of reactors are exchanged and mixed. Thus, the reactants contained in each of the reactors have the same physical properties that are homogenized by mixing with each other. As described above, the reactants are circulated or overflowed and mixed in each reaction period and homogenized with each other, so that even when the precursors are produced through a plurality of reactors, precursors having the same physical properties can be manufactured in large quantities.
[Example]
As an example, a cathode active material particle for a lithium secondary battery was produced by using the production apparatus shown in Fig. In Example 1, the average overall composition of the particles was Ni 0 . 6 Mn 0 . 2 Co 0 .2 (OH) 2 , and Example 2 is a positive electrode active material particle having an average particle composition of Ni 0 . 8 Mn 0 . 1 Co 0 .1 (OH) is a positive electrode active material particle is represented by 2.
[Comparative Example]
As a comparative example, cathode active material particles for a lithium secondary battery were produced using a conventional single reactor. Comparative Example 1 is a positive electrode active material particle having an average particle composition of Ni 0.6 Mn 0.2 Co 0.2 (OH) 2 , and Comparative Example 2 is an anode active material particle having an average particle composition of Ni 0.8 Mn 0.1 Co 0.1 (OH) 2 Active material particles.
[Production of cathode active material particle]
A metal mixed solution having the same composition as shown in Table 1 below was fed in the same manner as in the metal aqueous solution storage tank and the controlled material storage tank in both Examples and Comparative Examples, and a precursor for a lithium secondary battery was prepared using the reactor. In the case of the embodiment, as described above, the metering pump and the circulation pump were driven to supply a metal mixed solution to each reactor to prepare a precursor. As a comparative example, a precursor was prepared by supplying a metal mixed solution to a single reactor as in the prior art.
[Experimental Example 1]
SEM photographs of the precursors for lithium secondary batteries prepared in Examples and Comparative Examples were measured and the results were compared. As shown in FIG. 2, it can be confirmed that the particle size distribution is uniform in the examples as compared with the comparative example.
Table 2 below shows the results of measuring the reaction time, final particle size, filling density and yield of the lithium secondary battery precursors prepared in Examples and Comparative Examples.
㎛
g / cc
kg / batch
As shown in Table 2, in the examples, the production amount is much higher than that in the comparative example, and it can be confirmed that mass production in the case of this embodiment is possible.
[Experimental Example 2]
The particle sizes of the precursors for lithium secondary batteries prepared in Examples and Comparative Examples were measured according to the reaction time, and Fig. 3 shows the results. As shown in FIG. 3, even when manufactured according to the embodiment, it can be confirmed that the growth rate is similar to the comparative example without deteriorating.
While the illustrative embodiments of the present invention have been shown and described, various modifications and alternative embodiments may be made by those skilled in the art. Such variations and other embodiments will be considered and included in the appended claims, all without departing from the true spirit and scope of the invention.
10: Reactor 20: Metal aqueous solution storage tank
22:
30: Controlling agent storage tank 40: Chelating agent storage tank
50: Control material storage tank 60: circulation pump
62: circulation tube 64: recirculation tube
Claims (14)
Each of the reactors is connected in parallel to a metal aqueous solution reservoir and is supplied with a metal aqueous solution from a metal aqueous solution reservoir through a first metering pump and a branch,
The homogenizing unit includes a circulation pipe for connecting one of the reactors and the neighboring reactors, a circulation pump installed at one side of the circulation pipe for transferring the reactants of the one reaction chamber to the neighboring reactors, And a re-circulation tube connected to the reactor for supplying a portion of the reactant and returning a part of the reactant.
A pH adjusting agent supplied to the reactor; a single second metering pump installed in the adjusting agent storage tank to supply a pH adjusting agent to at least two or more reactors; and a second metering pump connected between the second metering pump and each of the reactors, And a branch pipe for separately feeding the regulator into each reactor.
A single third metering pump installed in the chelating agent storage tank for supplying a chelating agent to at least two or more reactors, and a third metering pump installed in the chelating agent storage tank for supplying the chelating agent to the reactor, And a branching pipe connected between the plurality of reactors and separately feeding the chelating agent to each of the reactors.
At least one fourth metering pump installed in at least one or more of the controlled material storage tanks for supplying the composition control material to the metal aqueous solution storage tank, And a supply pipe connected between the aqueous solution storage tank and supplying the composition control material to the metal aqueous solution storage tank.
Wherein the homogenizing step comprises transferring and circulating the reactants from one reactor to an adjacent reactor and a recirculation step of returning some of the reactants circulating from the one reactor to the neighboring reactor to the one reactor.
Wherein the step of supplying the raw material further comprises the step of feeding the pH adjuster branched from at least one reservoir containing the pH adjuster supplied to the reactor to at least two reactors.
Wherein the feedstock comprises branching and feeding the chelating agent to at least two reactors from one chelating agent storage tank where the chelating agent is fed to the reactor.
Wherein the step of supplying the raw material comprises the step of feeding the composition control material from at least one or more control material storage tanks storing the composition control material supplied to the metal aqueous solution storage tank to the metal aqueous solution storage tank.
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