KR20130032563A - Crystallization reaction apparatus and preparation method of high purity lithium carbonate - Google Patents

Crystallization reaction apparatus and preparation method of high purity lithium carbonate Download PDF

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Publication number
KR20130032563A
KR20130032563A KR1020110096233A KR20110096233A KR20130032563A KR 20130032563 A KR20130032563 A KR 20130032563A KR 1020110096233 A KR1020110096233 A KR 1020110096233A KR 20110096233 A KR20110096233 A KR 20110096233A KR 20130032563 A KR20130032563 A KR 20130032563A
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South Korea
Prior art keywords
reaction
crystallization
lithium carbonate
reactor
liquid
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KR1020110096233A
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Korean (ko)
Inventor
방상구
김우식
강혜련
김다영
장기섭
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케이엔디티앤아이 주식회사
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Priority to KR1020110096233A priority Critical patent/KR20130032563A/en
Publication of KR20130032563A publication Critical patent/KR20130032563A/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B01J19/1806—Stationary reactors having moving elements inside resulting in a turbulent flow of the reactants, such as in centrifugal-type reactors, or having a high Reynolds-number
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/08—Carbonates; Bicarbonates

Abstract

PURPOSE: A crystallization reactor and a method for preparing lithium carbonate are provided to prevent formation of scale and to produce a large amount of lithium carbonate which is used as a main ingredient for a secondary battery. CONSTITUTION: A crystallization reactor comprises a reaction tank(11) and an inner cylinder. Inlet ports(13,14) of a reaction ingredient and an outlet port are mounted in the reaction tank. The reaction tank has an inner reaction space(17) for crystallization. An inner cylinder is placed in the inner space of the reaction tank. Protrusions(18,19) are formed on the surface of the inner cylinder at predetermined intervals. A method for preparing lithium carbonate comprises: a step of inputting a lithium salt in a liquid phase and carbon dioxide in a vapor phase, or a lithium salt in a liquid phase and sodium carbonate in a liquid phase into the reactor; a step of rotating a rotor(12) and forming a Taylor vortex flow for crystallizing; and a step of performing solid-liquid separation from the solution discharged from the outlet(15) and separating high purity lithium carbonate.

Description

Crystallization reaction apparatus and preparation method of high purity lithium carbonate using the same {Crystallization reaction apparatus and Preparation method of high purity Lithium Carbonate}

The present invention relates to a crystallization reaction apparatus and a method for producing high purity lithium carbonate using the same, and more particularly, it is possible to prevent the formation of scale in advance, and a large amount of lithium carbonate, which is a lithium source used as a main raw material for secondary batteries and the like, in large quantities. It is to provide a crystallization reaction apparatus that can be produced by and a method for producing high purity lithium carbonate using the same.

Lithium is a raw material for secondary batteries used in electric vehicles, mobile phones, laptops, etc., and can be used as a next-generation fusion power source. However, the country has been keen to compete in securing lithium because of the severe resource bias, which accounts for about 70% of the world's lithium reserves. The international price of lithium carbonate, which is used as a rechargeable battery raw material, has tripled between 2002 and 2008. As a result, it is expected that automakers will be in serious competition to secure lithium batteries for electric vehicles.

As described above, the method for producing lithium carbonate used as a raw material of a secondary battery includes a gas-liquid reaction process in which carbon dioxide gas is injected into a solution in which lithium chloride is dissolved in sodium hydroxide, and a reaction between molten lithium chloride and molten sodium carbonate. The liquid-liquid reaction process to make is mentioned. Conventionally, both of these reactions have been carried out by a batch process, but the reaction time is long and the yield is significantly reduced.

The present invention has been proposed to solve the problems of the prior art as described above, the object of which is to prevent the formation of scale in advance, a large amount of lithium carbonate which is a lithium source used as a main raw material for secondary batteries, etc. It is to provide a crystallization reaction apparatus that can be produced by and a method for producing high purity lithium carbonate using the same.

The technical problem as described above is achieved by the following configuration according to the present invention.

(1) a reaction tank having an inlet and an outlet of a reaction raw material and having an internal reaction space in which a crystallization reaction takes place; And an inner cylinder located in the inner space of the reactor and having protrusions formed on the surface at predetermined intervals.

(2) The method according to claim 1,

Crystallization reactor, characterized in that the projections formed on the inner surface of the reactor at a predetermined interval.

(3) injecting a liquid lithium salt and a gaseous carbon dioxide, or a liquid lithium salt and a liquid sodium carbonate into the reactant inlet as a reactant in the crystallization reactor according to claim 1; Rotating the rotor to form a Taylor vortex in the reactant introduced to perform a crystallization reaction; And separating the high-purity lithium carbonate by solid-liquid separation of the solution from the outlet of the crystallization machine.

(4) The method according to claim 3,

The method for producing lithium carbonate using a crystallization reaction device, characterized in that the pH of the reaction of the formation of lithium carbonate.

(5) The method according to claim 1,

Crystallization reaction of lithium carbonate is a method for producing lithium carbonate using a crystallization reactor, characterized in that carried out at pH 10.5 to 10.8.

(6) The method according to 1,

The reactant is a method of producing lithium carbonate using a crystallization reactor, characterized in that the injection is divided into a plurality of inlet formed in the Kuet-Taylor crystallization.

(7) the method of paragraph 3,

A method for producing lithium carbonate using a crystallization reaction apparatus, characterized in that the carbon dioxide is injected into NaOH or LiCl and T-tube at the same time to the reactant inlet.

According to the above structure of the present invention, it is possible to produce a large amount of lithium carbonate, which is a source of lithium used as a main raw material for secondary batteries and the like, in high purity.

1 is a cross-sectional view of a Kuet-Taylor reactor used in the present invention.
2 is a block diagram of a system for producing a lithium carbonate by a continuous reaction according to the present invention
Figure 3 is an explanatory view showing the vortex characteristics in the Cuette-Taylor reactor used in the present invention

The present invention is a reaction tank is provided with the inlet and outlet of the reaction raw material, the reaction tank having an internal reaction space in which the crystallization reaction takes place; And a crystallization reactor positioned in the reaction vessel inner space and including an inner cylinder having protrusions formed on the surface at predetermined intervals.

In addition, the present invention comprises the steps of injecting a liquid lithium salt and gaseous carbon dioxide, or a liquid lithium salt and a liquid sodium carbonate to the reactant inlet as a reactant in the crystallization reactor; Rotating the rotor to form a Taylor vortex in the reactant introduced to perform a crystallization reaction; And solid-liquid separation of the solution from the outlet of the crystallizer to separate lithium carbonate of high purity.

Hereinafter, the crystallization reaction will be described in detail with reference to the accompanying drawings.

Figure 1 illustrates the configuration of a crystallization reactor that can be used in the crystallization reaction of the present invention. The reactor includes a reactor 11, an inner cylinder 12, raw material inlets 13 and 14, a product outlet 15, and a heat supply unit 16 for supplying heat to the reactor. Reference numeral 17 represents a reaction vessel internal space.

Protrusions 18 are formed on the surface of the inner cylinder 12 to prevent scale formation. Preferably, the protrusion is formed over the entire outer circumferential surface of the inner cylinder 12 at regular intervals. As such, by placing the projections 18 on the inner cylinder 12, crystals formed in the course of the crystallization reaction are scaled on the surface of the inner cylinder 12, which adversely affects the formation of vortices in the subsequent reaction process and thus the reaction. After you finish, you can save yourself from having to remove these scales every time. As such, the protrusion 18 formed on the inner cylinder 12 serves to block crystals from adhering to the outer circumferential surface when the inner cylinder 12 rotates, thus performing a repeated reaction for a long time. There is no need to separate the cylinder to remove the scale from sticking to the surface.

The crystallization reaction apparatus of the present invention preferably forms projections 19 at regular intervals on the inner circumferential surface of the reaction tank 11 to prevent the formation of scales that adhere to the surface of the inner circumferential surface in the course of the crystallization process.

The crystallization reaction apparatus of the present invention as described above is particularly useful in the reaction process for crystallizing lithium carbonate. This is because in the case of using a conventional Kuet-Taylor crystallization reactor, scales are better formed in other reaction processes, and the reaction tanks must be separated periodically to remove the scales formed in the inner cylinder and inside the reactor.

Hereinafter, the contents of the present invention will be described in detail by taking a process of performing a crystallization reaction of lithium carbonate using the crystallization reaction device according to the present invention as an example.

First, the liquid lithium salt as the crystallization raw material and the carbon dioxide in the gas phase, or the liquid lithium salt and the liquid sodium carbonate are introduced through the raw material inlets 13 and 15 provided at one side of the reaction tank 11. In this case, the raw material inlets 13 and 15 may be provided not only on one side of the reaction tank, but also located at the center of the reaction tank, or two or more may be provided. In the case where a plurality of raw material inlets 13 and 15 are installed at regular intervals, the reactants may be divided and introduced into a predetermined fraction. Splitting and adding the reactants in this manner is more advantageous in the case where the growth of the crystal is predominant to produce the macrocrystalline particles.

As an embodiment according to the first aspect of the present invention, in the case of gas-liquid reaction, the injection concentration of the reactant introduced into the reactor 11 is 0.2 to 0.3 M / min for lithium salt, 0.2 to 0.4 M / min for 50% NaOH, and carbon dioxide 0.3-0.5 M / min is preferable. If it is out of the above injection concentration range, the crystallization reaction is delayed or it is difficult to obtain the desired purity. Lithium chloride, lithium bromide, etc. are mentioned as said lithium salt in this invention.

In the case of the gas-liquid reaction according to the present invention, a reaction time of 5 to 10 minutes is sufficient, and the recovery rate of lithium carbonate is more than 80%.

As an embodiment according to the second aspect of the present invention, in the case of a liquid solution reaction, the concentration of the reactant introduced into the reactor 11 is 0.03 to 0.05 M / min for lithium salt and 0.02 to 0.03 M / min for 30% Na 2 CO 3. desirable. Similarly, if it is out of the above concentration range, the crystallization reaction is delayed or it is difficult to obtain the desired purity. Lithium chloride, lithium bromide, etc. are mentioned as said lithium salt in this invention.

In the case of the liquid-liquid reaction according to the present invention, it is sufficient that the reaction time is 30 to 40 minutes, and the recovery rate of lithium carbonate is more than 75%.

In the reaction process according to the present invention, the process for forming lithium carbonate is performed at pH 7 to 8, and the crystallization process is preferably performed at pH 10.5 to 10.8 in preparing high purity lithium carbonate.

Figure 2 illustrates the overall configuration of the lithium carbonate separation process system including the crystallization reactor of the present invention.

Reference numeral 20 denotes a solid-liquid separator for separating crystals from a solution containing crystals, reference numeral 30 denotes a distillation column for separating and recovering a solvent from a solution obtained after solid-liquid separation, and numerals 21 to 22 denote pumps.

As such, after dissolving lithium salt in a solvent at a desired concentration, a lithium-containing solution in a solution state is injected into the reactor 11 using the pump 21 through a reactant inlet 13, and at the same time, carbon dioxide or sodium carbonate in solution is pumped ( 22) through the reactant inlet (14). In this case, when the carbon dioxide is injected, it is preferable to inject the NaOH or LiCl and the T-tube at the same time to be injected into the reactant inlet to prevent the formation of crystals in the CO 2 tube and to block it.

As described above, each reactant injected into the reaction tank 11 is stirred in the Kuet-Taylor reactor 10 as the inner cylinder 12 rotates.

The inner cylinder 12 is rotated by a rotating motor (not shown) to the outside. When the rotational speed of the inner cylinder 12 is greater than or equal to the threshold value, the reactants around the inner cylinder 12 move under the centrifugal force in the vertical direction from the rotational axis, thereby forming a Taylor vortex. As a result, the flow of the reactants is very regular and the temperature distribution is very uniform, so that the reaction proceeds well. After a certain time, the pH of the reactants is increased to obtain uniform particle size of high purity. It becomes possible. Although the rotation speed of the said inner cylinder 12 in the manufacturing process of the lithium carbonate by a continuous process of this invention is not specifically limited, It is determined in the range of 300-900 rpm.

The process of forming the Taylor vortex in the solution according to the rotational movement of the inner cylinder 12 is shown in FIG. This allows the flow of fluid in the reactor to be characterized as vortex cells that are arranged periodically along the axis of the inner cylinder 12. For example, when the fluid flows between the inner cylinder 12 and the reaction tank 11, the inner cylinder 12 rotates, so that the fluid near the rotor is moved toward the fixed reactor 11 by the centrifugal force. Have. This causes the fluid layer to become unstable, forming a Taylor vortex. The vortex region appears when the rotor speed is above the threshold. Each flow element consists of an annular vortex pair that rotates in opposite directions, and the axial length of each cell is approximately equal to the distance between the inner cylinder 12 and the outer reactor 11. Therefore, the reactor according to the present invention will each have the same volume and residence time.

As described above, in the reaction apparatus of the present invention, by using the Taylor vortex, the flow is very regular and uniformly mixed, and the temperature distribution is uniform in all regions, thereby showing uniform particle size. In addition, due to the many projections formed on the inner cylinder, it is possible to fundamentally block the formation of the scale.

In the embodiment of the present invention preferably, the inner cylinder 12 installed inside the reactor 11 has a cylindrical shape, but in addition to providing sufficient surface area for crystallization while being able to efficiently perform heat transfer. If possible, it is not limited to this. Therefore, if the purpose of the production of macromolecules, the shape of the inner cylinder 12 may have a tapered shape, or a plurality of cylinders of different diameters may have a shape connected in series in decreasing diameter.

In addition, the above embodiment is described that the inner cylinder 12 is rotated by an external rotary motor (not shown), but is not limited thereto, and conversely, the reaction tank 11 is also implemented by rotating the external rotary motor. The effect can be obtained.

The control of the reaction temperature can be adjusted through the control of the amount of heat supplied by the heat supply unit 16 installed in the reaction tank (11). Preferably, the heat supply unit 16 may be implemented in the form of a jacket. The reaction temperature for the crystallization reaction of the present invention is not particularly limited, but is preferably maintained uniformly in the range of 20 ~ 80 ℃.

By the above process, lithium carbonate is synthesized by gas-liquid or liquid-liquid reaction by reactants uniformly mixed, and the crystals of lithium carbonate are precipitated by raising the pH to about 10.5 to 10.8. The crystal of lithium carbonate obtained as described above is discharged through the outlet 15, it is transmitted to the solid-liquid separator 20 can be obtained crystals of lithium carbonate purified with high purity.

Solvents other than the crystals of lithium carbonate separated by the solid-liquid separator 20 are recovered in the distillation column 30, respectively.

Hereinafter, the present invention will be described in more detail with reference to examples. However, the following illustrated examples are only presented to aid the understanding of the present invention and should not be construed as limiting the scope of the present invention.

Example 1 Preparation of Lithium Carbonate by Gas-Liquid Reaction

In accordance with the reaction conditions shown in Table 1 by using the following reaction formula, each raw material was added to the Kuet-Taylor reactor of FIG. 1, the reaction proceeded at pH 7.0 to 8.5, and the pH was raised to 10.5 to 10.8 to obtain high purity carbonic acid. Lithium crystals were recovered (Table 1, FIG. 4).

Scheme 1: 2LiCl + 2NaOH + CO 2 → LiCO 3 + 2NaCl + H 2 O

Throughput 9300 mL / hr Reaction time 5 minutes output 401.50 g / hr Recovery rate 81% Li injection concentration 0.2719 M / min CO 2 0.4464 M / min 50% NaOH 0.3200 M / min

Example 2 Preparation of Lithium Carbonate by Liquid Solution Reaction

In accordance with the reaction conditions shown in Table 2, using the following reaction formula, each raw material was added to the Kuet-Taylor reactor of FIG. 1, the reaction proceeded at pH 7.0 to 8.5, and the pH was raised to 10.5 to 10.8 to obtain high purity carbonic acid. Lithium crystals were recovered (Table 2, Figures 5, 6).

Scheme 2: 2LiCl + Na 2 CO 3 → LiCO 3 + 2NaCl

Throughput 990 mL / hr Reaction time 30 minutes output 39.885 g / 30 minutes Recovery rate 75% Li injection concentration 0.0479 M / min 30% Na 2 CO 3 0.0265 M / min

The method for producing lithium carbonate by the continuous process according to the present invention was confirmed that the production of about 10 times in the case of gas-liquid reaction and about 2.8 times in the case of liquid-liquid reaction compared to the case of using a conventional batch reactor.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. It can be understood that

11: Reactor
12: rotor
13, 14: reactant inlet
15: product outlet
16: heat supply
17: internal space of the reactor
18, 19: turning

Claims (7)

A reaction tank having an inlet and an outlet of a reaction raw material and having an internal reaction space in which a crystallization reaction occurs; And an inner cylinder located in the inner space of the reactor and having protrusions formed on the surface at predetermined intervals. The method of claim 1,
Crystallization reactor, characterized in that the projections formed on the inner surface of the reactor at a predetermined interval. Injecting a liquid lithium salt and a gaseous carbon dioxide, or a liquid lithium salt and a liquid sodium carbonate into the reactant inlet as a reactant in the crystallization reactor according to claim 1; Rotating the rotor to form a Taylor vortex in the reactant introduced to perform a crystallization reaction; And separating the high-purity lithium carbonate by solid-liquid separation of the solution from the outlet of the crystallization machine. The method of claim 3, wherein
The method for producing lithium carbonate using a crystallization reaction device, characterized in that the pH of the reaction of the formation of lithium carbonate. The method of claim 1,
Crystallization reaction of lithium carbonate is a method for producing lithium carbonate using a crystallization reactor, characterized in that carried out at pH 10.5 to 10.8. The method of claim 1,
The reactant is a method of producing lithium carbonate using a crystallization reactor, characterized in that the injection is divided into a plurality of inlet formed in the Kuet-Taylor crystallization. The method of claim 3, wherein
A method for producing lithium carbonate using a crystallization reaction apparatus, characterized in that the carbon dioxide is injected into NaOH or LiCl and T-tube at the same time to the reactant inlet.
KR1020110096233A 2011-09-23 2011-09-23 Crystallization reaction apparatus and preparation method of high purity lithium carbonate KR20130032563A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016060310A1 (en) * 2014-10-14 2016-04-21 주식회사 엘지화학 Method for producing core-shell laminated particles using continuous couette-tayler crystallizer
EP3010074A4 (en) * 2013-06-14 2017-01-04 Laminar Co., Ltd. Device for preparing core-shell particles and method for preparing core-shell particles by using same
WO2018043881A1 (en) * 2016-09-05 2018-03-08 포스코 Method for preparing lithium chloride and method for preparing lithium carbonate
WO2018043882A1 (en) * 2016-09-05 2018-03-08 주식회사 포스코 Method for preparing lithium chloride and method for preparing lithium carbonate
US10347913B2 (en) 2014-10-14 2019-07-09 Lg Chem, Ltd. Method for preparing core-shell structured particle by using continuous Couette-Taylor crystallizer
CN111790331A (en) * 2020-07-29 2020-10-20 贵州微化科技有限公司 Relative motion annular gap micro-reactor
CN113058285A (en) * 2021-05-19 2021-07-02 青海民族大学 A device for following extract lithium carbonate crystallization in salt lake brine
WO2023056676A1 (en) * 2021-10-09 2023-04-13 安徽大学绿色产业创新研究院 Method for preparing lithium carbonate with uniform particle size distribution by means of low-temperature homogenization
CN117299002A (en) * 2023-11-29 2023-12-29 崇义绿冶新能源有限公司 Lithium bicarbonate pyrolysis device for preparing lithium carbonate

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3010074A4 (en) * 2013-06-14 2017-01-04 Laminar Co., Ltd. Device for preparing core-shell particles and method for preparing core-shell particles by using same
US10601035B2 (en) 2013-06-14 2020-03-24 Posco Method of preparing core-shell particles
WO2016060310A1 (en) * 2014-10-14 2016-04-21 주식회사 엘지화학 Method for producing core-shell laminated particles using continuous couette-tayler crystallizer
US10347913B2 (en) 2014-10-14 2019-07-09 Lg Chem, Ltd. Method for preparing core-shell structured particle by using continuous Couette-Taylor crystallizer
WO2018043881A1 (en) * 2016-09-05 2018-03-08 포스코 Method for preparing lithium chloride and method for preparing lithium carbonate
WO2018043882A1 (en) * 2016-09-05 2018-03-08 주식회사 포스코 Method for preparing lithium chloride and method for preparing lithium carbonate
CN111790331A (en) * 2020-07-29 2020-10-20 贵州微化科技有限公司 Relative motion annular gap micro-reactor
CN113058285A (en) * 2021-05-19 2021-07-02 青海民族大学 A device for following extract lithium carbonate crystallization in salt lake brine
WO2023056676A1 (en) * 2021-10-09 2023-04-13 安徽大学绿色产业创新研究院 Method for preparing lithium carbonate with uniform particle size distribution by means of low-temperature homogenization
CN117299002A (en) * 2023-11-29 2023-12-29 崇义绿冶新能源有限公司 Lithium bicarbonate pyrolysis device for preparing lithium carbonate
CN117299002B (en) * 2023-11-29 2024-03-19 崇义绿冶新能源有限公司 Lithium bicarbonate pyrolysis device for preparing lithium carbonate

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