WO2014084547A1 - 혼합용 반응 장치 및 이 반응 장치를 이용한 제조 방법 - Google Patents
혼합용 반응 장치 및 이 반응 장치를 이용한 제조 방법 Download PDFInfo
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- WO2014084547A1 WO2014084547A1 PCT/KR2013/010605 KR2013010605W WO2014084547A1 WO 2014084547 A1 WO2014084547 A1 WO 2014084547A1 KR 2013010605 W KR2013010605 W KR 2013010605W WO 2014084547 A1 WO2014084547 A1 WO 2014084547A1
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- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/51—Methods thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
- B01F27/272—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/22—Control or regulation
- B01F35/221—Control or regulation of operational parameters, e.g. level of material in the mixer, temperature or pressure
- B01F35/2215—Temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
- B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
- B01F35/7176—Feed mechanisms characterised by the means for feeding the components to the mixer using pumps
- B01F35/717614—Venturi pumps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/71—Feed mechanisms
- B01F35/717—Feed mechanisms characterised by the means for feeding the components to the mixer
- B01F35/71805—Feed mechanisms characterised by the means for feeding the components to the mixer using valves, gates, orifices or openings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/80—Forming a predetermined ratio of the substances to be mixed
- B01F35/88—Forming a predetermined ratio of the substances to be mixed by feeding the materials batchwise
- B01F35/882—Forming a predetermined ratio of the substances to be mixed by feeding the materials batchwise using measuring chambers, e.g. volumetric pumps, for feeding the substances
- B01F35/8821—Forming a predetermined ratio of the substances to be mixed by feeding the materials batchwise using measuring chambers, e.g. volumetric pumps, for feeding the substances involving controlling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F35/92—Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
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- 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
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F2035/98—Cooling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F2035/99—Heating
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- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
- B01J2208/00212—Plates; Jackets; Cylinders
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- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00539—Pressure
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00162—Controlling or regulating processes controlling the pressure
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00761—Details of the reactor
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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
- H01M4/52—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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Definitions
- the present invention relates to a reaction apparatus, and more particularly, to a reaction apparatus capable of mixing a solid phase-liquid or gas phase-liquid using a vortex vortex.
- the reactor In the conventional gas hydrate reactor, water and gas are supplied from the water supply unit and the gas supply unit, and water and gas supplied from the mixing chamber are first mixed and then introduced into the reactor.
- the reactor is somewhat different depending on the gas hydrate formation conditions but should generally be formed in an atmosphere of high pressure and low temperature.
- the pressure inside the reactor is adjusted by the supply of gas, and the temperature is controlled by adjusting the temperature of the water bath. In particular, the temperature of the water bath must be significantly lower for low temperature maintenance.
- a stirrer may be used to promote the formation of gas hydrates, and the formed gas hydrates are stored in the gas hydrate storage unit.
- the conventional gas hydrate reactor as described above has the following problems. That is, in the conventional gas hydrate reactor, since the reactor is located in the water bath, accurate and rapid temperature control of the space inside the reactor in which the gas hydrate is generated is very difficult. The water is filled in the water bath, which is difficult to control precisely by the thermodynamic inertia of the water, and the temperature inside the reactor is indirectly affected by the water bath temperature even when the temperature of the water in the domestic water bath is precisely controlled. It does not lead to fast and accurate temperature control.
- the inside of the reactor must be maintained at a high pressure in accordance with the gas hydrate generation conditions, the problem that it is not easy to inject gas into the reaction of the high pressure, the rate of gas hydrate production rate due to the speed of gas and water reaction is not fast There is also a problem that is slowed down.
- the present invention has been made in view of such a conventional problem, and can perform a compression function without the configuration of expensive boosting means, thereby simplifying the configuration, smoothly injecting gas and water, and using a taylor flow.
- micromixing to improve the production rate of the gas hydrate as well as to provide a reactor for producing a gas hydrate continuously.
- Another object of the present invention by using a Taylor flow, it is possible to simply and easily obtain a good yield reactant through a series of processes in the mixing and reaction of the solid material and the solution, and also shorten the reaction time compared to the existing
- the present invention provides a reactor for mixing solid-liquid materials.
- the present invention includes a first and a second reactant accommodating parts, each containing a reactant in a solid phase, a gas phase, or a liquid phase; A pressure pump for pumping a reactant contained in any one or each of the first and second receiving parts; And a reactor for mixing reactants fed from the pump, wherein the reactor has a reaction chamber in which reactants are accommodated, and each of the first and second reactant receiving parts is connected to one upper part and one lower part of the reactor.
- a cylinder with a port And a stirring shaft rotatably installed in the cylinder to stir the reactants supplied from the first and second reactant accommodating parts and a stirring motor to provide a rotational force to the stirring shaft.
- the present invention can easily compress the reactants such as, for example, gas hydrate to an appropriate pressure by means of a pressure pump and a pressure control valve respectively installed at the injection port side of the reactor, and at the same time easily mix the gas and water constituting the gas hydrate. It has the advantage to do it.
- the components of the reactants such as gas and water can be easily injected into the high-pressure reactor, and the pressure control valve is used to easily boost the pressure inside the reactor.
- reaction time is shortened in mixing and reacting the solid material and the solution, it is possible to easily and quickly obtain a reactant having a uniform size distribution to produce an excellent product with high productivity Can be.
- FIG. 1 is a cross-sectional view showing an example of a reactor applied to the reaction apparatus of the present invention
- FIG. 2 is a block diagram showing the overall configuration of a reaction apparatus according to the present invention.
- FIG. 3 is a cross-sectional view of a reactor of another embodiment applied to the reaction apparatus of the present invention.
- Figure 4 is a block diagram showing the overall configuration of a reactor according to another embodiment of the present invention.
- Figure 5 is a cross-sectional view of a reactor of another embodiment applied to the reaction apparatus of the present invention.
- FIG. 6 is a manufacturing process diagram of a cathode active material for a lithium secondary battery using the reactor of FIG. 5.
- the present invention provides the first and second reactant accommodating parts (10) and (30), each of which contains a reactant of any one of solid, liquid, and gaseous phases, and the reactant accommodated in any one or each of the first and second accommodating parts.
- a cylinder 510 having injection ports 512 and 513 connected to the first and second reactant accommodating parts, respectively;
- a stirring shaft 520 rotatably installed in the cylinder 510 to stir the reactants supplied from the first and second reactant accommodating parts and a stirring motor 530 to provide a rotational force to the stirring shaft 520; Provide what is configured.
- the reaction apparatus of the present invention may be composed of a reactant supply means consisting of a reactant accommodating part and a pump, a reactor, and post-treatment means for post-treating the mixture passed through the reactor.
- a reactant supply means consisting of a reactant accommodating part and a pump
- a reactor and post-treatment means for post-treating the mixture passed through the reactor.
- a supply means, a reactor, and a post-treatment means are provided according to respective characteristics.
- a first embodiment of the present invention is a reaction apparatus for producing a gas hydrate.
- the reaction apparatus includes a first reactant accommodating part 10, a first reactant pressure pump 20, a second reactant accommodating part 30, and a first reactant.
- 2 includes a reactant pressure pump 40, a reactor 50, and as a weight treatment means, includes a water removal part 60 and a dryer (70).
- the first reactant accommodating part 10 When the first reactant accommodating part 10 is used to prepare a gas hydrate as in the present invention, the reactant of any one of water and gas is stored. When gas is contained in the first reactant accommodating part 10, airtightness is essential to prevent gas leakage.
- the first reactant pump 20 functions to pump the first reactant in the first reactant accommodating part 10 at a high pressure and press it into the reactor 500.
- the pump 20 for pumping the first reactant preferably has a pressure pressure in the range of 2 atm or more, but preferably has a pressure pressure in the range of 5 to 50 bar.
- the pump 20 for pumping the first reactant preferably has a pressure pressure in the range of 2 atm or more, but preferably has a pressure pressure in the range of 5 to 50 bar.
- water When gas is contained in the first reactant accommodating part 10, water may be stored in the second reactant accommodating part 30.
- one phase of a solid phase, a gas phase, or a liquid phase may be selectively stored in the first reactant accommodating part 10, but only a liquid phase is stored in the second reactant accommodating part 30.
- the pump 40 for pumping the second reactant is the same as or similar to the pump 20 for pumping the first reactant.
- a first backflow check valve 100 and a second backflow Prevention valve 110 may be installed respectively.
- Each of the non-return valves 100 and 110 prevents the reactants from flowing backward, and constitutes a one-way valve (check valve).
- the reactor 50 of the present invention includes a cylinder 510, a stirring shaft 520, a stirring motor 530, and a pressure control valve 540.
- the cylinder 510 has a reaction chamber 511 in which the first and second reactants are press-mixed together, and one of the first and second reactants is press-fitted into the reaction chamber 511 at an upper side thereof.
- a first injection port 512 is formed to be formed, and a second injection port 513 for inputting the other one of the first and second reactants is formed at one lower side thereof, and the first and second reactants are formed at the other side thereof.
- One discharge port 514 is formed through which a mixture of constituent factors mixed with each other is discharged.
- the first and second injection ports 512 and 513 are preferably in the form of a venturi tube formed such that its inner diameter d gradually decreases from the outside to the inside of the reactor 50.
- the reason for having such a shape is to help the first and second reactants introduced through the respective injection ports 512 and 513 to flow into the reaction chamber 511 more smoothly. If the diameter of) gradually narrows, the flow rate is increased by Bernoulli's theorem, so that each reactant can be introduced more smoothly.
- the stirring shaft 520 is rotatably installed in the cylinder 510 to be horizontally installed horizontally like the cylinder 510 to stir the first and second reactants.
- the stirring motor 530 may be directly connected to the stirring shaft 520 or indirectly.
- the belt pulley 550 and the belt which interconnect one end of the shaft 531 and the stirring shaft 520 of the stirring motor 530 so that the power of the stirring motor 530 is transmitted to the stirring shaft 520. 560 may be further configured.
- the pressure control valve 540 is installed on the outlet 514 serves to adjust the pressure inside the reaction chamber 511. That is, the pressure control valve 540 controls the pressure in the reaction chamber 511 by adjusting the opening and closing degree of the outlet 514, for example, if the opening degree of the pressure control valve 540 is reduced or closed. The pressure inside the reaction chamber 511 is increased, and when the opening degree of the pressure control valve 540 is relatively increased, the pressure inside the reaction chamber 511 is decreased.
- the reactor 50 if the reactants are gas hydrate, may be slightly different depending on the forming conditions, but generally should be formed in a high pressure and low temperature atmosphere.
- the pressure inside the high pressure reactor 50 is adjusted by the supply of gas, and the temperature is achieved by the cooling chamber 515.
- the reactor 50 may form a cooling chamber 515 in which the refrigerant is circulated outside the reaction chamber 511 to control the reaction temperature of the first and second reactants in the reaction chamber 511 at a low temperature. It was made.
- the reactor 50 injects the first and second reactants for mixing into the reaction chamber 511 through the first and second injection ports 512 and 513, but the first reactant is configured in the first injection port 512.
- the printing pumping pump 200 is connected to the first reactant is press-fitted, the second injection port 513 is connected to the pump 400, the second reactant is press-fitted, the discharge port 514 of the reaction chamber 511
- the pressure control valve 540 By controlling the opening and closing degree by the pressure control valve 540, the pressure inside the reaction chamber 511 is increased to compress the reactant constituent factors.
- the reactant constituents in the reaction chamber 511 is formed in accordance with the rotation of the stirring shaft 520, when the angular velocity of the stirring shaft 520 is slow, the laminar Taylor flow is generated, while the angular velocity is As the reactant constituents increase along the inner circumferential surface of the reaction chamber 511, the reactant constituents become unstable and a Taylor vortex occurs above a certain threshold speed. Taylor vortices are arranged in a very regular annular shape in the axial direction and rotate in opposite directions so that they do not mix in the axial direction, leading to uniform mixing.
- the stirring motor 530 is a variable speed motor, the speed can be adjusted, thereby easily controlling the rotation speed of the stirring shaft 520 to control the size of the particles by controlling the shear stress applied to the reactant components during the reaction time.
- This easy and high-speed rotation is possible compared to the stirring method, so that a large shear stress can be transmitted and the reaction time can be shortened.
- the same method can be applied to the batch reactor, of course.
- the water removal part 60 is installed on the outlet 514 side through which the mixed and compressed reactants in the high pressure reactor 50 are discharged, and serves to remove water contained in the reactants discharged from the high pressure reactor 50.
- a centrifugal dehydrator or concentrator may be applied to separate the filtrate from the slurry in the form of a reactant.
- the centrifugal dehydrator is a slurry-type reactant into a dehydration tank perforated with a plurality of micropores in the periphery, the water is discharged through the micropores by centrifugal force by rotating the dehydration tank at high speed, the moisture inside the dehydration tank Only the reactants in this removed state remain.
- Dryer 70 is installed on the discharge side of the water removal part 60 serves to completely dry the reactants in the water is removed, the reaction product is complete the water removal by the water removal part 60 then Since the water content is high even, for example, by blowing hot air to the reactants with a hot air dryer, the water content can be attenuated to 10% or less to obtain a high purity reactant.
- the grinding part 80 is installed on the discharge side of the dryer 70 may be further installed to finely grind the dried reaction material to a desired size.
- the grinding part 80 is, for example, installed two grinding screws facing each other, the grinding screw is rotated in the reverse direction, when the reaction material is introduced between the two grinding screws between the two grinding screws. It may take a configuration such that the mixture is crushed.
- the reaction apparatus of the present invention is for mixing the liquid-solid phase, in particular for the production of electronic paper, i.e. coating the nanoparticles to have excellent mobility without agglomeration in the microcapsule, furthermore To shorten the reaction time.
- the reaction apparatus for mixing solid-liquid materials of the present invention includes a solid material accommodating part 10 and a solid material weighing part corresponding to the first reactant accommodating part according to the order of the reaction process. 200, a feeder 300, a solution receiving part 30 corresponding to the second reactant accommodating part, a delivery pump 40, a reactor 50, a water removal part 60, and a dryer 70.
- the first embodiment differs from the first embodiment in that the reactant contained in the first reactant accommodating part is a solid material, includes a metering part, and a feeder corresponding to the pump.
- the solid material receiving part 10 of the components serves to store the solid material in powder form.
- the solid material accommodating part 10 may be applied in various forms such as a tank or a hopper.
- the solid material mooring part 200 serves to measure the amount of the solid material discharged automatically or manually from the solid material accommodating part 10 to the feeder 300 by measuring the set amount.
- the solid material metering part 200 may be, for example, a load cell, but is not limited thereto.
- the solid matter metering part 200 may control electronically the metered value of the solid matter by the control part 90.
- the feeder 300 serves to automatically supply the solid matter measured in the solid material accommodating part 10 to the reactor 50, a belt conveyor, a rotary type (watermill type), a screw type, and the like. It can be applied in the form.
- the solution receiving part 30 serves to store a liquid solution.
- the solution receiving part 30 may be configured in the form of a tank or a hopper, such as the solid material receiving part 10 above.
- the pump 40 serves to inject the solution in the solution receiving part 30 into the reactor 50 to be proportional to the amount of solid matter.
- a flow control valve 130 may be installed between the pump 40 and the mixing reactor 50 to control the flow rate of the solution.
- the flow control valve 130 is preferably configured to be electronically controlled to be electrically controlled automatically by the above-described control part 90 so that the supply amount of the solid material and the supply amount of the solution is proportionally controlled.
- Reactor 50 like the reactor described above, utilizes a Taylor fluid flow, and by this principle serves to mix the solution between the solid materials.
- the reactor 50 has a reaction chamber 511 in which the solid material and the solution are accommodated together, and a solid material injection port for injecting the solid material into the reaction chamber 511 on one side of the reactor 50.
- 512 is formed, and has a horizontal cylinder 510 each formed with a solution injection port 513 for injecting the solution on the lower side.
- the reactor 50 has a horizontal stirring shaft 520 rotatably installed in the cylinder 510 to stir the solid material and the solution so that the solution is mixed between the particles of the solid material.
- the reactor 50 has a stirring motor 530.
- the stirring motor 530 may be directly connected to the stirring shaft 530 or indirectly.
- the belt pulley 540 interconnecting one end of the shaft 531 and the stirring shaft 520 of the stirring motor 530 so that the power of the stirring motor 530 is transmitted to the stirring shaft 520.
- the belt 550 may be further configured.
- the reactor 50 of this configuration is injected into the reaction chamber 511 through the solid material injection port 512 and the solution injection port 513 for mixing, and the stirring shaft 520 is rotated Flow is formed. That is, when the angular velocity of the stirring shaft 520 is slow, a laminar Taylor flow is generated, while the angular velocity increases, the fluid becomes unstable due to the tendency of the fluid to follow the inner circumferential surface of the reaction chamber 511 and a specific critical velocity. Taylor vortex is generated in the above. Taylor vortices are arranged in a very regular annular shape in the axial direction and rotate in opposite directions so that they do not mix in the axial direction, leading to uniform mixing.
- the solid material may be a polymer, a metal, a metal oxide, or the like.
- the stirring motor 530 is a variable speed motor, the speed can be controlled, so that the size of the particles can be easily controlled by easily controlling the rotational speed of the stirring shaft 520 to control the shear stress applied to the reactants during the reaction time.
- high-speed rotation is possible, so that a large shear stress can be transmitted and the reaction time can be shortened.
- a filling chamber 514 in which a heat medium is filled is provided outside the reaction chamber 511 and the reaction chamber 511 is provided.
- the temperature sensor 560 and the temperature sensor 560 for sensing the internal temperature of the heating medium filling chamber 514 or the reaction chamber 511 for the accuracy and automation of temperature control It may further include a temperature control unit 570 for controlling the temperature, such as to sense the detected temperature data in real time to increase or decrease the temperature or maintain a constant temperature.
- oil is applied at 100 ° C. or higher, and water is applied at 100 ° C. or lower.
- the heat medium filling chamber 514 increases the temperature in the reaction chamber 511 to partially evaporate the moisture mixed in the reactant.
- the water removal part 60 is installed to be connected to the discharge side from which the mixed reactants in the mixing reactor 50 are discharged, and serves to remove moisture contained in the reactants discharged from the mixing reactor 50.
- a centrifugal dehydrator or concentrator may be applied to separate the filtrate from the reactants in the form of a slurry.
- the centrifugal dehydrator puts a slurry-type reactant into a dehydration tank in which a plurality of micropores are periphery, and then discharges water through the micropores by centrifugal force as the dehydration tank is rotated at high speed. This removes the reactants.
- the concentrator is to condense by evaporating the water in the reactant, and after adding the reactant to the heating furnace, by heating the heating furnace to the appropriate temperature, only the concentrated reactant remains by forcibly evaporating the moisture contained in the reactant. Device.
- Dryer 70 is installed on the discharge side of the water removal part 60 serves to completely dry the reactants in the water is removed, the reaction product is complete the water removal by the water removal part 70 then Since the water content is high even, for example, hot air is blown to the reactants by a hot air dryer, thereby attenuating the water content to 10% or less, thereby obtaining a high purity reactant.
- the grinding part 110 is installed on the discharge side of the dryer 70 may be further installed to finely grind the dried reaction material to a desired size.
- the grinding part 110 is, for example, installed two grinding screws facing each other and the grinding screw is rotated in opposite directions to each other, when the reaction material is introduced between the two grinding screws between the two grinding screws. It may take a configuration such that the mixture is crushed.
- the reaction apparatus of the present invention can be used to manufacture a cathode active material for a lithium secondary battery.
- the configuration of the reactor is the same as that described above, except that three supply means are provided, and a separator 300 and a dryer 70 are provided in the post-treatment means.
- the reaction furnace 500a which is a non-rotating body having a reaction chamber 511 therein;
- a stirring motor 530 disposed on one side of the reactor 500a;
- Reactor coupled to the motor shaft 531 of the stirring motor 530, the reactor having a stirring shaft 520 embedded in the reaction chamber 511, spaced apart from the wall surface of the reaction chamber 511 It includes.
- One or more reactant injection ports 512 and 513 formed in communication with the reaction chamber 511 and the reaction product discharge port 514 formed in communication with the reaction chamber 511 to discharge the reaction products are provided. Includes; A plurality of spare ports 516 are provided between the injection ports 512 and 513 and the reaction product discharge port 514 to communicate with the reaction chamber 511.
- an outer side of the reaction chamber 511 is provided with an annular filling chamber 515, the filling chamber 151 is filled with hot water 517, the flow path of the reactant injection ports 512, 513
- a particle crushing unit 600 which is installed at and grinds particles of the reactant injected through the reactant injection port; Is installed in at least one of the reactant injection port, the reaction product discharge port, the extra port 516 connected to the filling chamber 515 is a flow rate sensor 610 for detecting the flow rate of the reactant and the flow rate sensor 610 It may be configured to further include a flow rate control unit 620 for controlling the flow rate of the reactants flowing through the reactant injection port (512, 513) by the flow rate detection data fed back by).
- the injection ports 512 and 513 of the reaction apparatus include a plurality of reactant receiving parts 10a, 10b and 10c connected through respective connection lines L1, L2 and L3; Each supply pump is installed on each connection line (L1, L2, L3) for pumping the reactants in each of the reactant accommodating parts (10a.
- the dryer 70 may further include a dryer 70 for drying the cathode active material separated from the cathode active material separator 300.
- the first step is the reactant filling step.
- First to third reservoir tanks constituting the reactant accommodating parts (10a, 10b, 10c) are connected to the reactor, the first reservoir tank is nickel sulfate (NiSO 4 ), manganese sulfate (MnSO 4 ) and cobalt sulfate (COSO 4 ) is filled with an aqueous metal solution mixed in a molar ratio of 1: 1: 1 or 5: 2: 3, 5: 3: 2, 7: 2: 1.
- the second reservoir tank and the third reservoir tank are filled with ammonia gas (NH 3 ) and sodium hydroxide (NaOH), respectively.
- NH 3 ammonia gas
- NaOH sodium hydroxide
- concentration and, as for the density
- the second step is a reactor setting step.
- the internal pressure of the chamber formed inside the reactor is set to 1 to 2 bar, and the ambient temperature of the reactor is maintained at room temperature to 80 ° C. by the filling chamber.
- the internal pressure is a range for obtaining an optimized reaction effect by applying an appropriate pressure to the reactants introduced into the chamber, the chamber atmosphere temperature is difficult to obtain a high-density complex hydroxide because the produced cobalt hydroxide precipitates in complex salt form at a low temperature Because.
- the third step is the reactant input step. That is, the pump is installed at the outlet side of the first reservoir tank and the third reservoir tank, and the electromagnetic side or the manual side is installed at the outlet side of the second reservoir tank, and the liquid contents of the first and third reservoir tanks operate the pump. As a result, the feed pipe is introduced into the reactor, and the gaseous contents of the second reservoir tank are introduced into the chamber through the connection line according to the opening of the valve (electromagnetic valve or manual valve).
- a pH sensor is installed at the inlet of the chamber into which the reactant is introduced to detect the hydrogen ion concentration of the reactant, and when the detected hydrogen ion concentration value (pH) is lower than the set hydrogen ion concentration value, sodium hydroxide is detected.
- the hydrogen ion concentration is controlled by blocking the addition of sodium hydroxide.
- a suitable hydrogen ion concentration value (pH) is 10.8 to 12.5.
- the fourth step is a chemical reaction step. That is, the chemical reaction between the gas-liquid reactants introduced by holding and agitating the aqueous metal solution, ammonia gas, and sodium hydroxide introduced into the chamber by at least one rpm (preferably 100 to 1500 rpm) for 30 minutes or more by rotating the stirring shaft Let this happen.
- the chamber is hermetically sealed, gas phase-liquid reaction is possible.
- the gas is difficult to stay because the gas leaks to the outside. Therefore, gas-liquid liquid reaction is impossible.
- Table 1 below compares the conventional batch reactor with the gas phase-liquid reactor of the present invention.
- the gas-liquid phase reactor showed better characteristics than the batch reactor as a whole. Therefore, the method of manufacturing a cathode active material of the present application using a gas phase-liquid reactor is higher in efficiency than the conventional one, and a gas phase-liquid phase reaction is possible.
- the use of ammonia gas can further obtain effects such as energy density and waste liquid reduction.
- the fifth step is a discharge step. That is, when the chemical reaction between the reactants is completed, the reaction product in the form of slurry is discharged through the discharge port of the reactor.
- Step 6 is a separation step. That is, since the discharged reaction product contains water, the positive electrode active material and the filtrate are separated by dehydration by a dehydrator such as a separator or a dehydrator.
- a dehydrator such as a separator or a dehydrator.
- the present invention uses ammonia gas instead of ammonia water, the amount of the filtrate is significantly reduced compared to the conventional. Since the filtrate is a waste liquid to be disposed of, it is possible to improve the environmental friendliness of the process by reducing the amount of such waste liquid.
- the seventh step is a drying step. That is, the positive electrode active material recovered in step 6 is dried at 110 ° C to 130 ° C for at least 24 hours by a drying apparatus to obtain a powdery cathode active material.
- the eighth step is a particle size measurement step. That is, as a step of measuring the particle size distribution and the size of the powdery positive electrode active material using a scanning electron microscope, the average particle size of the positive electrode active material was measured to be uniformly distributed in a fine size of 8 ⁇ m or less. As the ammonia water was changed to ammonia gas, the particle size was smaller than before, and the small particle size had an improved effect on the density of the distribution. Therefore, when used in a lithium secondary battery has a subsequent effect of improving the life of the battery.
- the mixing reaction device may selectively mix reactants in a solid phase, a liquid phase, and a gas phase, and apply pressure to complete a product.
- the positive electrode active material for lithium secondary batteries, gas hydrate, as well as can be used in the manufacture of electronic paper.
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Abstract
Description
구분 | 회분식 반응기 | 기상-액상 반응기 |
유체 혼합 방식 | 거대 혼합(macro-mixing) | 미세혼합(micro-mixing) |
생산공정 | 비연속식 | 연속식 |
물질전달속도(m/s) | 1 | 3.3 |
교반강도(w/kg) | 0.8 | 5.8 |
공정시간(h) | 12~24 | 3~6 |
입자분포(CV%) | 30~50 | 20이내 |
Claims (12)
- 고상, 기상, 액상 중 어느 하나로 된 반응물이 수용되는 하나 또는 그 이상의 반응물 수용 파트;상기 반응물 수용 파트 중 하나 또는 각각에 수용되는 반응물을 압송하는 압송 펌프;상기 압송 펌프에서 압송된 반응물을 혼합하는 반응기;를 포함하며,상기 반응기는 내부에 반응물이 수용되는 반응 챔버를 가지며, 일측 상부와 하부 각각에 상기 반응물 수용 파트 각각이 연결되는 주입 포트가 구비된 실린더;상기 실린더 내에 회전 가능하게 설치되어 상기 반응물 수용 파트에서 공급된 반응물을 교반하는 교반축 및 상기 교반축에 회전력을 제공하는 교반 모터;로 구성된 것을 포함하는 혼합용 반응 장치.
- 제 1항에 있어서, 상기 반응기와 압송 펌프 사이에 역류방지밸브가 구비된 것을 더 포함하는 혼합용 반응 장치.
- 제 1항에 있어서, 상기 제 1 반응물 수용 파트에 고상의 반응물이 수용되고, 상기 제 1 반응물과 반응기 사이에, 고상의 반응물을 계량하여 공급하는 계량 파트와, 반응물을 반응기에 공급하는 피더가 구비되며,상기 제 2 반응물 수용 파트와 반응기 사이에, 펌프와 유량제어밸브가 더 구비된 것을 포함하는 혼합용 반응 장치.
- 제 3항에 있어서, 상기 계량 파트는 로드셀인 것을 포함하는 혼합용 반응 장치.
- 제 3항에 있어서, 상기 계량 파트는 계량 정도를 전자적으로 제어하는 제어 파트를 더 포함하는 혼합용 반응 장치.
- 제 1항에 있어서, 상기 송출 펌프와 반응기 사이에, 구비되는 유량제어밸브를 더 포함하되, 상기 유량제어밸브는 제어파트에 의해 그 개폐 정도가 전자적으로 제어되는 것을 포함하는 혼합용 반응 장치.
- 제 1항에 있어서, 상기 반응에서 혼합된 반응물이 배출되는 배출 측에 설치되어 반응기로부터 배출되는 반응물에 포함된 수분을 제거하는 수분제거파트를 더 포함하는 혼합용 반응 장치.
- 제 7항에 있어서, 상기 수분제거파트는 원심 탈수기, 농충기 중 어느 하나인 것을 포함하는 혼합용 반응 장치.
- 제 1항에 있어서, 상기 주입 포트는 상기 반응기의 외부로부터 내부를 향할 수록 적어도 그 내경이 점차적으로 작아지는 벤츄리관 형태로 된 것을 포함하는 혼합용 반응 장치.
- 제 1항에 있어서, 상기 반응 챔버의 외곽에 열매체 또는 냉매가 순환하는 충진 챔버가 구비되어, 반응 챔버 내의 반응 온도를 하향 또는 상향 제어할 수 있도록 하는 것을 더 포함하는 혼합용 반응 장치.
- 제 1항에 있어서, 상기 반응기의 배출구 상에 챔버의 내부 압력을 조절하는 압력조절밸브가 구비된 것을 포함하는 혼합용 반응 장치.
- 반응기를 이용한 제조방법으로서,상기 반응기와 연결되는 반응물 수용 파트를 제1 ~ 3 리저버탱크로 구성하고, 상기 제1 리저버탱크에는 황산니켈(NiSO4), 황산망간(MnSO4), 황산 코발트(CoSO4)가 동일 또는 상이한 몰비로 혼합된 금속 수용액이 충진되고, 제2 리저버 탱크에는 암모니아 가스(NH3)를 충진하며, 제3 리저버 탱크에는 수산화나트륨(NaOH)을 충진하는 반응물 충진단계;상기 반응기의 내부에 형성된 챔버의 내부 압력과 온도를 유지시키는 세팅단계;상기 제1 리저버탱크 및 제3 리저버탱크의 내용물은 펌프에 의해 펌핑하여 상기 반응로의 내부로 투입하고, 제2 리저버탱크의 내용물은 밸브의 개방에 의해 반응로의 내부로 투입되도록 하는 반응물 투입단계;상기 반응로 내부로 유입된 금속 수용액, 암모니아 가스 및 수산화나트륨을 교반시켜 유입된 기상-액상 반응물 간에 화학적 반응이 일어나도록 하는 화학반응 단계;상기 화학반응이 완료되면 반응로로부터 슬러리 형태의 반응결과물을 배출시키는 배출단계; 및상기 배출된 반응 결과물을 탈수장치에 의해 탈수시켜서 양극 활물질과 여액을 분리하는 분리단계;상기 분리단계 이후에, 상기 양극 활물질을 건조장치에 의해 건조시키는 건조단계;상기 건조단계 이후에, 건조된 양극 활물질의 평균입도를 측정하는 입도 측정단계;상기 반응물 투입단계에서, pH센서에 의해 반응물의 pH(수소이온농도)를 감지하고, 감지된 pH에 따라 수산화나트륨의 투입량을 조절하는 것을 특징으로 하는 혼합형 반응기를 이용한 제조방법.
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JP2015536725A JP6257636B2 (ja) | 2012-11-27 | 2013-11-21 | 混合用反応装置およびこの反応装置を用いた製造方法 |
EP13858740.7A EP2910300A4 (en) | 2012-11-27 | 2013-11-21 | REACTION DEVICE FOR MIXING AND MANUFACTURING PROCESS USING THE REACTION DEVICE |
US14/434,665 US10201797B2 (en) | 2012-11-27 | 2013-11-21 | Reaction device for mixing and manufacturing method using the reaction device |
IL238927A IL238927A0 (en) | 2012-11-27 | 2015-05-20 | Mixing reaction device and production method using the reaction device |
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KR1020120134923A KR101399057B1 (ko) | 2012-11-27 | 2012-11-27 | 고상-액상 물질의 혼합용 반응장치 |
KR10-2012-0134923 | 2012-11-27 | ||
KR10-2012-0156969 | 2012-12-28 | ||
KR1020120156969A KR101364691B1 (ko) | 2012-12-28 | 2012-12-28 | 고압 반응장치 |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109351311A (zh) * | 2018-12-14 | 2019-02-19 | 中国科学院合肥物质科学研究院 | 一种金属硫化物纳米材料合成装置 |
CN109351311B (zh) * | 2018-12-14 | 2023-09-08 | 中国科学院合肥物质科学研究院 | 一种金属硫化物纳米材料合成装置 |
CN109663560A (zh) * | 2019-01-29 | 2019-04-23 | 南通金通储能动力新材料有限公司 | 一种三元正极材料前驱体反应釜 |
CN109663560B (zh) * | 2019-01-29 | 2024-02-02 | 南通金通储能动力新材料有限公司 | 一种三元正极材料前驱体反应釜 |
CN115672196A (zh) * | 2021-07-23 | 2023-02-03 | 中国石油天然气股份有限公司 | 搅动式小颗粒催化剂加注设备 |
Also Published As
Publication number | Publication date |
---|---|
EP2910300A4 (en) | 2016-07-27 |
US10201797B2 (en) | 2019-02-12 |
JP6257636B2 (ja) | 2018-01-10 |
IL238927A0 (en) | 2015-07-30 |
EP2910300A1 (en) | 2015-08-26 |
US20150258524A1 (en) | 2015-09-17 |
JP2016501705A (ja) | 2016-01-21 |
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