CN109539792A - A kind of spray pyrolysis unit preparing tertiary cathode presoma and its application method - Google Patents
A kind of spray pyrolysis unit preparing tertiary cathode presoma and its application method Download PDFInfo
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- CN109539792A CN109539792A CN201811426834.3A CN201811426834A CN109539792A CN 109539792 A CN109539792 A CN 109539792A CN 201811426834 A CN201811426834 A CN 201811426834A CN 109539792 A CN109539792 A CN 109539792A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
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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
- C01G53/04—Oxides; Hydroxides
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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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
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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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
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Abstract
The present invention provides a kind of spray pyrolysis unit for preparing tertiary cathode presoma and its application methods, described device includes the first spray pyrolysis unit and the second spray pyrolysis unit, the first spray pyrolysis unit discharge port connects conveying device, and the outlet of the conveying device is arranged in the cavity of second spray pyrolysis unit.The described method includes: (1) ternary mixing salt solution sprays into the first spray pyrolysis unit, pre-product is generated；(2) pre-product enters the second spray pyrolysis unit, solid gas separation by conveying device, and solid is the tertiary cathode presoma, is handled or is recycled after gas discharge.The present invention ensure that material pyrolysis time sufficient in furnace while reducing device design diameter, reduce the chloride content in product by being connected to two groups of spray pyrolysis unit U-shapeds.It is similar to the pyrolysis effect of large-scale spray pyrolysis unit, and greatly reduce the occupied area of equipment.
Description
Technical field
The invention belongs to lithium battery manufacturing field, it is related to a kind of spray pyrolysis unit and its application method more particularly to one
Kind is used to prepare the spray pyrolysis unit and its application method of tertiary cathode presoma.
Background technique
Lithium ion battery has without containing noxious materials such as lead, cadmium, mercury in new-energy automobile, energy storage, consumer electronics field
It is widely applied.As the scale of lithium ion battery is constantly expanded, the price of related raw material is higher and higher, especially relevant dilute
Resource, such as metallic cobalt are lacked, is held at high price.The rise of cost of material leads to the cost increase of lithium ion battery, to lithium from
The further application of sub- battery adversely affects.Since positive electrode accounts for relatively high, the positive material of reduction in entire battery cost
The processing cost of material and presoma is to reduce the important means of entire battery cost.
Current tertiary cathode presoma mainly passes through Co deposited synthesis, and process flow is complicated, and time-consuming, while in life
A large amount of ammonia nitrogen waste water can be generated during production, is handled, and biggish environmentally friendly cost is generated.Spray pyrolysis preparation three
First anode presoma process flow is simple, time-consuming short, and the hydrogen chloride gas of generation can also repeat benefit by absorbing processing recycling
With the processing cost of material can be effectively reduced.
Spray pyrolysis prepares tertiary cathode presoma and refers to by the way that three kinds of nickel, cobalt, manganese metal salt solutions are equal in proportion
It is sprayed into high-temperature atmosphere after even mixing with mist, by the rapid evaporation of solvent and the hydrolysis of metal salt, it is mixed to obtain component
Close uniform ternary oxide presoma.
CN106197025B discloses a kind of spray pyrolysis furnace for preparing pure phase cobaltosic oxide, comprising: pyrolysis oven, two
Gas proportion mixing instrument, spray gun gas regulation conveying device, spray gun, combustion air atmosphere adjustment device, burner, burning zone atmosphere
Adjust conveying device, conveying section atmosphere adjustment device.Compressed air is mixed with oxygen by gas proportion mixing instrument, by spray
Enter spray gun after rifle gas regulation conveying device；Mixed gas enters pyrolysis oven after contacting atomization in spray gun with cobalt salt solution
It is interior；Combustion air atmosphere adjustment device is adjusted simultaneously, oxygen content in combustion air is adjusted, into burner；In addition, compressed air with
Oxygen enters burning zone atmosphere after the mixing of gas proportion mixing instrument and adjusts conveying device and input in pyrolysis oven；Open conveying
Section atmosphere adjustment device.It is sub- that the cobaltosic oxide that the spray pyrolysis furnace can thoroughly solve conventional spray pyrolysis furnace production contains oxidation
The problem of cobalt.
However, sufficiently atomization needs biggish pressure could shape due to when raw material is sprayed into from top during spray pyrolysis
At uniform droplet, so droplet has biggish initial velocity when entering furnace body.Simultaneously under gravity, droplet is further
Accelerate, quickly through heating zone, pyrolytic process is easy to cause to be not thorough, reaction is incomplete.In conventional spray pyrolysis equipment,
Certain negative pressure is formed on top, and the exhaust gas that reaction is generated is extracted out, is formed simultaneously a upward air-flow, reduces the decline of droplet
Speed increases the reaction time.Whole process needs a biggish reaction compartment, so general spray pyrolysis furnace design diameter
All at two meters or more.
CN106587172A discloses the production technology and process units of a kind of power battery anode ternary oxide, ternary
Mixed solution sprays into pyrolysis oven by top jet nozzle, passes through gas heating furnace body and the solution of penetrating, solution water in pyrolysis oven
Solution is at ternary oxide, hydrogen chloride and vapor.Enter absorption tower, ternary oxygen after the cyclone separator dedusting that gas passes through furnace roof
Compound then passes through natural subsidence and is discharged from the discharging equipment of furnace bottom.The hot gas that furnace bottom fuel gas buring generates is upward, can be effective
Increase reaction time of the drop in furnace, react fully progress.But it is very big to the diameter design requirement of furnace body in this way, generally
Need 2 meters or more.When furnace diameter is less than 1 meter, same design will lead to a large amount of materials and be sticked on furnace wall, generate a large amount of useless
Material is unfavorable for experiment and carries out.If being designed to that exhaust gas and oxide are passed in and out from furnace bottom simultaneously and will lead to oxide and exhaust gas is anti-
It answers, the ratio of chloride in oxide is significantly increased, cause the chloride content in product to severely exceed, simultaneous oxidation object is in furnace
The time of sintering can also be greatly decreased.
In general, there are still design diameter, equipment scale and land occupations for spray pyrolysis unit disclosed in the prior art
Area is big, and the raw material, energy consumption needed for thus causing in the actual production process are significantly increased, and is unfavorable for exploitation and the tune of technique
It is whole, also it is unfavorable for the integrated arrangement of equipment.Therefore, it is badly in need of changing the structure of spray pyrolysis unit disclosed in the prior art
Into, with solve the problems, such as presently, there are.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of spray for preparing tertiary cathode presoma
Mist pyrolysis installation and its application method, by the way that two groups of spray pyrolysis unit U-shapeds are connected to, effective reduction spray pyrolysis unit
Design diameter, while increasing the reaction time of material in the device, while keeping large-scale spray pyrolysis unit pyrolysis effect
Effectively reduce experimental cost.
To achieve this purpose, the present invention adopts the following technical scheme:
In a first aspect, described device includes 1 He of the first spray pyrolysis unit the present invention provides a kind of spray pyrolysis unit
Second spray pyrolysis unit 2,1 discharge port of the first spray pyrolysis unit connect conveying device, and the conveying device goes out
Mouth is arranged in the cavity of second spray pyrolysis unit 2.
The spray pyrolysis unit that the present invention designs, have U-shaped two-part structure, material in the first spray pyrolysis unit into
The preliminary pyrolysis of row, is then delivered to the second spray pyrolysis unit by conveying device, continues deeper into pyrolysis, the present invention is reducing
It ensure that material enough pyrolytic reaction time in furnace while device design diameter, reduce the chloride content in product.
As currently preferred technical solution, the conveying device includes the discharge port with the first spray pyrolysis unit 1
The pipeline 13 for conveying the powder conveying valve 5 of material and connecting with the powder conveying valve 5 of connection, the pipeline 13 go out
Mouth is arranged in the cavity of second spray pyrolysis unit 2.
Preferably, the powder conveying valve 5 is rotary valve, butterfly valve or slide valve.
Preferably, the powder conveying valve 5 is rotary valve, and the rotation valve housing is provided with a feed inlet, one
First air inlet 8 and a discharge port, the feed inlet are connect with 1 discharge port of the first spray pyrolysis unit, first air inlet
Mouth 8 is connect for being passed through the rotation of gas push rotary valve, the discharge port with the import of pipeline 13；The valve body packet of the rotary valve
Include valve rod and the flap shutter along valve rod genesis analysis.The gas that first air inlet 8 is passed through can push the leaf of rotary valve
Piece, band movable vane piece rotates, while keeping the temperature of rotary valve and discharge port, preliminarily forms in the first spray pyrolysis unit 1
It after particle is sent to pipeline by rotary valve, is driven by gas to the second spray pyrolysis unit 2, is further dried and hot
Solution.
Preferably, the outlet of the pipeline 13 is located at the 1/3~2/3 of the cavity of the second spray pyrolysis unit 2.If pipeline
13 outlet port is excessively high, causes the pre-product sprayed into the second spray pyrolysis unit 2 via pipeline 13 distance to be made a slip of the tongue out close, from
And pyrolysis time of the pre-product in the second spray pyrolysis unit 2 is shortened, it is unfavorable for deepening the extent of reaction；And pipeline 13 go out
Mouth position is too low, causes material collection chamber of the pre-product away from bottom entered in the second spray pyrolysis unit 2 excessively close, leads to pre- production
Sedimentation time of the object in the second spray pyrolysis unit 2 is too short, and pyrolytic reaction is not thorough.
As currently preferred technical solution, first spray pyrolysis unit 1 includes the first cavity and is arranged in institute
State the nozzle 3 at the top of the first cavity.
Preferably, first spray pyrolysis unit 1 further includes the first heating part that first chamber outer wall is arranged in
Part 11.
Preferably, the nozzle 3 is two-fluid aerosol nozzle or pressure nozzle.The maximum spray angle of spray head 3
It is appropriately adjusted according to the diameter of cavity, should guarantee that material is dispersed in entire cavity, prevent jet angle from spending again
Cause material to inject directly to cavity inner wall greatly, be adhered on cavity inner wall, causes the loss of effecting reaction material.This field skill
Art personnel can select according to professional knowledge, such as when the diameter is 1.2m, the spray angle of spray head is 60 degree.
Preferably, the diameter of first cavity be 0.5-1.8m, such as can be 0.5m, 0.6m, 0.7m, 0.8m,
0.9m, 1.0m, 1.1m, 1.2m, 1.3m, 1.4m, 1.5m, 1.6m, 1.7m or 1.8m.When cavity diameter is less than 0.5 meter, can lead
The a large amount of material sticks for causing spray head to eject generate a large amount of waste materials on furnace wall, are unfavorable for experiment and carry out.If being designed to exhaust gas
Passing in and out simultaneously from furnace bottom with oxide will lead to oxide and waste gas reaction again, and the ratio of chloride in oxide is significantly increased,
The chloride content in product is caused to severely exceed, the time that simultaneous oxidation object is sintered in furnace can also be greatly decreased.
As currently preferred technical solution, second spray pyrolysis unit 2 includes the second cavity and is set to the
The material collection chamber 7 of two cavity bottoms.Tertiary cathode presoma of the material collection chamber 7 to accept sedimentation.
Preferably, second spray pyrolysis unit 2 further includes the second heating part for being set to second chamber outer wall
Part 12.Heating element 12 is to heat the second spray pyrolysis unit 2.
Preferably, second spray pyrolysis unit 2 further includes the heating device 4 for being set to the second cavity bottom.
Preferably, the top of the material collection chamber 7 is arranged in the heating device 4.The heating of second cavity bottom fills
4 are set as 2 supplying heat of the second spray pyrolysis unit, is cooperated with the second heating element 12, so that into the second spray pyrolysis unit 2
Interior pre-product can be thoroughly pyrolyzed, and the tertiary cathode presoma being sufficiently pyrolyzed finally is prepared.
Preferably, the heating device 4 is gas nozzle or igniter burner.
Preferably, second cavity bottom is provided with the second air inlet 9 for being passed through gas.Present invention setting second
The first purpose of air inlet 9 is to maintain the micro-positive pressure in the second spray pyrolysis unit 2；The second purpose is from the second air inlet
9 are passed through the reaction temperature in high-temperature gas the second spray pyrolysis unit 2 of maintenance, while pre- production of the ascending air sprayed into sedimentation
Object generates the effect of twice dispersing, extends reaction time of the pre-product in the second spray pyrolysis unit 2.
Preferably, the diameter of second cavity be 0.5-1.8m, such as can be 0.5m, 0.6m, 0.7m, 0.8m,
0.9m, 1.0m, 1.1m, 1.2m, 1.3m, 1.4m, 1.5m, 1.6m, 1.7m or 1.8m.The diameter of first cavity and the second cavity is equal
Less than the design diameter of existing large-scale spray pyrolysis unit, in actual industrial processes, two small-sized spraying heat
It solves device to connect by conveying device, compared with one large-scale spray pyrolysis unit, in the base for ensuring identical pyrolysis effect
On plinth, have more flexible dynamic role, flexible arrangement can be carried out according to construction condition and workshop layout.
As currently preferred technical solution, 2 top of the second spray pyrolysis unit setting gas outlet and feedback outlet；
Second spray pyrolysis unit 2 further includes separator 6, the import of the separator 6 and the second spray pyrolysis unit 2
Gas outlet connection, the outlet of the separator 6 is connect with the feedback outlet of the second spray pyrolysis unit 2.
Preferably, the separator 6 is rotating separator or double-rotation type separator.Separator 6 can recycle again
Tertiary cathode presoma in exhaust gas.
Preferably, the exhaust outlet 10 for exhaust gas or dust to be discharged is equipped at the top of the separator 6.
Second aspect, the present invention provides a kind of methods for preparing tertiary cathode presoma, and the method is in such as first party
Device described in face carries out；
Preferably, which comprises
(I) the first spray pyrolysis unit 1 and the second spray pyrolysis unit 2 are preheated, the first spray pyrolysis unit 1 is dropped
Pressure, is pressurized the second spray pyrolysis unit 2；
(II) ternary mixing salt solution is sprayed by the first spray pyrolysis unit 1 by nozzle 3, generates pre-product；
(III) pre-product that step (II) obtains enters the second spray pyrolysis unit 2 by conveying device, and solid gas separates, Gu
Body is the tertiary cathode presoma, is handled or is recycled after gas discharge；
Preferably, which comprises
(I) the first spray pyrolysis unit 1 and the second spray pyrolysis unit 2 are preheated, is passed through gas, powder to the first air inlet 8
Body transfer valve 5 operating the first spray pyrolysis unit 1 is depressured, connect the second air inlet 9 to the second spray pyrolysis unit 2 into
Row pressurization；
(II) ternary mixing salt solution is sprayed by the first spray pyrolysis unit 1 by nozzle 3, pyrolysis generates pre-product；
(III) pre-product that step (II) obtains drop to rotary valve, is delivered to the second spray pyrolysis unit 2 through pipeline 13
In continue to be pyrolyzed, after reaction, solid, which is collected, obtains the tertiary cathode presoma, gas to material collection chamber 7
Into separator 6；
Preferably, it includes the outlet that gas passes through the second spray pyrolysis unit 2 that gas, which is discharged into the process of separator 6,
Mouth enters separator 6 and carries out solid gas separation, and exhaust gas is handled or recycled, and solid is recycled in the second spray pyrolysis unit 2.
Ternary mixing salt solution is sprayed into spray pyrolysis unit provided by the invention by nozzle 3, in the first spray pyrolysis
Preliminary fast hydrolyzing and drying are carried out in device 1, form the oxide particle of ball-type, the hydrogen chloride and steam generated with hydrolysis
The second spray pyrolysis unit 2 is entered by the powder conveying valve 5 that the first spray pyrolysis fills bottom together, is filled in the second spray pyrolysis
While setting that the reaction was continued in 2, ternary oxide is slowly settled, and completes the initial gross separation of exhaust gas and ternary oxide.Exhaust gas row
A small amount of ternary oxide in removing exhaust gas is removed by rotating separator after the second spray pyrolysis unit 2 out, is carried out into absorption tower
Recycling, gas outlet need to provide certain draft.The present invention reduces large-scale spray pyrolysis by using U-shaped two-piece design substantially
The reaction environment of device, when ensure that oxide enough pyrolytic reactions in furnace while the design diameter for reducing furnace body
Between, reduce the chloride content in product.
As currently preferred technical solution, the ternary salt-mixture is chlorate.
Preferably, the cation in the ternary salt-mixture is respectively nickel, cobalt and manganese.
Preferably, the mass ratio of the material of the nickel, cobalt and manganese is denoted as x:y:z, and the x:y:z is (0.33~0.9):
(0.03~0.33): (0.03~0.33), wherein x+y+z=1, such as can be 0.5:0.2:0.3,0.6:0.2:0.2,0.7:
0.2:0.1 or 0.8:0.1:0.1.
Preferably, the total concentration of nickel, cobalt and manganese element is 40~250g/L in the ternary mixing salt solution, such as can be with
It is 50g/L, 100g/L, 150g/L, 200g/L or 250g/L, preferably 100~200g/L, further preferred 150~180g/L.
Preferably, also doped in Al, Mg, Zr, Ti, Mn, La, Mo, W, Si, B and P in the ternary mixing salt solution
Any one or at least two combination.
As currently preferred technical solution, the preheating temperature of first spray pyrolysis unit 1 is 600~1200
DEG C, such as can be 600 DEG C, 700 DEG C, 800 DEG C, 900 DEG C, 1000 DEG C, 1100 DEG C or 1200 DEG C, preferably 700~1100 DEG C, into
Preferably 850~950 DEG C of one step.
Preferably, the preheating temperature of second spray pyrolysis unit 2 be 500~1000 DEG C, such as can be 500 DEG C,
600 DEG C, 700 DEG C, 800 DEG C, 900 DEG C or 1000 DEG C, preferably 600~900 DEG C, further preferred 700~800 DEG C.
Preferably, first spray pyrolysis unit 1 is depressurized to -500~-100Pa, for example, can be -500Pa, -
450Pa, -400Pa, -350Pa, -300Pa, -250Pa, -200Pa, -150Pa or -100Pa.
Preferably, the gauge pressure in second spray pyrolysis unit 2 be 0~200Pa, such as can be 0Pa, 50Pa,
100Pa, 150Pa or 200Pa.
As currently preferred technical solution, being passed through temperature to the first air inlet 8 in step (I) is 300~800 DEG C
Gas, such as can be 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C, 700 DEG C or 800 DEG C, preferably 500~700 DEG C, it is further excellent
Select 550~650 DEG C.
Preferably, it is passed through the gas that temperature is 300~800 DEG C to second air inlet 9 in step (III), such as
It can be 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C, 700 DEG C or 800 DEG C, preferably 500~700 DEG C, further preferred 550~650
℃。
The third aspect, the present invention provides a kind of tertiary cathode presoma, the tertiary cathode presoma uses such as second
Method described in aspect is prepared.
Preferably, the content of Cl element < 0.8% of the tertiary cathode presoma, for example, can be 0.1%, 0.2%,
0.3%, 0.4%, 0.5%, 0.6% or 0.7%.
Numberical range of the present invention not only includes enumerated point value, further includes the above-mentioned numerical value not included
Arbitrary point value between range, as space is limited and for concise consideration, range described in the present invention no longer exclusive list includes
Specific point value.
Compared with prior art, the invention has the benefit that
The present invention reduces the reaction environment of large-scale spray pyrolysis furnace by using U-shaped two-piece design substantially, is reducing
It ensure that oxide pyrolysis time sufficient in furnace while Proper Design diameter, reduce the chloride content in product,
Compared with the tertiary cathode presoma for using small-sized single furnace body spray pyrolysis unit to be prepared, using two sections provided by the invention
Chlorinity declines to a great extent in the tertiary cathode presoma that formula spray pyrolysis unit is prepared, and minimum is down to by 8.57%
0.32%.
Detailed description of the invention
Fig. 1 is the apparatus structure schematic diagram that one embodiment of the present invention provides.
Wherein, 100- spray pyrolysis unit；The first spray pyrolysis unit of 110-；The second spray pyrolysis unit of 120-；130-
Conveying device.
Fig. 2 is the apparatus structure schematic diagram that one embodiment of the present invention provides.
Wherein, the first spray pyrolysis unit of 1-；The second spray pyrolysis unit of 2-；3- nozzle；4- heating device；5- powder is defeated
Send valve；6- separator；7- material collection chamber；The first air inlet of 8-；The second air inlet of 9-；10- exhaust outlet；11- first is heated
Component；The second heating element of 12-；13- pipeline.
Specific embodiment
To further illustrate the technical scheme of the present invention below with reference to the accompanying drawings and specific embodiments.
In a specific embodiment, described the present invention provides a kind of spray pyrolysis unit 100 as shown in Figure 1
Spray pyrolysis unit 100 includes the first spray pyrolysis unit 110 and the second spray pyrolysis unit 120, first spray pyrolysis
The discharge port of device connects conveying device 130, and the outlet of the conveying device 130 is arranged in second spray pyrolysis unit
In 120 cavity.
In another specific embodiment, the present invention provides a kind of spray pyrolysis unit, the spray pyrolysis unit is such as
Shown in Fig. 2, including the first spray pyrolysis unit 1 and the second spray pyrolysis unit 2, the connection of 1 discharge port of the first spray pyrolysis unit
The outlet of conveying device, conveying device is arranged in the cavity of the second spray pyrolysis unit 2.
The conveying device include connect with the discharge port of the first spray pyrolysis unit 1 for convey material powder it is defeated
The outlet setting of the pipeline 13 for sending valve 5 and connecting with the powder conveying valve 5, the pipeline 13 is filled in second spray pyrolysis
It sets in 2 cavity.
First spray pyrolysis unit 1 includes the first cavity and the nozzle 3 being set at the top of the first cavity, the first cavity
Diameter be 1.2m, outer wall is coated with the first heating element 11；Nozzle 3 can be two-fluid aerosol nozzle or pressure-type spray
Mouth, the maximum spray angle of nozzle 3 are 90 degree.
Second spray pyrolysis unit 2 includes the second cavity and the material collection chamber 7 for being set to the second cavity bottom, the
The diameter of two cavitys is 1.2m, and outer wall is coated with the second heating element 12；Heating device 4 is provided with above material collection chamber 7,
Heating device 4 can be gas nozzle or igniter burner；Cavity bottom is additionally provided with the second air inlet 9 for being passed through gas.
Second spray pyrolysis unit 2 further includes separator 6, and gas outlet is arranged in 2 top of the second spray pyrolysis unit
And feedback outlet, the import of the separator 6 are connect with the gas outlet of the second spray pyrolysis unit 2, the separator 6 goes out
Mouth is connect with the feedback outlet of the second spray pyrolysis unit 2, and top is equipped with the exhaust outlet 10 for exhaust gas or dust to be discharged；Separation
Device 6 can be rotating separator or double-rotation type separator.
The process flow of spray pyrolysis unit provided by the invention are as follows:
(I) the first spray pyrolysis unit 1 and the second spray pyrolysis unit 2 are preheated, rotary valve 5 is opened, connects the first air inlet
8 pair of first spray pyrolysis unit 1 of mouth is depressured, and is connected the second air inlet 9 and is pressurized to the second spray pyrolysis unit 2；
(II) ternary mixing salt solution is sprayed into the first spray pyrolysis unit 1 by nozzle 3 and is tentatively pyrolyzed, generated
Pre-product；
(III) pre-product that step (II) obtains is entered in the second spray pyrolysis unit 2 by conveying device continues heat
Solution reaction, after reaction, reaction product is settled down to material collection chamber 7, recycles tertiary cathode presoma therein, remaining component
Enter separator 6 by the gas outlet of the second spray pyrolysis unit 2 further to separate, solid particle therein is recycled to second
In spray pyrolysis unit 2, exhaust gas is handled or is recycled after the discharge of the top vent 10 of separator 6.
Embodiment 1
The present embodiment prepares tertiary cathode presoma, the side using the spray pyrolysis unit provided in specific embodiment
Method includes: that configuration ternary mixing salt solution, furnace body preheating, spray pyrolysis and sedimentation separation, specific implementation step are as follows:
(1) it configures ternary mixing salt solution: weighing a certain amount of nickel chloride, cobalt chloride and manganese chloride by the ratio of the amount of substance
50L ternary mixed solution is configured for 0.5:0.2:0.3, nickel cobalt manganese total material is added in 150g/L in metal concentration control therein
Amount 0.5% aluminium chloride.
(2) furnace body preheats: 1150 DEG C is preheated to the first spray pyrolysis unit 1 by the first heating element 11, to first
Air inlet 8 is passed through 800 DEG C of gas, and driving powder conveying valve 5 rotates, by the vacuum cavitations in the first spray pyrolysis unit 1-
400Pa；1000 DEG C are preheated to the second spray pyrolysis unit 2 by the second heating element 12 and heating device 4, to the second air inlet
Mouthfuls 9 are passed through 800 DEG C of gas, by the intracorporal temperature control of 7 chamber of material collection chamber at 800 DEG C, the chamber of the second spray pyrolysis unit 2
The voltage-controlled system of body surface is in 100Pa.
(3) spray pyrolysis: after pyrolysis installation to be sprayed is stable, by configured ternary mixed solution with the speed of 5L/h
Degree is sprayed into the first pyrolysis installation 1 by nozzle 3 and is tentatively pyrolyzed, and the pre-product for reacting generation passes through 5 He of powder conveying valve
Pipeline 13 enters the second spray pyrolysis unit 2.
(4) sedimentation separation: pre-product is sufficiently pyrolyzed in the second spray pyrolysis unit 2, obtains tertiary cathode forerunner
Body, under the ascending air effect that the second air inlet 9 is passed through, solid particle obtains twice dispersing；Obtained gas is reacted to pass through
The gas outlet of second spray pyrolysis unit 2 enters separator 6, separates and recovers solid therein again via separator 6
Grain, exhaust gas are handled or are recycled after being discharged by the exhaust outlet 10 at 6 top of separator, exhausted to solution, continue to spray into
Air, blowing out after 15 minutes, and stop being passed through gas to the first air inlet 8 and the second air inlet 9, it is down to room temperature to temperature, is sunk
Aluminium therein is recycled in material collection chamber 7 after drop is complete adulterates 523 oxide precursors.
The content of chlorine element in 523 oxide precursors is adulterated using the aluminium that XRF ray fluorescence spectrometer device is tested,
Test result is shown in Table 1.
Embodiment 2
The present embodiment prepares tertiary cathode presoma, the side using the spray pyrolysis unit provided in specific embodiment
Method includes: that configuration ternary mixing salt solution, furnace body preheating, spray pyrolysis and sedimentation separation, specific implementation step are as follows:
(1) configure ternary mixing salt solution: weigh a certain amount of nickel chloride, cobalt chloride, manganese chloride by the amount of substance ratio
40L ternary mixed solution is configured for 0.5:0.2:0.3, nickel cobalt manganese total material is added in 180g/L in metal concentration control therein
Amount 0.5% aluminium chloride.
(2) furnace body preheats: 1080 DEG C is preheated to the first spray pyrolysis unit 1 by the first heating element 11, to first
Air inlet 8 is passed through 700 DEG C of gas, and driving powder conveying valve 5 rotates, by the vacuum cavitations in the first spray pyrolysis unit 1-
150Pa；900 DEG C are preheated to the second spray pyrolysis unit 2 by the second heating element 12 and heating device 4, to the second air inlet
Mouthfuls 9 are passed through 700 DEG C of gas, by the intracorporal temperature control of 7 chamber of material collection chamber at 700 DEG C, the chamber of the second spray pyrolysis unit 2
The voltage-controlled system of body surface is in 150Pa.
(3) spray pyrolysis: after pyrolysis installation to be sprayed is stable, by configured ternary mixed solution with the speed of 5L/h
Degree is sprayed into the first pyrolysis installation 1 by nozzle 3 and is tentatively pyrolyzed, and the pre-product for reacting generation passes through 5 He of powder conveying valve
Pipeline 13 enters the second spray pyrolysis unit 2.
(4) sedimentation separation: pre-product is sufficiently pyrolyzed in the second spray pyrolysis unit 2, obtains tertiary cathode forerunner
Body, under the ascending air effect that the second air inlet 9 is passed through, solid particle obtains twice dispersing；Obtained gas is reacted to pass through
The gas outlet of second spray pyrolysis unit 2 enters separator 6, separates and recovers solid therein again via separator 6
Grain, exhaust gas are handled or are recycled after being discharged by the exhaust outlet 10 at 6 top of separator, exhausted to solution, continue to spray into
Air, blowing out after 15 minutes, and stop being passed through gas to the first air inlet 8 and the second air inlet 9, it is down to room temperature to temperature, is sunk
Aluminium therein is recycled in material collection chamber 7 after drop is complete adulterates 523 oxide precursors.
The content of chlorine element in 523 oxide precursors is adulterated using the aluminium that XRF ray fluorescence spectrometer device is tested,
Test result is shown in Table 1.
Embodiment 3
The present embodiment prepares tertiary cathode presoma, the side using the spray pyrolysis unit provided in specific embodiment
Method includes: that configuration ternary mixing salt solution, furnace body preheating, spray pyrolysis and sedimentation separation, specific implementation step are as follows:
(1) configure ternary mixing salt solution: weigh a certain amount of nickel chloride, cobalt chloride, manganese chloride by the amount of substance ratio
50L ternary mixed solution is configured for 0.6:0.2:0.2, nickel cobalt manganese total material is added in 170g/L in metal concentration control therein
Amount 0.5% aluminium chloride.
(2) furnace body preheat: 930 DEG C are preheated to the first spray pyrolysis unit 1 by the first heating element 11, to first into
Air port 8 is passed through 600 DEG C of gas, and driving powder conveying valve 5 rotates, by the vacuum cavitations in the first spray pyrolysis unit 1-
190Pa；860 DEG C are preheated to the second spray pyrolysis unit 2 by the second heating element 12 and heating device 4, to the second air inlet
Mouthfuls 9 are passed through 600 DEG C of gas, by the intracorporal temperature control of 7 chamber of material collection chamber at 600 DEG C, the chamber of the second spray pyrolysis unit 2
The voltage-controlled system of body surface is in 130Pa.
(3) spray pyrolysis: after pyrolysis installation to be sprayed is stable, by configured ternary mixed solution with the speed of 5L/h
Degree is sprayed into the first pyrolysis installation 1 by nozzle 3 and is tentatively pyrolyzed, and the pre-product for reacting generation passes through 5 He of powder conveying valve
Pipeline 13 enters the second spray pyrolysis unit 2.
(4) sedimentation separation: pre-product is sufficiently pyrolyzed in the second spray pyrolysis unit 2, obtains tertiary cathode forerunner
Body, under the ascending air effect that the second air inlet 9 is passed through, solid particle obtains twice dispersing；Obtained gas is reacted to pass through
The gas outlet of second spray pyrolysis unit 2 enters separator 6, separates and recovers solid therein again via separator 6
Grain, exhaust gas are handled or are recycled after being discharged by the exhaust outlet 10 at 6 top of separator, exhausted to solution, continue to spray into
Air, blowing out after 15 minutes, and stop being passed through gas to the first air inlet 8 and the second air inlet 9, it is down to room temperature to temperature, is sunk
Aluminium therein is recycled in material collection chamber 7 after drop is complete adulterates 622 oxide precursors.
The content of chlorine element in 622 oxide precursors is adulterated using the aluminium that XRF ray fluorescence spectrometer device is tested,
Test result is shown in Table 1.
Embodiment 4
The present embodiment prepares tertiary cathode presoma, the side using the spray pyrolysis unit provided in specific embodiment
Method includes: that configuration ternary mixing salt solution, furnace body preheating, spray pyrolysis and sedimentation separation, specific implementation step are as follows:
(1) configure ternary mixing salt solution: weigh a certain amount of nickel chloride, cobalt chloride, manganese chloride by the amount of substance ratio
50L ternary mixed solution is configured for 0.8:0.1:0.1, nickel cobalt manganese total material is added in 170g/L in metal concentration control therein
Amount 0.3% aluminium chloride.
(2) furnace body preheat: 860 DEG C are preheated to the first spray pyrolysis unit 1 by the first heating element 11, to first into
Air port 8 is passed through 550 DEG C of gas, and driving powder conveying valve 5 rotates, by the vacuum cavitations in the first spray pyrolysis unit 1-
350Pa；790 DEG C are preheated to the second spray pyrolysis unit 2 by the second heating element 12 and heating device 4, to the second air inlet
Mouthfuls 9 are passed through 550 DEG C of gas, by the intracorporal temperature control of 7 chamber of material collection chamber at 550 DEG C, the chamber of the second spray pyrolysis unit 2
The voltage-controlled system of body surface is in 100Pa.
(3) spray pyrolysis: after pyrolysis installation to be sprayed is stable, by configured ternary mixed solution with the speed of 3L/h
Degree is sprayed into the first pyrolysis installation 1 by nozzle 3 and is tentatively pyrolyzed, and the pre-product for reacting generation passes through 5 He of powder conveying valve
Pipeline 13 enters the second spray pyrolysis unit 2.
(4) sedimentation separation: pre-product is sufficiently pyrolyzed in the second spray pyrolysis unit 2, obtains tertiary cathode forerunner
Body, under the ascending air effect that the second air inlet 9 is passed through, solid particle obtains twice dispersing；Obtained gas is reacted to pass through
The gas outlet of second spray pyrolysis unit 2 enters separator 6, separates and recovers solid therein again via separator 6
Grain, exhaust gas are handled or are recycled after being discharged by the exhaust outlet 10 at 6 top of separator, exhausted to solution, continue to spray into
Air, blowing out after 15 minutes, and stop being passed through gas to the first air inlet 8 and the second air inlet 9, it is down to room temperature to temperature, is sunk
Aluminium therein is recycled in material collection chamber 7 after drop is complete adulterates 811 oxide precursors.
The content of chlorine element in 811 oxide precursors is adulterated using the aluminium that XRF ray fluorescence spectrometer device is tested,
Test result is shown in Table 1.
Embodiment 5
The present embodiment prepares tertiary cathode presoma, the side using the spray pyrolysis unit provided in specific embodiment
Method includes: that configuration ternary mixing salt solution, furnace body preheating, spray pyrolysis and sedimentation separation, specific implementation step are as follows:
(1) configure ternary mixing salt solution: weigh a certain amount of nickel chloride, cobalt chloride, manganese chloride by the amount of substance ratio
50L ternary mixed solution is configured for 0.8:0.1:0.1, nickel cobalt manganese total material is added in 170g/L in metal concentration control therein
Amount 0.3% aluminium chloride.
(2) furnace body preheat: 700 DEG C are preheated to the first spray pyrolysis unit 1 by the first heating element 11, to first into
Air port 8 is passed through 450 DEG C of gas, and driving powder conveying valve 5 rotates, by the vacuum cavitations in the first spray pyrolysis unit 1-
200Pa；600 DEG C are preheated to the second spray pyrolysis unit 2 by the second heating element 12 and heating device 4, to the second air inlet
Mouthfuls 9 are passed through 450 DEG C of gas, by the intracorporal temperature control of 7 chamber of material collection chamber at 450 DEG C, the chamber of the second spray pyrolysis unit 2
The voltage-controlled system of body surface is in 100Pa.
(3) spray pyrolysis: after pyrolysis installation to be sprayed is stable, by configured ternary mixed solution with the speed of 3L/h
Degree is sprayed into the first pyrolysis installation 1 by nozzle 3 and is tentatively pyrolyzed, and the pre-product for reacting generation passes through 5 He of powder conveying valve
Pipeline 13 enters the second spray pyrolysis unit 2.
(4) sedimentation separation: pre-product is sufficiently pyrolyzed in the second spray pyrolysis unit 2, obtains tertiary cathode forerunner
Body, under the ascending air effect that the second air inlet 9 is passed through, solid particle obtains twice dispersing；Obtained gas is reacted to pass through
The gas outlet of second spray pyrolysis unit 2 enters separator 6, separates and recovers solid therein again via separator 6
Grain, exhaust gas are handled or are recycled after being discharged by the exhaust outlet 10 at 6 top of separator, exhausted to solution, continue to spray into
Air, blowing out after 15 minutes, and stop being passed through gas to the first air inlet 8 and the second air inlet 9, it is down to room temperature to temperature, is sunk
Aluminium therein is recycled in material collection chamber 7 after drop is complete adulterates 811 oxide precursors.
The content of chlorine element in 811 oxide precursors is adulterated using the aluminium that XRF ray fluorescence spectrometer device is tested,
Test result is shown in Table 1.
Embodiment 6
The present embodiment prepares tertiary cathode presoma, the side using the spray pyrolysis unit provided in specific embodiment
Method includes: that configuration ternary mixing salt solution, furnace body preheating, spray pyrolysis and sedimentation separation, specific implementation step are as follows:
(1) configure ternary mixing salt solution: weigh a certain amount of nickel chloride, cobalt chloride, manganese chloride by the amount of substance ratio
50L ternary mixed solution is configured for 0.8:0.1:0.1, nickel cobalt manganese total material is added in 150g/L in metal concentration control therein
Amount 0.6% aluminium chloride.
(2) furnace body preheat: 600 DEG C are preheated to the first spray pyrolysis unit 1 by the first heating element 11, to first into
Air port 8 is passed through 300 DEG C of gas, and driving powder conveying valve 5 rotates, by the vacuum cavitations in the first spray pyrolysis unit 1-
100Pa；500 DEG C are preheated to the second spray pyrolysis unit 2 by the second heating element 12 and heating device 4, to the second air inlet
Mouthfuls 9 are passed through 300 DEG C of gas, by the intracorporal temperature control of 7 chamber of material collection chamber at 300 DEG C, the chamber of the second spray pyrolysis unit 2
The voltage-controlled system of body surface is in 50Pa.
(3) spray pyrolysis: after pyrolysis installation to be sprayed is stable, by configured ternary mixed solution with the speed of 3L/h
Degree is sprayed into the first pyrolysis installation 1 by nozzle 3 and is tentatively pyrolyzed, and the pre-product for reacting generation passes through 5 He of powder conveying valve
Pipeline 13 enters the second spray pyrolysis unit 2.
(4) sedimentation separation: pre-product is sufficiently pyrolyzed in the second spray pyrolysis unit 2, obtains tertiary cathode forerunner
Body, under the ascending air effect that the second air inlet 9 is passed through, solid particle obtains twice dispersing；Obtained gas is reacted to pass through
The gas outlet of second spray pyrolysis unit 2 enters separator 6, separates and recovers solid therein again via separator 6
Grain, exhaust gas are handled or are recycled after being discharged by the exhaust outlet 10 at 6 top of separator, exhausted to solution, continue to spray into
Air, blowing out after 15 minutes, and stop being passed through gas to the first air inlet 8 and the second air inlet 9, it is down to room temperature to temperature, is sunk
Aluminium therein is recycled in material collection chamber 7 after drop is complete adulterates 811 oxide precursors.
The content of chlorine element in 811 oxide precursors is adulterated using the aluminium that XRF ray fluorescence spectrometer device is tested,
Test result is shown in Table 1.
Comparative example 1
523 oxide precursors are prepared using small-sized single furnace body spray pyrolysis unit, the preparation method uses and implementation
The ternary mixed solution of the identical proportion of example 1, the furnace diameter of spray pyrolysis unit are 0.8m, and preheating temperature is 950 DEG C, by ternary
Mixed solution is sprayed into spray pyrolysis unit with the speed of 3L/h and carries out pyrolytic reaction, and 523 oxide precursors are prepared.
The content of chlorine element in 523 oxide precursors tested using XRF ray fluorescence spectrometer device, test knot
Fruit is shown in Table 1.
Comparative example 2
523 oxide precursors are prepared using the large-scale spray pyrolysis unit for producing 2000t per year.The preparation method use with
The ternary mixed solution of the identical proportion of embodiment 1, the furnace diameter of spray pyrolysis unit are 4.8m, and preheating temperature is 960 DEG C, will
Ternary mixed solution is sprayed into spray pyrolysis unit with the speed of 500L/h and carries out pyrolytic reaction, before 523 oxides are prepared
Drive body.
The content of chlorine element in 523 oxide precursors tested using XRF ray fluorescence spectrometer device, test knot
Fruit is shown in Table 1.
The content of chlorine element in 1 tertiary cathode presoma of table
| Content of Cl element (wt%) | |
| Embodiment 1 | 0.32 |
| Embodiment 2 | 0.38 |
| Embodiment 3 | 0.43 |
| Embodiment 4 | 0.48 |
| Embodiment 5 | 0.64 |
| Embodiment 6 | 0.79 |
| Comparative example 1 | 8.57 |
| Comparative example 2 | 0.39 |
Since the chlorine element in the tertiary cathode presoma that is finally prepared is from the ternary salt-mixture not being pyrolyzed completely
Solution, thus, content of Cl element can reflect the degree and efficiency of pyrolytic reaction with side, if the chlorinity in presoma is higher
Then illustrate that pyrolytic reaction is not thorough, it is on the contrary then illustrate that pyrolytic reaction is complete.
The test result of content of Cl element can be seen that the embodiment of the present invention 1 and be prepared into from embodiment 1 and comparative example 1
To tertiary cathode presoma in content of Cl element compared with comparative example 1 compared to significantly decreasing, illustrate that comparative example 1 uses small-sized
Single furnace body spray pyrolysis unit cannot achieve sufficient pyrolytic reaction, this is because spray pyrolysis unit used in comparative example 1
For single furnace body spray pyrolysis unit of diameter 0.8m, reaction time of the material liquid in pyrolysis installation is insufficient, and the extent of reaction is inadequate,
Pyrolytic reaction is not thorough.
The test result of content of Cl element can be seen that the embodiment of the present invention 1 and be prepared into from embodiment 1 and comparative example 2
To tertiary cathode presoma in the content of Cl element then very close large-scale spray pyrolysis furnace preparation for producing 2000t per year ternary
Content of Cl element in positive presoma, also side illustration the two is very close in pyrolytic reaction degree for this, but this hair
Bright advantage is the design diameter (0.5-1.8m) of spray pyrolysis unit provided by the invention much smaller than the large size for producing 2000t per year
The design diameter (4.8m) of spray pyrolysis furnace, therefore during actual industrial application, compared with large-scale spray pyrolysis furnace,
The occupied area of spray pyrolysis unit provided by the invention is then smaller, and investment, operation and maintenance cost will be lower, can be according to construction
The actual conditions at scene carry out flexible arrangement.
The Applicant declares that the foregoing is merely a specific embodiment of the invention, but protection scope of the present invention not office
It is limited to this, it should be clear to those skilled in the art, any to belong to those skilled in the art and take off in the present invention
In the technical scope of dew, any changes or substitutions that can be easily thought of, and all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of spray pyrolysis unit, which is characterized in that described device includes the first spray pyrolysis unit (1) and the second spraying heat
It solves device (2), the first spray pyrolysis unit (1) discharge port connects conveying device, the outlet setting of the conveying device
In the cavity of second spray pyrolysis unit (2).
2. the apparatus according to claim 1, which is characterized in that the conveying device includes and the first spray pyrolysis unit
(1) pipeline for conveying the powder conveying valve (5) of material and being connect with the powder conveying valve (5) of discharge port connection
(13), the outlet of the pipeline (13) is arranged in the cavity of second spray pyrolysis unit (2)；
Preferably, the powder conveying valve (5) is rotary valve, butterfly valve or slide valve；
Preferably, the powder conveying valve (5) is rotary valve, and the rotation valve housing is provided with a feed inlet, one the
One air inlet (8) and a discharge port, the feed inlet are connect with the first spray pyrolysis unit (1) discharge port, described first into
Air port (8) is connect for being passed through the rotation of gas push rotary valve, the discharge port with the import of pipeline (13)；The rotary valve
Valve body includes valve rod and the flap shutter along valve rod genesis analysis；
Preferably, the outlet of the pipeline (13) is located at the 1/3~2/3 of the cavity of the second spray pyrolysis unit (2).
3. device according to claim 1 or 2, which is characterized in that first spray pyrolysis unit (1) includes the first chamber
Body and the nozzle (3) being arranged at the top of first cavity；
Preferably, first spray pyrolysis unit (1) further includes the first heating element that first chamber outer wall is arranged in
(11)；
Preferably, the nozzle (3) is two-fluid aerosol nozzle or pressure nozzle；
Preferably, the diameter of first cavity is 0.5-1.8m.
4. device according to claim 1-3, which is characterized in that second spray pyrolysis unit (2) includes
Second cavity and the material collection chamber (7) for being set to the second cavity bottom；
Preferably, second spray pyrolysis unit (2) further includes the second heating element for being set to second chamber outer wall
(12)；
Preferably, second spray pyrolysis unit (2) further includes the heating device (4) for being set to the second cavity bottom；
Preferably, the heating device (4) is arranged in the top of the material collection chamber (7)；
Preferably, the heating device (4) is gas nozzle or igniter burner；
Preferably, second cavity bottom is provided with the second air inlet (9) for being passed through gas；
Preferably, the diameter of second cavity is 0.5-1.8m.
5. device according to claim 1-4, which is characterized in that the second spray pyrolysis unit (2) top
Gas outlet and feedback outlet are set；Second spray pyrolysis unit (2) further includes separator (6), the separator (6)
Import is connect with the gas outlet of the second spray pyrolysis unit (2), the outlet of the separator (6) and the second spray pyrolysis unit
(2) feedback outlet connection；
Preferably, the separator (6) is rotating separator or double-rotation type separator；
Preferably, the exhaust outlet (10) for exhaust gas or dust to be discharged is equipped at the top of the separator (6).
6. a kind of method for preparing tertiary cathode presoma, which is characterized in that the method is described in the claim any one of 1-5
Device in carry out；
Preferably, which comprises
(I) the first spray pyrolysis unit (1) and the second spray pyrolysis unit (2) are preheated, the first spray pyrolysis unit (1) is carried out
Decompression, is pressurized the second spray pyrolysis unit (2)；
(II) ternary mixing salt solution is sprayed into the first spray pyrolysis unit (1) by nozzle (3), generates pre-product；
(III) pre-product that step (II) obtains enters the second spray pyrolysis unit (2) by conveying device, solid gas separation, solid
For the tertiary cathode presoma, is handled or recycled after gas discharge；
Preferably, which comprises
(I) the first spray pyrolysis unit (1) and the second spray pyrolysis unit (2) are preheated, is passed through gas to the first air inlet (8),
Powder conveying valve (5) operating is depressured the first spray pyrolysis unit (1), connects the second air inlet (9) to the second spraying heat
Solution device (2) is pressurized；
(II) ternary mixing salt solution is sprayed into the first spray pyrolysis unit (1) by nozzle (3), pyrolysis generates pre-product；
(III) pre-product that step (II) obtains drop to rotary valve, is delivered to the second spray pyrolysis unit (2) through pipeline (13)
In continue to be pyrolyzed, after reaction, solid, which is collected, obtains the tertiary cathode presoma, gas to material collection chamber (7)
Body enters separator (6)；
Preferably, it includes the outlet that gas passes through the second spray pyrolysis unit (2) that gas, which is discharged into the process of separator (6),
Mouth enters separator (6) and carries out solid gas separation, and exhaust gas is handled or recycled, and solid is recycled to the second spray pyrolysis unit
(2) in.
7. according to the method described in claim 6, it is characterized in that, the ternary salt-mixture is chlorate；
Preferably, the cation in the ternary salt-mixture is respectively nickel, cobalt and manganese；
Preferably, the mass ratio of the material of the nickel, cobalt and manganese is denoted as x:y:z, and the x:y:z is (0.33~0.9): (0.03~
0.33): (0.03~0.33), wherein x+y+z=1；
Preferably, in the ternary mixing salt solution nickel, cobalt and manganese element total concentration be 40~250g/L, preferably 100~
200g/L, further preferred 150~180g/L；
Preferably, also doped with any in Al, Mg, Zr, Ti, Mn, La, Mo, W, Si, B and P in the ternary mixing salt solution
It is a kind of or at least two combination.
8. method according to claim 6 or 7, which is characterized in that the preheating temperature of first spray pyrolysis unit (1)
Degree is 600~1200 DEG C, preferably 700~1100 DEG C, further preferred 850~950 DEG C；
Preferably, the preheating temperature of second spray pyrolysis unit (2) be 500~1000 DEG C, preferably 600~900 DEG C, into one
Preferably 700~800 DEG C of step；
Preferably, first spray pyrolysis unit (1) is depressurized to -500~-100Pa；
Preferably, the gauge pressure in second spray pyrolysis unit (2) is 0~200Pa.
9. according to the described in any item methods of claim 6-8, which is characterized in that logical to the first air inlet (8) in step (I)
Entering temperature is 300~800 DEG C of gas, preferably 500~700 DEG C, further preferred 550~650 DEG C；
Preferably, it is passed through the gas that temperature is 300~800 DEG C to second air inlet (9) in step (III), preferably
500~700 DEG C, further preferred 550~650 DEG C.
10. a kind of tertiary cathode presoma, which is characterized in that the tertiary cathode presoma is used as claim 6-9 is any
Method described in is prepared；
Preferably, content of Cl element < 0.8% of the tertiary cathode presoma.
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| CN112758893A (en) * | 2019-10-21 | 2021-05-07 | 荆门市格林美新材料有限公司 | Spray pyrolysis preparation method and device of ternary cathode material |
| CN114180649A (en) * | 2021-12-14 | 2022-03-15 | 天津巴莫科技有限责任公司 | Preparation method of doped modified ternary precursor oxide |
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