CN107834069A - The production technology of improved nanometer lithium iron phosphate cathode material - Google Patents

The production technology of improved nanometer lithium iron phosphate cathode material Download PDF

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Publication number
CN107834069A
CN107834069A CN201711313715.2A CN201711313715A CN107834069A CN 107834069 A CN107834069 A CN 107834069A CN 201711313715 A CN201711313715 A CN 201711313715A CN 107834069 A CN107834069 A CN 107834069A
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fixed
tank
frame
pipe
iron phosphate
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CN107834069B (en
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林晓丽
陈晔
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Hunan Pengbo New Material Co ltd
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Haining Yongxin Technology Consulting Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/45Phosphates containing plural metal, or metal and ammonium
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Crushing And Pulverization Processes (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention provides a kind of production technology of improved nanometer lithium iron phosphate cathode material.It solves that the step of existing manufacture method is excessively simple, can not ensure the technical problems such as the quality of product, poor product quality.The production technology of this improved nanometer lithium iron phosphate cathode material, is comprised the technical steps that:A, by Li source compound, ferric iron source compound, P source compound, stoichiometrically ratio adds water to mix, and adds doped metal ion oxide and a carbon source, is well mixed, and spray drying obtains drying powder;B, the powder in step a is pre-processed into 3 8h in 350 550 DEG C of temperature ranges in nitrogen, secondary carbon source and water is added after cooling, spray drying obtains spherical powder;C, the spherical powder in step b is crushed by airflow comminution system, the powder after crushing handles 8 24h in nitrogen by 600 650 DEG C, then carries out 700 960 DEG C of 16h of high-temperature heat treatment 8, and nanometer lithium iron phosphate cathode material is obtained after cooling.The present invention has the advantages of product quality is high.

Description

The production technology of improved nanometer lithium iron phosphate cathode material
Technical field
The present invention relates to a kind of production technology, particularly a kind of production work of improved nanometer lithium iron phosphate cathode material Skill.
Background technology
Lithium iron phosphate electrode material is mainly used in various lithium ion batteries.The NTT Japanese from 1996 is disclosed first AyMPO4(A is alkali metal, and M is both CoFe combination:LiFeCoPO4) olivine structural anode material of lithium battery after, Texas, USA in 1997 stands the research group such as university, has also then reported LiFePO4Reversibly move into abjection lithium Characteristic, the U.S. coincidentally deliver olivine structural (LiMPO with Japan4) so that the material receives great attention, and Cause extensive research and rapidly development.With traditional lithium ion secondary battery anode material, the LiMn of spinel structure2O4 With the LiCoO of layer structure2Compare, LiMPO4Raw material source more extensively, price is less expensive and non-environmental-pollution.
Through retrieval, as Chinese patent literature discloses a kind of manufacture method of LiFePO4【Application number: 201280029356.7;Publication number:CN 103596877A】.The manufacture method of this LiFePO4, it is characterised in that possess with Lower process:Aqueous solution preparatory process, prepare the aqueous solution comprising phosphoric acid and hydroxycarboxylic acid;1st production process, in the aqueous solution The iron particle of middle oxygen of the addition containing 0.1~2 mass %, makes the phosphoric acid in the aqueous solution and the hydroxyl in an oxidizing environment Yl carboxylic acid reacts with the iron particle and makes the 1st reaction solution;2nd production process, in the 1st reaction solution add lithium source and Make the 2nd reaction solution;3rd production process, add carbon source in the 2nd reaction solution and make the 3rd reaction solution;Precursor generates work Sequence, make the 3rd reaction solution dry and generate iron lithium phosphate precursor;And calcination process, by the iron lithium phosphate precursor non- Calcined under oxidative environment and obtain LiFePO4.
Although the manufacture method disclosed in the patent can produce LiFePO4, the step of the manufacture method excessively Simply, the quality of product can not be ensured, poor product quality, therefore, design a kind of improved nanometer lithium iron phosphate cathode material Production technology be necessary.
The content of the invention
The purpose of the present invention is above mentioned problem be present for existing technology, it is proposed that a kind of improved nano-grade lithium iron phosphate The production technology of positive electrode, the production technology have the characteristics of product quality is high.
The purpose of the present invention can be realized by following technical proposal:The production of improved nanometer lithium iron phosphate cathode material Technique, it is characterised in that comprise the technical steps that:
A, by Li source compound, ferric iron source compound, P source compound, stoichiometrically ratio adds water to mix, and adds Doped metal ion oxide and a carbon source, it is well mixed;The slurry of formation carries out a high energy Ultrafine Grinding processing 2-3h, obtains The slurry D50 arrived is less than 0.2 μm, and spray drying obtains drying powder, sieves;
B, the powder in step a is pre-processed into 3-8h in 350-550 DEG C of temperature range in nitrogen, added after cooling secondary Carbon source and water, the slurry of formation is stirred, after the processing of secondary high energy Ultrafine Grinding, obtained slurry D50 is less than 0.2 μm, spraying Spherical powder is dried to obtain, is sieved;
C, the spherical powder in step b is crushed by airflow comminution system, the powder after crushing passes through in nitrogen 600-650 DEG C of processing 8-24h is crossed, then carries out 700-960 DEG C of high-temperature heat treatment 8-16h, nano-grade lithium iron phosphate is being obtained after cooling just Pole material.
Using process above, required size can be crushed to by airflow comminution system, it is ensured that the one of the size of product Cause property, product quality are high.
Airflow comminution system in the step c includes frame, be provided with the frame feed device, decomposer and Collection device, the feed device include storage tank and feed pipe, and storage tank is fixed in frame, and storage tank upper end has input Mouthful, storage tank lower end is connected by guide pipe with the tube wall of feed pipe, and installing pipe is provided between storage tank and guide pipe, is pacified Tubulature upper end is connected with storage tank lower end, and installing pipe lower end is connected with guide pipe, and having in installing pipe can be by storage tank Material is transported to the conveying mechanism of guide pipe, and the dredging mechanism that can dredge storage tank lower end is provided with frame;The decomposition Device includes decomposing tank, locating ring, some air supply pipes, feeder sleeve and air compressor machine, decomposes tank and is arranged in frame, locating ring is set Decomposing in tank, and locating ring, positioned at decomposing in the middle part of tank, the outlet side of some air supply pipes is fixed on positioning through pot sidewall is decomposed On ring, and outlet side is connected towards locating ring center, the inlet end of air supply pipe by the first communicating pipe with air compressor machine, feeder sleeve Discharge end be fixed on and decompose in tank, and discharge end is towards locating ring, and the feed end of feeder sleeve is through decomposing pot sidewall and feeding Pipe is connected, and decomposes tank top and is provided with sorting mechanism, decomposes tank bottom and is provided with recovering mechanism;The collection device includes receiving Collection tank, efferent duct and output screw, collecting tank are fixed in frame, and collecting tank upper end has an import, the import of collecting tank and point Solution tank top is connected, and collecting tank lower end has outlet, and the outlet of collecting tank is connected with the tube wall of efferent duct, efferent duct one end For blind end, the efferent duct other end is output end, the keeper for positioning is provided with output end, output screw one end is located at In efferent duct, the output screw other end, which passes the blind end of efferent duct and one, can drive its drive mechanism rotated to be connected, frame On be further fixed on baffle box, baffle box sidepiece has opening, be hinged with baffle box can by closure of openings live chamber door, efferent duct Output end be located at through baffle box side wall in baffle box, being additionally provided with frame can be by the vacuum cleaner of dust absorption in baffle box Structure.
The operation principle of airflow comminution system is as follows:By conveying mechanism by the feedstock transportation in storage tank to guide pipe In, raw material is entered in feed pipe in the presence of self gravitation, so as to realize its feeding operation;Raw material in feed pipe is led to Cross feeder sleeve be transported to decompose tank in, air compressor machine by the air after compression by air supply pipe be transported to decompose tank in, raw material by The high speed impact of air, produce between each other and rub and resolve into nanoscale powder material, by sorting mechanism by satisfactory Grain filters out, and is reclaimed undesirable particle by recovering mechanism, so as to complete its apportioned effort;Nanoscale powder material is defeated It is sent in collecting tank, material bag is fixed in the output end of efferent duct by keeper, output spiral shell is driven by drive mechanism Bar is rotated, and with the rotation of output screw, the nanoscale powder material in collecting tank is transported in material bag, will by dust collection mechanism Dust absorption in baffle box, so as to realize that it collects operation.
The conveying mechanism includes conveying axis and reducing motor, and conveying axis are horizontally set in installing pipe, and conveys axle position Below the gas outlet of appendix, conveying shaft end is connected with the output shaft of reducing motor, and some conveyings are fixed with conveying axis Blade.
When needing the feedstock transportation by storage tank into guide pipe, the output shaft of reducing motor is controlled to drive conveying axis to turn Dynamic, conveying axis drive conveying blade to rotate, can be by the feedstock transportation of storage tank into guide pipe with the rotation of conveying blade.
The dredging mechanism includes appendix, and the gas outlet of appendix is located in installing pipe through the tube wall of installing pipe, and The end is vertical upward, and the air inlet of appendix is connected with above-mentioned air compressor machine, and magnetic valve is provided with appendix, is also set in frame The control structure of electromagnetic valve work can be controlled by being equipped with.
When the lower end of storage tank blocks, magnetic valve is controlled to obtain by control structure electric, magnetic valve connects appendix, empty Mechanism of qi is delivered air in the air inlet of appendix, and the gas outlet of appendix moves up the raw material of storage tank lower end, will It is dredged, so as to can ensure that being normally carried out for feeding operation, good operating stability.
The control structure includes flexure strip, travel switch and the first controller, and flexure strip one end is fixed on guide pipe On tube wall, the flexure strip other end is free end, and travel switch is fixed on the tube wall of guide pipe, and travel switch is located at flexure strip Top, the free end of flexure strip can be with travel switch contact, and travel switch and magnetic valve are connected with first controller.
Under normal circumstances, under the Action of Gravity Field of raw material, flexure strip deforms downwards flexure strip, the free end of flexure strip and row Cheng Kaiguan is separated, and signal is passed to the first controller by travel switch, and the first controller makes magnetic valve dead electricity;When under storage tank When end blocks, signal is passed to the first controller, the first control by the free end of flexure strip and travel switch contact, travel switch It is electric that device obtains magnetic valve, easy to control, quick.
The sorting mechanism includes screen plate, vibration motor, discharge nozzle and the first asepwirator pump, and screen plate is arranged on decomposition tank It is interior, and screen plate offers some material paths, vibration motor is fixed on sieve by mounting bracket positioned at tank top is decomposed on screen plate Select on plate, discharge nozzle one end is connected with tank top is decomposed, and the discharge nozzle other end is connected with collecting tank, and the first asepwirator pump is set In discharge nozzle.
When needing satisfactory particle screen selecting, the first asepwirator pump is opened, satisfactory particle may pass through sieve The material path of plate is selected, is transported to by discharge nozzle in collecting tank, screening is quick;Screen plate is set to produce shake by vibration motor It is dynamic, material path can be avoided to block, good operating stability.
The recovering mechanism includes recovery tube and the second asepwirator pump, and recovery tube one end is connected with tank bottom is decomposed, and reclaims The pipe other end is connected with storage tank, and the second asepwirator pump is arranged in recovery tube.
When needing to reclaim undesirable particle, the second asepwirator pump is opened, storing is transported to by recovery tube In tank, it is decomposed again.
Be additionally provided with the frame can adjust first communicating pipe flow regulating and controlling mechanism, regulating and controlling mechanism includes pressure sensing Device, first flow regulating valve and second controller, pressure sensor and first flow regulating valve were successively set on for the first communicating pipe In, and between pressure sensor is located at first flow regulating valve and decomposes tank, pressure sensor and first flow regulating valve with The second controller is connected.
Using above structure, signal is passed to by second controller, second controller control first by pressure sensor The opening degree of flow control valve, so as to can realize first communicating pipe flow dynamic regulation, regulation and control are accurate.
The keeper includes rubber ring, and rubber ring is arranged and is fixed in the output end of efferent duct, rubber ring lateral surface It is upper that there are some protuberances.
Using above structure, material bag is enclosed in the output end of efferent duct, determined material bag by the elastic force of rubber ring Position is lived, and positioning is reliable;Frictional force between rubber ring and material bag, good operating stability can be increased by protuberance.
The dust collection mechanism includes the first blower fan, the 3rd asepwirator pump and air intake duct, and the first blower fan is fixed in baffle box, and First blower fan is located above efferent duct, and the air-out mouth down of the first blower fan, air intake duct one end is connected with baffle box bottom, air-breathing The pipe other end and the 3rd asepwirator pump are connected, and filter bag is provided with air intake duct.
When needing dust absorption in baffle box, the air in baffle box is conveyed downwards by the first blower fan, powder Dirt moves down with air, by the 3rd asepwirator pump by the dust absorption of baffle box, in suction filter bag, absorbs convenient, fast Speed.
The drive mechanism includes motor, driving gear and driven gear, and motor is fixed in frame, and driving gear is fixed On the output shaft of motor, driven gear is fixed on output screw, and driving gear is meshed with driven gear.
When needing to rotate output screw, the output shaft of controlled motor drives driving gear to rotate, and driving gear drives Driven gear rotates, and driven gear drives output screw to rotate, so as to rotate output screw.
Be provided with the cooling body for being cooled down to air compressor machine in the frame, cooling body include mounting bracket and Second blower fan, mounting bracket are arranged in frame, have snubber block between mounting bracket and frame, and the second blower fan can band by one Move its travel mechanism moved horizontally to be arranged in mounting bracket, the second blower fan be located at air compressor machine top, and the second blower fan goes out Air port is towards air compressor machine.
When needing to cool to air compressor machine, the second horizontal fan is driven to move by travel mechanism, the second mobile blower fan Air compressor machine can integrally be cooled down, reliable operation.
The travel mechanism includes the first curved guide rail, the first sliding block, installing plate, servomotor and gear, and first Guide rail is fixed in mounting bracket, and has teeth on the intrados of the first guide rail, and the first sliding block is arranged in the first guide rail, peace Loading board is fixed on the first sliding block, and servomotor is fixed on installing plate upper surface, the output shaft of servomotor straight down, gear It is fixed on the output shaft of servomotor, gear is meshed with the teeth of the first guide rail, and the second blower fan can drive thereon by one The elevating mechanism of lower lifting is arranged on installing plate lower surface.
When needing to make the second horizontal fan to move, the output shaft of servomotor is controlled to drive pinion rotation, gear and the The teeth of one guide rail, which are meshed, makes the first sliding block be moved horizontally along the first guide rail, and the first sliding block drives installing plate to move horizontally, Installing plate drives the movement of the second horizontal fan, so as to move the second horizontal fan.
The elevating mechanism includes push-rod electric machine, the second sliding block and the second guide rail, and the second guide rail is fixed on by link Installing plate lower surface, the second sliding block are arranged in the second guide rail, and push-rod electric machine is fixed on installing plate lower surface, and push-rod electric machine pushes away Straight down, the push rod end of push-rod electric machine is connected bar with the second sliding block, and the second blower fan is fixed on the second sliding block.
When needing to move up and down the second blower fan, the push rod of push-rod electric machine is controlled to drive the second sliding block along the second guide rail Move up and down, the second sliding block drives the second blower fan to move up and down, and the air compressor machine of different model can be cooled down, strong adaptability.
The controlling organization of servomotor start and stop can be controlled by being additionally provided with the frame, and controlling organization passes including some temperature Sensor, display screen and the 3rd controller, if dry temperature sensor is separately positioned on air compressor machine, and the uniform cloth of temperature sensor Put, display screen is fixed in frame, and temperature sensor, display screen and servomotor are connected with the 3rd controller.
Using above structure, the temperature at air compressor machine is detected by temperature sensor, signal is passed into the 3rd control Device, the 3rd controller show its temperature value by display screen, meanwhile, the control servomotor work of the 3rd controller, servomotor The second horizontal fan is moved, it is easy to control.
Compared with prior art, the production technology of this improved nanometer lithium iron phosphate cathode material has advantages below:
1st, required size can be crushed to by airflow comminution system in production technology, it is ensured that the size of product it is consistent Property, product quality is high.
2nd, delivered air to by air compressor machine in appendix, appendix moves up the raw material of storage tank lower end, can Ensure being normally carried out for feeding operation, good operating stability.
3rd, raw material is made to be produced between each other by high speed impact and rub and resolve into nanoscale powder material, will accord with by air Close desired particle screen selecting to go out, undesirable particle is reclaimed, cross multioperation without artificial, decomposition efficiency is high.
4th, the dust in baffle box is moved down by the first blower fan, inhaled the dust of baffle box by the 3rd asepwirator pump Remove, it is convenient to absorb.
5th, the second sliding block is driven to move up and down by push-rod electric machine, the second sliding block drives the second blower fan to move up and down, can be right The air compressor machine of different model is cooled down, strong adaptability.
Brief description of the drawings
Fig. 1 is the planar structure schematic diagram of this feed device.
Fig. 2 is the sectional view that this feed device removes part.
Fig. 3 is the sectional view of this decomposer.
Fig. 4 is the sectional view that this decomposer removes part.
Fig. 5 is the planar structure schematic diagram of this collection device.
Fig. 6 is the close-up schematic view at A in Fig. 5.
Fig. 7 is the dimensional structure diagram of baffle box in this collection device.
Fig. 8 is the dimensional structure diagram of this cooling body.
Fig. 9 is the dimensional structure diagram that this cooling body removes part.
In figure, 1, frame;2nd, reducing motor;3rd, guide pipe;4th, feed pipe;4a, connecting portion;5th, the first controller;6th, pacify Tubulature;7th, storage tank;8th, appendix;9th, magnetic valve;11st, conveying axis;12nd, conveying blade;13rd, guide housing;14th, travel switch; 15th, flexure strip;20th, air compressor machine;21st, first flow regulating valve;22nd, the first communicating pipe;23rd, pressure sensor;24th, the second control Device;25th, rubber slab;26th, recovery tube;27th, the second asepwirator pump;28th, air supply pipe;29th, locating ring;30th, tank is decomposed;30a, maintenance Mouthful;31st, screen plate;32nd, vibration motor;33rd, mounting bracket;34th, the first asepwirator pump;35th, discharge nozzle;36th, feeder sleeve;37th, cover plate; 40th, output screw;41st, the second communicating pipe;42nd, efferent duct;42a, blind end;42b, output end;43rd, second flow regulating valve; 44th, the 3rd asepwirator pump;45th, air intake duct;46th, baffle box;47th, collecting tank;48th, driving gear;49th, motor;50th, driven gear; 51st, filter bag;52nd, chamber door;53rd, the first blower fan;54th, rubber ring;55th, access panel;60th, the 3rd controller;61st, display screen;63、 Snubber block;64th, mounting bracket;65th, the first guide rail;65a, teeth;66th, gear;67th, servomotor;68th, installing plate;69th, second Blower fan;70th, temperature sensor;71st, push-rod electric machine;72nd, the second sliding block;73rd, the second guide rail;74th, link;75th, the first sliding block.
Embodiment
It is the specific embodiment of the present invention and with reference to accompanying drawing below, technical scheme is further described, But the present invention is not limited to these embodiments.
The production technology of this improved nanometer lithium iron phosphate cathode material, is comprised the technical steps that:
A, by Li source compound, ferric iron source compound, P source compound, stoichiometrically ratio adds water to mix, and adds Doped metal ion oxide and a carbon source, it is well mixed;The slurry of formation carries out a high energy Ultrafine Grinding processing 2-3h, obtains The slurry D50 arrived is less than 0.2 μm, and spray drying obtains drying powder, sieves;In the present embodiment, the slurry of formation carries out one Secondary high energy Ultrafine Grinding handles 2.5h;Li source compound is lithium carbonate;Ferric iron source compound is Fe2O3;P source compound is FePO4;Doped metal ion oxide is MnO2、TiO2, MgO and Nb2O5;Carbon source is glucose;
B, the powder in step a is pre-processed into 3-8h in 350-550 DEG C of temperature range in nitrogen, added after cooling secondary Carbon source and water, the slurry of formation is stirred, after the processing of secondary high energy Ultrafine Grinding, obtained slurry D50 is less than 0.2 μm, spraying Spherical powder is dried to obtain, is sieved;In the present embodiment, the powder in step a is located in advance in nitrogen in 450 DEG C of temperature ranges Manage 6h;Secondary carbon source is chitosan;
C, the spherical powder in step b is crushed by airflow comminution system, the powder after crushing passes through in nitrogen 600-650 DEG C of processing 8-24h is crossed, then carries out 700-960 DEG C of high-temperature heat treatment 8-16h, nano-grade lithium iron phosphate is being obtained after cooling just Pole material;In the present embodiment, the powder after crushing handles 16h in nitrogen by 620 DEG C, then carries out at 800 DEG C of high warms Manage 12h.
Using process above, required size can be crushed to by airflow comminution system, it is ensured that the one of the size of product Cause property, product quality are high.
As shown in Figure 1, Figure 2, shown in Fig. 3, Fig. 4, Fig. 5, Fig. 7, the airflow comminution system in step c includes frame 1, in frame 1 Feed device, decomposer and collection device are provided with, feed device includes storage tank 7 and feed pipe 4, and storage tank 7 is fixed on In frame 1, storage tank 7 is fixed in frame 1 by bolted connection, and the upper end of storage tank 7 has input port, storage tank 7 Lower end is connected by guide pipe 3 with the tube wall of feed pipe 4;Installing pipe 6, installing pipe are provided between storage tank 7 and guide pipe 3 6 upper ends are connected with the lower end of storage tank 7, and the lower end of installing pipe 6 is connected with guide pipe 3, and having in installing pipe 6 can be by storage tank 7 Middle material is transported to the conveying mechanism of guide pipe 3, and the dredging mechanism that can dredge the lower end of storage tank 7 is provided with frame 1;Feeding It is in horn-like connecting portion 4a that the both ends of pipe 4, which have, using the structure, feed pipe 4 and feeder sleeve 36 can be facilitated to link together;Point Solving device includes decomposing tank 30, locating ring 29, some air supply pipes 28, feeder sleeve 36 and air compressor machine 20, decomposes tank 30 and is arranged on machine On frame 1, decompose and be additionally provided with buffer structure between tank 30 and frame 1, using the structure, can avoid decomposing tank by buffer structure 30 and frame 1 directly contact and produce collision, it is small using noise;Buffer structure is rubber slab 25, using the structure, can make its tool There are preferably buffering and the performance of damping;Locating ring 29, which is arranged on, to be decomposed in tank 30, and locating ring 29 is located at the middle part of decomposition tank 30, The outlet side of some air supply pipes 28 is fixed on locating ring 29 through the side wall of tank 30 is decomposed, in the present embodiment, air supply pipe 28 Quantity is 12, and the outlet side of air supply pipe 28 is fixed on locating ring 29 by bolted connection;And outlet side direction The center of locating ring 29, the inlet end of air supply pipe 28 are connected by the first communicating pipe 22 with air compressor machine 20, the discharging of feeder sleeve 36 End, which is fixed on, is decomposed in tank 30, and the discharge end of feeder sleeve 36 is fixed on by connecting rod to be decomposed in tank 30;And discharge end direction is fixed Position ring 29, the feed end of feeder sleeve 36 are connected through the side wall of tank 30 is decomposed with feed pipe 4, decompose the top of tank 30 and are provided with screening Mechanism, decompose the bottom of tank 30 and be provided with recovering mechanism;Decompose and access hole 30a is further opened with tank 30, decompose and be hinged with tank 30 Can be by cover plate 37 that access hole 30a is closed;Collection device includes collecting tank 47, efferent duct 42 and output screw 40, collecting tank 47 are fixed in frame 1, and collecting tank 47 is fixed in frame 1 by bolted connection, and the upper end of collecting tank 47 has import, The import of collecting tank 47 is connected with the top of tank 30 is decomposed, and the lower end of collecting tank 47 has outlet, the outlet and output of collecting tank 47 The tube wall of pipe 42 is connected, and the outlet of collecting tank 47 is connected by the second communicating pipe 41 with the tube wall of efferent duct 42;Efferent duct 42 one end are blind end 42a, and the other end of efferent duct 42 is output end 42b, and the positioning for positioning is provided with output end 42b Part, material bag is fixed on output end 42b by keeper;The one end of output screw 40 is located in efferent duct 42, output screw 40 other ends, which pass the blind end 42a of efferent duct 42 and one, can drive its drive mechanism rotated to be connected, and be further fixed in frame 1 Baffle box 46, baffle box 46 is further fixed on by bolted connection in frame 1;The sidepiece of baffle box 46 has opening, barrier The chamber door 52 that closure of openings can be lived is hinged with case 46, the output end 42b of efferent duct 42 is located at resistance through the side wall of baffle box 46 In cell 46, being additionally provided with frame 1 can be by the dust collection mechanism of dust absorption in baffle box 46.
As shown in Figure 1 and Figure 2, conveying mechanism includes conveying axis 11 and reducing motor 2, and conveying axis 11 are horizontally set on installation In pipe 6, and conveying axis 11 are located at below the gas outlet of appendix 8, and the end of conveying axis 11 is connected with the output shaft of reducing motor 2, Reducing motor 2 is fixed in installing pipe 6, and output shaft of the end of conveying axis 11 with reducing motor 2 by way of key connection is connected; Some conveying blades 12 are fixed with conveying axis 11, are fixed with four conveying blades 12 on conveying axis 11 by way of welding.
As shown in Figure 1 and Figure 2, dredging mechanism includes appendix 8, and in the present embodiment, the quantity of appendix 8 is four, defeated The gas outlet of tracheae 8 be located in installing pipe 6 through the tube wall of installing pipe 6, and the end is vertical upward, the air inlet of appendix 8 with Air compressor machine 20 is connected, and magnetic valve 9 is provided with appendix 8, and the control that magnetic valve 9 can be controlled to work is additionally provided with frame 1 Structure;Control structure includes flexure strip 15, the controller 5 of travel switch 14 and first, and the one end of flexure strip 15 is fixed on guide pipe 3 On tube wall, one end of flexure strip 15 is fixed on by way of welding on the tube wall of guide pipe 3;The other end of flexure strip 15 is freely End, travel switch 14 are fixed on the tube wall of guide pipe 3, and travel switch 14 is fixed on guide pipe 3 by bolted connection Tube wall on, the top of travel switch 14 is additionally provided with guide housing 13, and material can be avoided to drop on travel switch 14;And stroke is opened Closing 14 can contact positioned at the top of flexure strip 15, the free end of flexure strip 15 with travel switch 14, and travel switch 14 and magnetic valve 9 are equal It is connected with first controller 5, in the present embodiment, the controller that the first controller 5 can be bought using in the market, controller Controlling the program of travel switch and magnetic valve, its program need not update to be existing.
As shown in figure 3, sorting mechanism includes screen plate 31, vibration motor 32, the asepwirator pump 34 of discharge nozzle 35 and first, screening Plate 31, which is arranged on, to be decomposed in tank 30, and screen plate 31 offers some material paths positioned at the top of tank 30 is decomposed on screen plate 31, The present embodiment, the quantity of material path is 500;Vibration motor 32 is fixed on screen plate 31 by mounting bracket 33, passes through shake Dynamic motor 32 makes screen plate 31 produce vibrations, material path can be avoided to block;The one end of discharge nozzle 35 and the decomposition top phase of tank 30 Connection, the other end of discharge nozzle 35 are connected with collecting tank 47, and the first asepwirator pump 34 is arranged in discharge nozzle 35.
As shown in figure 3, recovering mechanism includes the asepwirator pump 27 of recovery tube 26 and second, the one end of recovery tube 26 and decompose under tank 30 Portion is connected, and the other end of recovery tube 26 is connected with storage tank 7, and the second asepwirator pump 27 is arranged in recovery tube 26.
As shown in figure 3, the regulating and controlling mechanism that can adjust the flow of the first communicating pipe 22 is additionally provided with frame 1, regulating and controlling mechanism bag Include pressure sensor 23, first flow regulating valve 21 and second controller 24, pressure sensor 23 and first flow regulating valve 21 It is successively set in the first communicating pipe 22, and pressure sensor 23 is located between first flow regulating valve 21 and decomposition tank 30, pressure Force snesor 23 and first flow regulating valve 21 are connected with the second controller 24, in the present embodiment, second controller 24 The single-chip microcomputer that can be bought using in the market, it is existing, its journey that single-chip microcomputer, which controls the program of sensor and first flow regulating valve, Sequence need not update;Using the structure, signal is passed to by second controller 24, the second control by pressure sensor 23 Device 24 controls the opening degree of first flow regulating valve 21, so as to realize the dynamic regulation of the flow of the first communicating pipe 22, regulation and control Precisely.
As shown in Figure 5, Figure 6, keeper includes rubber ring 54, and rubber ring 54 is arranged and is fixed on the output end of efferent duct 42 On 42b, there are some protuberances on the lateral surface of rubber ring 54, in the present embodiment, the quantity of protuberance is 50, by convex Frictional force between rubber ring 54 and material bag can be increased by going out portion.
As shown in Figure 5, Figure 6, dust collection mechanism includes the first blower fan 53, the 3rd asepwirator pump 44 and air intake duct 45, the first blower fan 53 are fixed in baffle box 46, and the first blower fan 53 is fixed in baffle box 46 by bolted connection;And first blower fan 53 Above efferent duct 42, the air-out mouth down of the first blower fan 53, one end of air intake duct 45 is connected with the bottom of baffle box 46, air-breathing The other end of pipe 45 and the 3rd asepwirator pump 44 are connected, and filter bag 51 is provided with air intake duct 45, and filter bag 51 can using in the market With the existing product bought;Second flow regulating valve 43 is provided with air intake duct 45, using the structure, is adjusted by second flow Valve 43 can adjust the big of suction in air intake duct 45.
As shown in figure 5, drive mechanism includes motor 49, driving gear 48 and driven gear 50, motor 49 is fixed on frame 1 On, motor 49 is fixed in frame 1 by bolted connection;Driving gear 48 is fixed on the output shaft of motor 49, main Moving gear 48 is fixed on by way of key connection on the output shaft of motor 49;Driven gear 50 is fixed on output screw 40, Driven gear 50 is fixed on output screw 40 by bolted connection;Driving gear 48 is meshed with driven gear 50.
As shown in fig. 7, being further opened with observation panel in baffle box 46, transparent access panel 55 is provided with observation panel, is observed The organic plates that plate 55 can be bought using in the market, using the structure, can be viewed inside baffle box 46 by access panel 55 Operation irregularity.
As shown in figure 8, being provided with the cooling body for being cooled down to air compressor machine 20 in frame 1, cooling body includes The blower fan 69 of mounting bracket 64 and second, mounting bracket 64 are arranged in frame 1, have damping between mounting bracket 64 and frame 1 Block 63, using the structure, the vibrations at mounting bracket 64 can be reduced by snubber block 63, it is small using noise;Second blower fan 69 is logical Crossing one can drive its travel mechanism moved horizontally to be arranged in mounting bracket 64, and the second blower fan 69 is located at the top of air compressor machine 20, And second blower fan 69 air outlet towards air compressor machine 20.
As shown in Figure 8, Figure 9, travel mechanism includes the first curved guide rail 65, the first sliding block 75, installing plate 68, servo Motor 67 and gear 66, the first guide rail 65 are fixed in mounting bracket 64, and the first guide rail 65 is fixed by bolted connection In mounting bracket 64;And first guide rail 65 intrados on there is teeth 65a, the first sliding block 75 is arranged on the first guide rail 65 In, the first sliding block 75 can move along the first guide rail 65;Installing plate 68 is fixed on the first sliding block 75, and installing plate 68 passes through bolt The mode of connection is fixed on the first sliding block 75;Servomotor 67 is fixed on the upper surface of installing plate 68, and servomotor 67 passes through spiral shell Tether the upper surface that the mode connect is fixed on installing plate 68;Straight down, gear 66 is fixed on to be watched the output shaft of servomotor 67 On the output shaft for taking motor 67, gear 66 is fixed on by way of key connection on the output shaft of servomotor 67;Gear 66 with The teeth 65a of first guide rail 65 is meshed, and the second blower fan 69 can drive the elevating mechanism of its oscilaltion to be arranged on peace by one The lower surface of loading board 68.
As shown in Figure 8, Figure 9, elevating mechanism includes push-rod electric machine 71, the second sliding block 72 and the second guide rail 73, the second guide rail 73 are fixed on the lower surface of installing plate 68 by link 74, and the second sliding block 72 is arranged in the second guide rail 73, and the second sliding block 72 can Moved along the second guide rail 73;Push-rod electric machine 71 is fixed on the lower surface of installing plate 68, the side that push-rod electric machine 71 is bolted Formula is fixed on the lower surface of installing plate 68;The push rod of push-rod electric machine 71 straight down, the push rod end of push-rod electric machine 71 and second Sliding block 72 is connected, and the push rod end of push-rod electric machine 71 is connected with the second sliding block 72 by bolted connection;Second blower fan 69 It is fixed on the second sliding block 72, the second blower fan 69 is fixed on the second sliding block 72 by bolted connection.
As shown in figure 8, being additionally provided with the controlling organization that can control the start and stop of servomotor 67 in frame 1, controlling organization includes If dry temperature sensor 70, the controller 60 of display screen 61 and the 3rd, in the present embodiment, the quantity of temperature sensor 70 is four It is individual;If dry temperature sensor 70 is separately positioned on air compressor machine 20, and temperature sensor 70 is evenly arranged, and display screen 61 is fixed on In frame 1, display screen 61 is fixed in frame 1 by bolted connection;Temperature sensor 70, display screen 61 and servo electricity Machine 67 is connected with the 3rd controller 60;In the present embodiment, the monolithic that the 3rd controller 60 can be bought using in the market Machine, it is existing that single-chip microcomputer, which controls the program of sensor, motor and display screen, and its program need not update.
The operation principle of airflow comminution system is as follows:The output shaft of control reducing motor 2 drives conveying axis 11 to rotate, and conveys Axle 11 drives conveying blade 12 to rotate, former by the feedstock transportation of storage tank 7 into guide pipe 3 with the rotation of conveying blade 12 Material is entered in the presence of self gravitation in feed pipe 4, so as to realize its feeding operation;Raw material in feed pipe 4 is passed through Feeder sleeve 36, which is transported to, to be decomposed in tank 30, and the air after compression is transported to and decomposed in tank 30 by air compressor machine 20 by air supply pipe 28, Raw material is produced rub and resolve into nanoscale powder material between each other by the high speed impact of air;The first asepwirator pump 34 is opened, is accorded with The material path that desired particle passes through screen plate 31 is closed, is transported to by discharge nozzle 35 in collecting tank 47;Second is opened to inhale Air pump 27, it is transported in storage tank 7 by recovery tube 26, it is decomposed again, so as to completes its apportioned effort;Will Material bag is enclosed on the output end 42b of efferent duct 42, is positioned material bag by the elastic force of rubber ring 54, controlled motor 49 Output shaft drives driving gear 48 to rotate, and driving gear 48 drives driven gear 50 to rotate, and driven gear 50 drives output screw 40 are rotated, and with the rotation of output screw 40, the nanoscale powder material in collecting tank 47 is transported in material bag, passes through the first wind Machine 53 conveys downwards the air in baffle box 46, and dust moves down with air, by the 3rd asepwirator pump 44 by baffle box 46 dust absorption, in suction filter bag 51, so as to realize that its collects operation.
Specific embodiment described herein is only to spirit explanation for example of the invention.Technology belonging to the present invention is led The technical staff in domain can be made various modifications or supplement to described specific embodiment or be replaced using similar mode Generation, but without departing from the spiritual of the present invention or surmount scope defined in appended claims.

Claims (6)

1. the production technology of improved nanometer lithium iron phosphate cathode material, it is characterised in that comprise the technical steps that:
A, by Li source compound, ferric iron source compound, P source compound, stoichiometrically ratio adds water to mix, and adds doping Metal ion oxide and a carbon source, it is well mixed;The slurry of formation carries out a high energy Ultrafine Grinding processing 2-3h, obtains Slurry D50 is less than 0.2 μm, and spray drying obtains drying powder, sieves;Li source compound is lithium carbonate;Ferric iron source compound For Fe2O3;P source compound is FePO4;Doped metal ion oxide is MnO2、TiO2, MgO and Nb2O5;Carbon source is Portugal Grape sugar;
B, the powder in step a is pre-processed into 3-8h in 350-550 DEG C of temperature range in nitrogen, secondary carbon source is added after cooling And water, the slurry of formation is stirred, after the processing of secondary high energy Ultrafine Grinding, obtained slurry D50 is less than 0.2 μm, spray drying Spherical powder is obtained, is sieved;Secondary carbon source is chitosan;
C, the spherical powder in step b is crushed by airflow comminution system, the powder after crushing passes through in nitrogen 600-650 DEG C of processing 8-24h, then 700-960 DEG C of high-temperature heat treatment 8-16h is carried out, nano-grade lithium iron phosphate positive pole is obtained after cooling Material;Airflow comminution system in the step c includes frame, and feed device, decomposer and receipts are provided with the frame Acquisition means, the feed device include storage tank and feed pipe, and storage tank is fixed in frame, and storage tank upper end has input Mouthful, storage tank lower end is connected by guide pipe with the tube wall of feed pipe, and installing pipe is provided between storage tank and guide pipe, is pacified Tubulature upper end is connected with storage tank lower end, and installing pipe lower end is connected with guide pipe, and having in installing pipe can be by storage tank Material is transported to the conveying mechanism of guide pipe, and the dredging mechanism that can dredge storage tank lower end is provided with frame;The decomposition Device includes decomposing tank, locating ring, some air supply pipes, feeder sleeve and air compressor machine, decomposes tank and is arranged in frame, locating ring is set Decomposing in tank, and locating ring, positioned at decomposing in the middle part of tank, the outlet side of some air supply pipes is fixed on positioning through pot sidewall is decomposed On ring, and outlet side is connected towards locating ring center, the inlet end of air supply pipe by the first communicating pipe with air compressor machine, feeder sleeve Discharge end be fixed on and decompose in tank, and discharge end is towards locating ring, and the feed end of feeder sleeve is through decomposing pot sidewall and feeding Pipe is connected, and decomposes tank top and is provided with sorting mechanism, decomposes tank bottom and is provided with recovering mechanism;The collection device includes receiving Collection tank, efferent duct and output screw, collecting tank are fixed in frame, and collecting tank upper end has an import, the import of collecting tank and point Solution tank top is connected, and collecting tank lower end has outlet, and the outlet of collecting tank is connected with the tube wall of efferent duct, efferent duct one end For blind end, the efferent duct other end is output end, the keeper for positioning is provided with output end, output screw one end is located at In efferent duct, the output screw other end, which passes the blind end of efferent duct and one, can drive its drive mechanism rotated to be connected, frame On be further fixed on baffle box, baffle box sidepiece has opening, be hinged with baffle box can by closure of openings live chamber door, efferent duct Output end be located at through baffle box side wall in baffle box, being additionally provided with frame can be by the vacuum cleaner of dust absorption in baffle box Structure.
2. the production technology of improved nanometer lithium iron phosphate cathode material according to claim 2, it is characterised in that described Drive mechanism includes motor, driving gear and driven gear, and motor is fixed in frame, and driving gear is fixed on the output of motor On axle, driven gear is fixed on output screw, and driving gear is meshed with driven gear.
3. the production technology of improved nanometer lithium iron phosphate cathode material according to claim 2, it is characterised in that described The cooling body for being cooled down to air compressor machine is provided with frame, cooling body includes mounting bracket and the second blower fan, peace Dress support is arranged in frame, has snubber block between mounting bracket and frame, and the second blower fan can drive its level to move by one Dynamic travel mechanism is arranged in mounting bracket, and the second blower fan is located above air compressor machine, and the air outlet direction of the second blower fan is empty Press.
4. the production technology of improved nanometer lithium iron phosphate cathode material according to claim 3, it is characterised in that described Travel mechanism includes the first curved guide rail, the first sliding block, installing plate, servomotor and gear, and the first guide rail passes through bolt The mode of connection is fixed in mounting bracket, and has teeth on the intrados of the first guide rail, and the first sliding block is arranged on first and led In rail, installing plate is fixed on the first sliding block by bolted connection, and servomotor is fixed on installing plate upper surface, servo Straight down, gear is fixed on the output shaft of servomotor the output shaft of motor, and gear is meshed with the teeth of the first guide rail, Second blower fan can drive the elevating mechanism of its oscilaltion to be arranged on installing plate lower surface by one.
5. the production technology of improved nanometer lithium iron phosphate cathode material according to claim 4, it is characterised in that described Elevating mechanism includes push-rod electric machine, the second sliding block and the second guide rail, and the second guide rail is fixed on installing plate lower surface by link, Second sliding block is arranged in the second guide rail, and push-rod electric machine is fixed on the lower surface of installing plate, push rod by bolted connection Straight down, the push rod end of push-rod electric machine is connected the push rod of motor with the second sliding block, and the second blower fan is fixed on the second sliding block.
6. the production technology of improved nanometer lithium iron phosphate cathode material according to claim 4, it is characterised in that described The controlling organization of servomotor start and stop can be controlled by being additionally provided with frame, and controlling organization includes four temperature sensors, display screens With the 3rd controller, four temperature sensors are separately positioned on air compressor machine, and temperature sensor is evenly arranged, and display screen is fixed In frame, temperature sensor, display screen and servomotor are connected with the 3rd controller.
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