CN203890063U - Continuous lithium iron phosphate preparation device - Google Patents

Continuous lithium iron phosphate preparation device Download PDF

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Publication number
CN203890063U
CN203890063U CN201420118533.5U CN201420118533U CN203890063U CN 203890063 U CN203890063 U CN 203890063U CN 201420118533 U CN201420118533 U CN 201420118533U CN 203890063 U CN203890063 U CN 203890063U
Authority
CN
China
Prior art keywords
reactor
lithium phosphate
preparation device
iron lithium
reaction pipe
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
CN201420118533.5U
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Chinese (zh)
Inventor
何向明
王莉
罗晶
李建军
张建利
徐程浩
尚玉明
高剑
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tsinghua University
Jiangsu Huadong Institute of Li-ion Battery Co Ltd
Original Assignee
Tsinghua University
Jiangsu Huadong Institute of Li-ion Battery Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tsinghua University, Jiangsu Huadong Institute of Li-ion Battery Co Ltd filed Critical Tsinghua University
Priority to CN201420118533.5U priority Critical patent/CN203890063U/en
Application granted granted Critical
Publication of CN203890063U publication Critical patent/CN203890063U/en
Priority to PCT/CN2015/070980 priority patent/WO2015139527A1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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
    • 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
    • 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)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The utility model relates to a lithium iron phosphate preparation device comprising a continuous lithium iron phosphate preparation device. The continuous lithium iron phosphate preparation device comprises a raw material tank, a reaction kettle, an intermediate pump, a continuous reaction pipe, a product storage tank and a gas input device, wherein the feed port of the reaction kettle is connected with the raw material tank by virtue of a sealed pipeline; the intermediate pump is respectively connected with the discharge port of the reaction kettle and the continuous reaction pipe by virtue of the sealed pipeline to ensure that materials are continuously transported to the continuous reaction pipe from the reaction kettle and are output to the product storage tank; one end of the continuous reaction pipe is connected with the intermediate pump, and the other end of the continuous reaction pipe is connected with the product storage tank by virtue of the sealed pipeline; the gas input device is respectively connected with the reaction kettle and the product storage tank by virtue of the sealed pipeline to ensure that predetermined reaction pressure can be maintained in the reaction kettle and the continuous reaction pipe.

Description

Iron lithium phosphate continuous preparation device
Technical field
The utility model relates to a kind of iron lithium phosphate continuous preparation device.
Background technology
Energy problem is a significant problem of human society and scientific technological advance always.Lithium ion battery, as the higher green secondary cell of energy density, has been widely used in the consumption electronic products such as notebook computer, mobile phone, Kamera.
Iron lithium phosphate has a better security as a kind of, and cheap and environment amenable anode active material of lithium ion battery is subject to people always and greatly pays close attention to.The in vitro synthetic method of iron lithium phosphate mainly contains high temperature solid-state method, spray method, hydrothermal synthesis method, coprecipitation method, emulsion desiccating method and microwave process for synthesizing etc. at present.Mainly synthetic on a large scale by high temperature solid-state method at industrial iron lithium phosphate.Yet high temperature solid-state method need to carry out sintering under comparatively high temps, product granularity is larger, poor-performing.Hydrothermal Synthesis and solvent thermal are synthetic is to synthesize at a lower temperature the method for the iron lithium phosphate of reduced size crystal grain.Yet these two kinds of synthetic methods need to be positioned over raw material pressurized, heated in the autoclave of sealing, each synthetic output is subject to the restriction of autoclave volume, is difficult to be applied to large-scale industrialization and produces.And synthetic iron lithium phosphate is easily subject to the impact of reaction conditions difference in batches, the iron lithium phosphate product performance that different batches is produced are inconsistent.
Summary of the invention
In view of this, necessaryly provide a kind of iron lithium phosphate continuous preparation device, by this device, can realize the continuous production of iron lithium phosphate hydrothermal synthesis method, meet industrialization product consistence needs.
A kind of iron lithium phosphate preparation facilities, comprise a kind of iron lithium phosphate continuous preparation device, comprise head tank, reactor, line pump, successive reaction pipe, product storage tank and gas input device, the opening for feed of this reactor is connected with this head tank by airtight pipeline, this line pump is connected by airtight pipeline with discharge port and this successive reaction pipe of this reactor respectively, make material continuously from this reactor, be delivered to this successive reaction pipe, and export this product storage tank to, one end of this successive reaction pipe is connected with this line pump, the other end is connected by airtight pipeline with this product storage tank, this gas input device is connected by airtight pipeline with this reactor and this product storage tank respectively, make to maintain predetermined reaction pressure in reactor and successive reaction pipe.
The utility model is divided into two parts by the original reactor of hydrothermal synthesis method, be stirring reaction device and temperature-controlling reaction apparatus, and provide these two pressure that device is required by gas input device, make these two devices of the continuous process of raw material, can realize in material operational process and constantly react and generate iron lithium phosphate, can realize product heavy industrialization and produce continuously, greatly improve the consistence of iron lithium phosphate product.
Accompanying drawing explanation
Fig. 1 is the structural representation of the utility model embodiment iron lithium phosphate continuous preparation device.
Main element nomenclature
Iron lithium phosphate continuous preparation device 1
Head tank 10
Volume pump 12
Reactor 20
Heating jacket 22
Agitator 24
Frequency transformer 26
Baiting valve 28
Thermopair 30
Line pump 40
Successive reaction pipe 50
Thermostatical oil bath cabinet 52
Well heater 54
Gas input device 60
Pressure gas tank 62
Strainer 64
Reducing valve 66
Check valve 68
Ball valve 70
Pressure-detecting device 80
Product storage tank 90
Back pressure valve 92
Following embodiment further illustrates the utility model in connection with above-mentioned accompanying drawing.
Embodiment
The iron lithium phosphate continuous preparation device below in conjunction with the accompanying drawings and the specific embodiments the utility model being provided is described in further detail.
Refer to Fig. 1, the utility model provides a kind of iron lithium phosphate continuous preparation device 1, for passing through hydrothermal synthesis method or solvent thermal synthesis method continuous production iron lithium phosphate, this iron lithium phosphate continuous preparation device 1 comprises head tank 10, mixed stirring device, line pump 40, temperature-controlling reaction apparatus, product storage tank 90 and gas input device 60.
This head tank 10 is for storing the material solution of Hydrothermal Synthesis or solvent thermal synthesizing iron lithium phosphate, the present embodiment comprises two head tanks 10, one of them head tank 10 stores ferrous phosphate solution, and another head tank 10 stores phosphoric acid and the reacted solution of lithium hydroxide.
This mixed stirring device is for evenly mixing mixed being incorporated under predetermined temperature and pressure of material solution.This mixed stirring device comprises reactor 20, heating jacket 22 and agitator 24.The opening for feed of this reactor 20 is connected with head tank 10 by airtight pipeline, on the airtight pipeline between head tank 10 and reactor 20, volume pump 12 can be further set, operating pressure is 0~2MPa, for material solution being transported to reactor 20 and controlling the ratio between the material solution of carrying from different head tanks 10.This agitator 24 is arranged on reactor 20 inside, it can be specifically the agitator arm with stirring arm, this agitator 24 can be arranged on the outside electric control gear of reactor 20 and be connected, this electric control gear can have frequency transformer 26, for adjusting the rotating speed of agitator 24, this rotating speed can be 0~200 rev/min.This heating jacket 22 is arranged on this reactor 20 outsides, for this reactor 20 is heated and is incubated, and specifically can be around these reactor 20 outer wall settings.This mixed stirring device can further comprise a temperature measurer, as thermopair 30, the temperature of these reactor 20 inside is measured.This mixed stirring device is mainly material solution evenly will be mixed, and in this mixed stirring device, chemical reaction can not occur material solution.For enhancing productivity, also can make material solution in this mixed stirring device, start to occur chemical reaction, carry out the reaction of hydro-thermal or solvent thermal synthesizing iron lithium phosphate.The working temperature of these reactor 20 inside can be at 25~250 ℃, and operating pressure can be at 0~1.6MPa, and volume can be 10L to 20L.The discharge port of this reactor 20 can be positioned on the bottom or sidewall of reactor 20, when being positioned at the sidewall of reactor 20, the centrifugal force producing due to the stirring of agitator 24 can make reacted material excessive from the discharge port of sidewall, when being positioned at the bottom of reactor 20, material flows out naturally by action of gravity.This reactor 20 can further comprise a baiting valve 28, is arranged on discharge port place, for controlling the discharge of reactor 20 materials inside.This reactor 20 can enter one and have gas barrier, as needle valve, for controlling reactor 20 internal pressures at predetermined interval.
This temperature-controlling reaction apparatus comprises thermostatical oil bath cabinet 52 and is arranged on the successive reaction pipe 50 in this thermostatical oil bath cabinet 52.This temperature-controlling reaction apparatus is for to heating under predetermined pressure through the material of this successive reaction pipe 50, and makes the process of material by whole successive reaction pipe 50 all in constant temperature and pressure state, thereby carries out hydro-thermal or solvent thermal reaction.Pressure in this successive reaction pipe 50 is regulated by gas input device 60.This successive reaction pipe 50 has the time sufficiently long that enough length stops material in successive reaction pipe 50.Particularly, material can be 2 hours~6 hours in the residence time of this successive reaction pipe 50, corresponding, the length of this successive reaction pipe 50 can be 10 meters~20 meters, internal diameter can be 5 millimeters~20 millimeters.This successive reaction pipe 50 can be crooked be arranged in this thermostatical oil bath cabinet 52 to save space.This thermostatical oil bath cabinet 52 heats by well heater 54, makes inner oil temperature evenly constant, and the operating temperature range of this thermostatical oil bath cabinet 52 can be 5~250 ℃.This temperature-controlling reaction apparatus can further comprise temperature measurer, as thermopair 30, the temperature of the oil temperature of thermostatical oil bath cabinet 52 inside and well heater 54 is measured.
This line pump 40 is arranged between this reactor 20 and this successive reaction pipe 50, is connected respectively with discharge port and this successive reaction pipe 50 of this reactor 20 by airtight pipeline.This line pump 40 is for being continuously input to the material of reactor 20 in successive reaction pipe 50, and fine adjustment mass flow, the time that material is stopped through successive reaction pipe 50 is controlled, finally by this successive reaction pipe 50, exports this product storage tank to.This line pump 40 can adopt surge pump, and rated flow can be at 0~2 l/h, and can to flow, adjust by frequency transformer, and top hole pressure can be 0~2MPa.One end of this successive reaction pipe 50 is connected by line pump 40 with this reactor 20, and the other end is connected with product storage tank 90.This reactor 20 can regulate respectively by gas input device 60 with the pressure in this successive reaction pipe 50, thereby can be identical or different.
This gas input device 60 is connected by airtight pipeline with this reactor 20 and this product storage tank 90 respectively; for high voltage protective gas is constantly inputed to this reactor 20 and this product storage tank 90, make in reactor 20 and successive reaction pipe 50, to maintain predetermined reaction pressure in tandem reaction sequence.This shielding gas can be hydrogen or nitrogen.This gas input device 60 can comprise pressure gas tank 62, strainer 64 and the reducing valve 66 connecting by pipeline liquid injecting device.High pressure gas in this pressure gas tank 62 are decompressed to suitable reaction pressure through reducing valve 66 after filtering by strainer 64, by pipeline liquid injecting device, are delivered to respectively this reactor 20 and this product storage tank 90.Further, a check valve 68 can be set in the exit of this gas input device 60, to protect this gas input device 60.This product storage tank 90 can be connected with back pressure valve 92, makes product storage tank 90 internal pressures in reaction process be no more than predetermined pressure.The volume of this product storage tank 90 can be 10L~20L, and inner operating temperature range can be 0~250 ℃, and working pressure range can be 0~1.6MPa.On the pipeline of this connection gas input device 60 and reactor 20 and product storage tank 90, can be provided with valve, as ball valve, thereby the gaseous tension of output be regulated, the connecting pipeline between this product storage tank 90 and this successive reaction pipe 50 also can be provided with ball valve.
The different positions of this iron lithium phosphate continuous preparation device 1 can be respectively arranged with pressure-detecting device 80, each is installed to inner pressure, monitor, for example in the inside of this gas input device 60 and entrance and the product storage tank inside of outlet, successive reaction pipe 50 be provided with pressure-detecting device 80.The different positions of this iron lithium phosphate continuous preparation device 1 can be respectively arranged with valve, as ball valve 70, so that preparation facilities 1 is carried out to segmentation control and maintenance.
In the continuous production process of this iron lithium phosphate, material solution is extracted out by volume pump 12 respectively from head tank 10 separately, is input in reactor 20.20 heating of 22 pairs of reactors of this heating jacket, 24 pairs of material solutions of agitator stir, gas input device 60 passes into gas in reactor 20, make the pressure of reactor 20 be increased to predetermined pressure range, make material solution evenly mixed being incorporated under predetermined pressure and temperature condition, carry out preliminary pre-reaction.According to hydro-thermal or solvent thermal reaction principle, the crystallization under this temperature and pressure condition of iron lithium phosphate product crystal grain generates.The residence time of material in this reactor 20 determined by the difference between input speed and discharging speed, can adjust by adjusting the flow of volume pump and line pump, makes material stop enough time in this reactor 20, to reach the object of pre-reaction.Material after pre-reaction is transported to successive reaction pipe 50 by line pump 40, by this thermostatical oil bath cabinet 52, make the temperature of successive reaction pipe 50 remain on the preset temperature interval of reaction, and these successive reaction pipe 50 inside still keep this predetermined reaction pressure, therefore this hydro-thermal or solvent thermal reaction can be proceeded, iron lithium phosphate product crystal grain is on the increase, the process that the length of this successive reaction pipe 50 can make material advance from entrance to outlet, can stop the sufficiently long reaction times, the product generating after completion of the reaction inputs to this product storage tank 90.This gas input device 60 makes product storage tank 90 identical with the pressure of reactor 20, thereby can make successive reaction pipe 50 inside of between UNICOM have identical pressure.
The utility model is divided into two parts by the original reactor of hydrothermal synthesis method, be stirring reaction device and temperature-controlling reaction apparatus, and provide these two pressure that device is required by gas input device, make these two devices of the continuous process of raw material, can realize in the operational process of material and constantly react and generate iron lithium phosphate, and can obtain good crystal habit, and can realize product heavy industrialization and produce continuously, greatly improve the consistence of iron lithium phosphate product.
In addition, those skilled in the art also can do other and change in the utility model spirit, and certainly, the variation that these are done according to the utility model spirit, within all should being included in the utility model scope required for protection.

Claims (10)

1. an iron lithium phosphate continuous preparation device, it is characterized in that, comprise head tank, reactor, line pump, successive reaction pipe, product storage tank and gas input device, the opening for feed of this reactor is connected with this head tank by airtight pipeline, this line pump is connected by pipeline with discharge port and this successive reaction pipe of this reactor respectively, one end of this successive reaction pipe is connected with this line pump, the other end is connected by pipeline with this product storage tank, and this gas input device is connected by pipeline with this reactor and this product storage tank respectively.
2. iron lithium phosphate continuous preparation device as claimed in claim 1, is characterized in that, further comprises the volume pump on the airtight pipeline being arranged between head tank and reactor.
3. iron lithium phosphate continuous preparation device as claimed in claim 1, is characterized in that, further comprises heating jacket that this reactor is heated and at the agitator of this reactor inside.
4. iron lithium phosphate continuous preparation device as claimed in claim 1, is characterized in that, further comprises the thermostatical oil bath cabinet that this successive reaction pipe is heated, and this successive reaction pipe is arranged in this thermostatical oil bath cabinet.
5. iron lithium phosphate continuous preparation device as claimed in claim 1, is characterized in that, the length of this successive reaction pipe is 10 meters~20 meters, and internal diameter is 5 millimeters~20 millimeters.
6. iron lithium phosphate continuous preparation device as claimed in claim 4, is characterized in that, being arranged in this thermostatical oil bath cabinet of this successive reaction pipe bending.
7. iron lithium phosphate continuous preparation device as claimed in claim 1, is characterized in that, the rated flow of this line pump is 0~2 l/h.
8. iron lithium phosphate continuous preparation device as claimed in claim 1, is characterized in that, this gas input device comprises pressure gas tank, strainer and the reducing valve connecting by pipeline liquid injecting device.
9. iron lithium phosphate continuous preparation device as claimed in claim 1, is characterized in that, further comprises the check valve that is arranged on this gas input device exit.
10. iron lithium phosphate continuous preparation device as claimed in claim 1, is characterized in that, further comprises the back pressure valve being connected with this product storage tank.
CN201420118533.5U 2014-03-17 2014-03-17 Continuous lithium iron phosphate preparation device Expired - Lifetime CN203890063U (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201420118533.5U CN203890063U (en) 2014-03-17 2014-03-17 Continuous lithium iron phosphate preparation device
PCT/CN2015/070980 WO2015139527A1 (en) 2014-03-17 2015-01-19 Device for continuously preparing lithium iron phosphate

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Application Number Priority Date Filing Date Title
CN201420118533.5U CN203890063U (en) 2014-03-17 2014-03-17 Continuous lithium iron phosphate preparation device

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015139527A1 (en) * 2014-03-17 2015-09-24 江苏华东锂电技术研究院有限公司 Device for continuously preparing lithium iron phosphate
CN104986796A (en) * 2015-06-09 2015-10-21 张家港合志纳米科技有限公司 Device system and preparation technology for preparing submicron material through continuous hydrothermal method
WO2016119518A1 (en) * 2015-01-28 2016-08-04 江苏华东锂电技术研究院有限公司 Continuous lithium iron phosphate preparation device and preparation method
CN106129408A (en) * 2016-08-29 2016-11-16 张家港合志纳米科技有限公司 Solvent-thermal method is utilized to prepare technique and the device of low specific surface high electrochemical performance LFP
CN106379877A (en) * 2015-12-27 2017-02-08 天津赫维科技有限公司 Continuous preparation device of iron phosphate
CN110589790A (en) * 2019-10-25 2019-12-20 嘉兴双军环保科技有限公司 Phosphating slag recycling treatment mechanism
CN114348986A (en) * 2021-12-31 2022-04-15 江苏贝特瑞纳米科技有限公司 Lithium iron phosphate production equipment and preparation method thereof

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CN114768686A (en) * 2022-05-19 2022-07-22 济宁长兴塑料助剂有限公司 Closed feeding system for DOTP synthesis
CN114956188B (en) * 2022-06-19 2023-09-29 安徽大学 Method for continuously preparing manganese dioxide with specific crystal form by microfluidic control

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CN201634424U (en) * 2009-12-25 2010-11-17 北京工业大学 Device for continuously producing LiFePO4 via industrial utilization of hydro-thermal reaction
CN101759173B (en) * 2009-12-25 2011-07-27 北京工业大学 Device for continuously producing LiFeP04 by utilizing hydro-thermal reaction in industry
CN203890063U (en) * 2014-03-17 2014-10-22 江苏华东锂电技术研究院有限公司 Continuous lithium iron phosphate preparation device

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015139527A1 (en) * 2014-03-17 2015-09-24 江苏华东锂电技术研究院有限公司 Device for continuously preparing lithium iron phosphate
WO2016119518A1 (en) * 2015-01-28 2016-08-04 江苏华东锂电技术研究院有限公司 Continuous lithium iron phosphate preparation device and preparation method
CN104986796A (en) * 2015-06-09 2015-10-21 张家港合志纳米科技有限公司 Device system and preparation technology for preparing submicron material through continuous hydrothermal method
CN104986796B (en) * 2015-06-09 2016-05-25 张家港合志纳米科技有限公司 Serialization hydro-thermal method is prepared apparatus system and the preparation technology thereof of submicron material
CN106379877A (en) * 2015-12-27 2017-02-08 天津赫维科技有限公司 Continuous preparation device of iron phosphate
CN106129408A (en) * 2016-08-29 2016-11-16 张家港合志纳米科技有限公司 Solvent-thermal method is utilized to prepare technique and the device of low specific surface high electrochemical performance LFP
CN106129408B (en) * 2016-08-29 2018-09-11 张家港合志纳米科技有限公司 The technique and device of low specific surface high electrochemical performance LFP are prepared using solvent-thermal method
CN110589790A (en) * 2019-10-25 2019-12-20 嘉兴双军环保科技有限公司 Phosphating slag recycling treatment mechanism
CN114348986A (en) * 2021-12-31 2022-04-15 江苏贝特瑞纳米科技有限公司 Lithium iron phosphate production equipment and preparation method thereof
CN114348986B (en) * 2021-12-31 2023-01-17 江苏贝特瑞纳米科技有限公司 Lithium iron phosphate production equipment and preparation method thereof

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