CN103779540A - Lithium-ion cell material synthesis device and synthesis method thereof - Google Patents
Lithium-ion cell material synthesis device and synthesis method thereof Download PDFInfo
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- CN103779540A CN103779540A CN201410016754.6A CN201410016754A CN103779540A CN 103779540 A CN103779540 A CN 103779540A CN 201410016754 A CN201410016754 A CN 201410016754A CN 103779540 A CN103779540 A CN 103779540A
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- ion battery
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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
- H01M4/58—Selection 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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
Abstract
The invention discloses a lithium-ion cell material synthesis device and a synthesis method thereof. The synthesis device comprises an atomization feeder, a fluidized bed reactor, a separator and an exhaust purifier, wherein the atomization feeder comprises a raw material storage tank, a high-pressure gas storage tank and an atomization nozzle; the atomization nozzle is arranged in an inner cavity of a fluidized bed; the high-pressure gas storage tank is connected with the raw material storage tank; the raw material storage tank is connected to the atomization nozzle; the top end of the fluidized bed reactor is connected with the separator through a pipeline; a temperature control heating element is mounted on the external wall of the fluidized bed reactor; the top end of the separator is connected with the exhaust purifier through a pipeline; the bottom of the separator is connected with a lower end of the side wall of the fluidized bed reactor through a pipeline; and a three-way valve and a discharging opening are formed in the pipeline at the bottom of the separator. The lithium-ion cell material synthesis method comprises the steps of spraying the raw material of a lithium-ion cell into the fluidized bed reactor in the form of mist to perform fast pyrolysis reaction, then performing gas-solid separation and returning solids generated by the reaction to the fluidized bed reactor or discharging from the discharging opening to obtain a lithium-ion cell material.
Description
Technical field
The present invention relates to lithium ion battery material preparation field, relate in particular to a kind of particle diameter controlled lithium ion battery material synthesis device and synthetic method.
Background technology
At present, lithium ion battery material LiFePO4, LiMn2O4, nickel LiMn2O4, ternary material, lithium titanate etc. all adopt the methods such as conventional solid-phase ball milling method, coprecipitation, sol-gal process or hydro thermal method to produce, and in recent years also have the report spray pyrolysis such as document CN102148374, CN103043639 simultaneously in conjunction with the novel battery such as wet ball grinding and microwave sintering material synthesis method.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of synthesis device of lithium ion battery material.
Another technical problem that the present invention will solve is to provide a kind of synthetic method of lithium ion battery material.
For lithium ion battery material synthesis device, lithium ion battery material comprises LiFePO4, ternary material, lithium titanate, LiMn2O4, nickel LiMn2O4 and rich lithium material, and the technical solution used in the present invention is: comprise atomized feed device, fluidized-bed reactor, separator and exhaust purifier; Atomized feed device comprises raw material storage tank, high pressure gas storage tank and is placed in the atomizer of fluid bed inner chamber, and high pressure gas storage tank is connected with raw material storage tank, and raw material storage tank is connected to atomizer; The top of fluidized-bed reactor is connected with separator by pipeline, and fluidized-bed reactor outer wall is equipped with temperature control heating element; The top of separator is connected with exhaust purifier by pipeline, the bottom of separator is connected with fluidized-bed reactor from the side wall lower ends of fluidized-bed reactor by connecting pipe, separator bottom is also provided with three-way valve and discharging opening, the break-make of three-way valve control connecting pipe and discharging opening.
As preferably, the bottom of fluidized-bed reactor is connected with fluidized carrier gas heater by pipeline.
As preferably, atomizer is arranged on top, bottom or the sidewall of fluidized-bed reactor inner chamber.
As preferably, temperature control heating element is the electrical heating elements with temperature control equipment.
As preferably, exhaust purifier comprises dust cleaning apparatus, tail gas absorber and induced draft fan; Dust cleaning apparatus, tail gas absorber and induced draft fan are connected by pipeline successively.
As preferably, dust cleaning apparatus is sack cleaner; Tail gas absorber is the pneumatic filter that is filled with physics or chemosorbent.
As preferably, separator is cyclone separator.
Lithium ion battery material synthesis device provided by the invention, target lithium ion battery material needed raw material is sprayed into fluidized-bed reactor by feeder atomization and carry out fast pyrogenation reaction, after separator carries out gas solid separation, the solid that reaction produces is got back in fluidized-bed reactor or from discharging opening and is discharged and obtain lithium ion battery material by separator bottom pipe.The circular response time by the three-way valve control pressed powder of separator bottom in high-temperature fluidized bed device, guarantee the fully reaction in fluidized-bed reactor of each raw material, reach synthetic required particle diameter and the degree of crystallinity of target battery material.
The slurry that lithium ion battery material synthesis device provided by the invention also can meet wet ball grinding gained is that raw material carries out spray pyrolysis, but follow-uply need to add other solid-phase sintering operations, the accuracy of the stoichiometric proportion of guarantee resulting materials.
For lithium ion battery material synthetic method, lithium ion battery material comprises LiFePO4, ternary material, lithium titanate, LiMn2O4, nickel LiMn2O4 and rich lithium material, the technical solution used in the present invention is: the raw material of lithium ion battery material is carried out to fast pyrogenation reaction with the vaporific fluidized-bed reactor that sprays into, after gas solid separation, the solid that reaction produces is got back in fluidized-bed reactor or from discharging opening and is discharged and obtain lithium ion battery material.
As preferably, the preferred homogeneous solution state of the raw material of lithium ion battery material mixture.
As preferably, fast pyrogenation reaction temperature is 300~1100 ℃.
Lithium ion battery material synthetic method of the present invention, in order to ensure raw material spraying into not segregation while forming fluidisation state in fluidized-bed reactor, guarantee the chemical element proportioning of synthetic material, adopting uniform solution mixture is raw material, what during as synthetic nickel LiMn2O4, in raw material storage tank, store can be the water solution mixture of lithium nitrate, nickel nitrate and the manganese nitrate of stoichiometric proportion, and what when synthetic LiFePO4/C, in raw material storage tank, store can be the water solution mixture of lithium nitrate, ferric nitrate, phosphoric acid and the glucose of stoichiometric proportion.
The invention has the beneficial effects as follows:
The particle diameter that can realize synthetic material is uniformly distributed, meanwhile, the particle diameter of finished-product material can be by material the time of staying in fluidized-bed reactor control; Consersion unit can intermittent operation, also can realize continous way operation, meets different production status demands.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is the structural representation of the present invention for the synthetic special equipment embodiment of lithium ion battery material.
1-raw material storage tank, 2-nitrogen cylinder, 3-fluidized-bed reactor (high 2m, internal diameter 0.5m), 4-cyclone separator, 5-bag-type dust collector, 6-tail gas absorber, 7-is placed in the atomizer (nozzle can be arranged on fluid bed top, side or bottom) of fluid bed inner cavity top, 8-fluidized carrier gas heater, 9-electrical heating elements, 10-three-way valve, 11-induced draft fan.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but the present invention is not limited to following examples.
Fig. 1 is for the synthetic special equipment of lithium ion battery material, is made up of atomized feed device, fluidized-bed reactor 3, cyclone separator 4 and exhaust purifier.Lithium ion battery material comprises LiFePO4, ternary material, lithium titanate, LiMn2O4, nickel LiMn2O4 and rich lithium material.
Wherein, atomized feed device is made up of raw material storage tank 1, nitrogen cylinder 2 and the atomizer 7 that is placed in fluid bed inner cavity top, and nitrogen cylinder 2 is connected with raw material storage tank 1, and raw material storage tank 1 is connected to atomizer.
In addition, atomizer can also be arranged on side or the bottom of fluid bed.
Exhaust purifier is made up of bag-type dust collector 5, tail gas absorber 6 and induced draft fan 11.Bag-type dust collector 5, tail gas absorber 6 and induced draft fan 11 are connected by pipeline successively.Wherein tail gas absorber 6 is for being filled with the pneumatic filter of physics or chemosorbent.
The height of fluidized-bed reactor 3 is 2m, and the diameter of inner chamber is 0.5m.The top of fluidized-bed reactor 3 is connected with cyclone separator 4 by pipeline, and fluidized-bed reactor outer wall is equipped with the electrical heating elements 9 of temperature control.In addition, the bottom of fluidized-bed reactor 3 is connected with fluidized carrier gas heater 8 by pipeline.
The top of cyclone separator 4 is connected with bag-type dust collector 5 by pipeline, then connects successively tail gas absorber 6 and induced draft fan 11.
The bottom of cyclone separator 4 is connected with the side wall lower ends of fluidized-bed reactor 3 by pipeline, three-way valve 10 is housed in separator bottom pipe, discharging opening is located at the end of bottom pipe, and three-way valve 10 is controlled the switching of being communicated with of cyclone separator 4 and fluidized-bed reactor 3 and discharging opening.
Embodiment 1:
In raw material storage tank 1, add concentration to be the aqueous solution of lithium nitrate, nickel nitrate and the manganese nitrate of 3mol/L by the stoichiometric proportion of Li:Ni:Mn=1.01:0.5:1.5, stir and form homogeneous solution, regulating raw material storage tank 1 internal pressure by nitrogen cylinder 2 Pressure gauges, is 2L/min thereby control sprays into 900 ± 10 ℃ of materials in fluidized-bed reactor by atomizer from fluidized-bed reactor 3 tops; Take air as fluidized carrier gas, the temperature of carrier gas heater is controlled at 900 ± 10 ℃, and carrier gas flux is 10 m3/h.Adopt batch (-type) synthesis mode, under the condition of opening in carrier gas, regulating three-way valve door 10 is closed discharging opening, open the connecting pipe between separator and fluidized-bed reactor, atomized feed 5min continuously, raw material is again got back in fluidized-bed reactor by bottom pipe from cyclone separator 4 pressed powder out after 900 ℃ of fast pyrogenations, form ciculation fluidized, state keeps 20min according to this, last regulating three-way valve door 10 is closed ciculation fluidized loop and opens discharging opening, collects from cyclone separator 4 pressed powder out.XRD characterization result shows that this powder is spinel-type nickel lithium manganate battery material.In this process, tail gas, after bag-type dust, is discharged after the 2mol/L NaOH aqueous solution absorbs, and can again introduce in fluid bed as fluid bed carrier gas circulation.
Embodiment 2:
With embodiment 1 identical parameters and the synthetic nickel lithium manganate material of method, control the ciculation fluidized 1h of material, obtain nickel lithium manganate material, characterize through SEM, the present embodiment resulting materials is compared with the large 0.5um of embodiment 1 resulting materials average primary particle diameter.Thereby the control ciculation fluidized time of material can be controlled the particle diameter of material.
Embodiment 3:
In raw material storage tank 1 by Li:Fe:P: the stoichiometric proportion of glucose=1.02:1:1:0.1 adds concentration to be the aqueous solution of lithium nitrate, ferric nitrate, phosphoric acid and the glucose of 3mol/L, stir and form homogeneous solution, regulating raw material storage tank 1 internal pressure by nitrogen cylinder 2 Pressure gauges, is 1.5L/min thereby control sprays into 680 ± 10 ℃ of materials in fluidized-bed reactor by atomizer from fluidized-bed reactor 3 bottoms; Take high pure nitrogen as fluidized carrier gas, the temperature of carrier gas heater is controlled at 680 ± 10 ℃, and carrier gas flux is 7m3/h.Adopt continous way synthesis mode, under the condition of opening in carrier gas, atomized feed continuously, it is that open mode the ciculation fluidized loop that keeps cyclone separator 4 to be connected with fluidized-bed reactor 3 are closed condition that regulating three-way valve door 10 makes discharging opening, directly collect from cyclone separator 4 black solid powder out, XRD characterization result shows that this powder is ferric phosphate lithium cell material.In this process, tail gas, after bag-type dust, is discharged after the 2mol/L NaOH aqueous solution absorbs.
Embodiment 4:
In raw material storage tank 1 by Li:Fe:P: the stoichiometric proportion of glucose=1.02:1:1:0.1 adds concentration to be the lithium dihydrogen phosphate of 3mol/L and the aqueous solution of glucose and nanometer di-iron trioxide, ultrasonic being uniformly dispersed, regulating raw material storage tank 1 internal pressure by nitrogen cylinder 2 Pressure gauges, is 1L/min thereby control sprays into 730 ± 10 ℃ of materials in fluidized-bed reactor by atomizer from fluidized-bed reactor 3 bottoms; Take high pure nitrogen as fluidized carrier gas, the temperature of carrier gas heater is controlled at 730 ± 10 ℃, and carrier gas flux is 6m3/h.Adopt continous way synthesis mode, under the condition of opening in carrier gas, atomized feed continuously, it is that open mode the ciculation fluidized loop that keeps cyclone separator 4 to be connected with fluidized-bed reactor 3 are closed condition that regulating three-way valve door 10 makes discharging opening, directly collect from cyclone separator 4 black solid powder out, XRD characterization result shows that this powder is ferric phosphate lithium cell material.In this process, tail gas, after bag-type dust, is discharged after activated carbon filtration purifies, and also can again introduce in fluid bed as fluid bed carrier gas circulation.
Above-described embodiment of the present invention, does not form limiting the scope of the present invention.Any modification of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in claim protection range of the present invention.
Claims (10)
1. a lithium ion battery material synthesis device, described lithium ion battery material comprises LiFePO4, ternary material, lithium titanate, LiMn2O4, nickel LiMn2O4 and rich lithium material; It is characterized in that: comprise atomized feed device, fluidized-bed reactor, separator and exhaust purifier; Described atomized feed device comprises raw material storage tank, high pressure gas storage tank and is placed in the atomizer of fluid bed inner chamber, and described high pressure gas storage tank is connected with raw material storage tank, and described raw material storage tank is connected to atomizer; The top of described fluidized-bed reactor is connected with described separator by pipeline, and described fluidized-bed reactor outer wall is equipped with temperature control heating element; The top of described separator is connected with exhaust purifier by pipeline, the bottom of described separator is connected with fluidized-bed reactor from the side wall lower ends of fluidized-bed reactor by connecting pipe, described separator bottom is also provided with three-way valve and discharging opening, the break-make of described three-way valve control connecting pipe and discharging opening.
2. lithium ion battery material synthesis device according to claim 1, is characterized in that: the bottom of described fluidized-bed reactor is connected with fluidized carrier gas heater by pipeline.
3. lithium ion battery material synthesis device according to claim 1 and 2, is characterized in that: described atomizer is arranged on top, bottom or the sidewall of fluidized-bed reactor inner chamber.
4. lithium ion battery material synthesis device according to claim 1, is characterized in that: described temperature control heating element is the electrical heating elements with temperature control equipment.
5. lithium ion battery material synthesis device according to claim 1 and 2, is characterized in that: described exhaust purifier comprises dust cleaning apparatus, tail gas absorber and induced draft fan; Described dust cleaning apparatus, tail gas absorber and induced draft fan are connected by pipeline successively.
6. lithium ion battery material synthesis device according to claim 5, is characterized in that: described dust cleaning apparatus is sack cleaner; Described tail gas absorber is the pneumatic filter that is filled with physics or chemosorbent.
7. lithium ion battery material synthesis device according to claim 1, is characterized in that: described separator is cyclone separator.
8. a lithium ion battery material synthetic method, described lithium ion battery material comprises LiFePO4, ternary material, lithium titanate, LiMn2O4, nickel LiMn2O4 and rich lithium material; It is characterized in that: the raw material of lithium ion battery material is carried out to fast pyrogenation reaction with the vaporific fluidized-bed reactor that sprays into, and after gas solid separation, the solid that reaction produces is got back in fluidized-bed reactor or from discharging opening and discharged and obtain lithium ion battery material.
9. lithium ion battery material synthetic method according to claim 8, is characterized in that: the preferred homogeneous solution state of the raw material mixture of described lithium ion battery material.
10. lithium ion battery material synthetic method according to claim 8 or claim 9, is characterized in that: described fast pyrogenation reaction temperature is 300~1100 ℃.
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CN105244491A (en) * | 2015-10-20 | 2016-01-13 | 四川科能锂电有限公司 | Technology for preparing lithium titanate lithium-ion battery anode material |
CN105990569A (en) * | 2015-02-13 | 2016-10-05 | 中国科学院大连化学物理研究所 | Preparation method of sulfur-carbon composite powder material, powder material, and application of powder material |
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CN106602045A (en) * | 2017-02-18 | 2017-04-26 | 山东六聚新材料科技有限公司 | Pneumatic fluidized coating device and lithium ion battery cathode material coating process |
JP2018502035A (en) * | 2014-11-26 | 2018-01-25 | ビーエーエスエフ ソシエタス・ヨーロピアBasf Se | Method for producing lithiated transition metal oxide |
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CN109666918A (en) * | 2018-11-07 | 2019-04-23 | 中国科学院过程工程研究所 | A kind of system and method preparing metal fluoride coated lithium ion battery positive electrode based on fluidized-bed chemical vapor deposition method |
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CN108842140B (en) * | 2018-05-31 | 2020-10-23 | 中国科学院过程工程研究所 | System and method for carbon coating modification of lithium ion battery anode material |
CN108842140A (en) * | 2018-05-31 | 2018-11-20 | 中国科学院过程工程研究所 | A kind of system and method for anode material for lithium-ion batteries coated modified carbon |
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CN109621847B (en) * | 2018-11-07 | 2021-10-26 | 中国科学院过程工程研究所 | System and method for coating lithium ion battery anode material by compounding carbon and metal oxide |
CN111009639A (en) * | 2019-12-12 | 2020-04-14 | 山东金品能源有限公司 | Sintering process for preparing lithium ion battery anode material |
CN111009639B (en) * | 2019-12-12 | 2022-05-17 | 山东金品能源有限公司 | Sintering process for preparing lithium ion battery anode material |
CN111023813A (en) * | 2019-12-13 | 2020-04-17 | 山东金品能源有限公司 | Fluidized bed reaction furnace for sintering lithium ion battery anode material |
CN112919552A (en) * | 2021-01-28 | 2021-06-08 | 中南大学 | High tap density multi-element oxide precursor and preparation method and preparation system thereof |
CN114497505A (en) * | 2022-01-28 | 2022-05-13 | 佛山市德方纳米科技有限公司 | Method and device for continuously preparing anode material by spray drying |
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