CN109650457A - A kind of preparation method of spherical mangano-manganic oxide - Google Patents

A kind of preparation method of spherical mangano-manganic oxide Download PDF

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Publication number
CN109650457A
CN109650457A CN201910137284.1A CN201910137284A CN109650457A CN 109650457 A CN109650457 A CN 109650457A CN 201910137284 A CN201910137284 A CN 201910137284A CN 109650457 A CN109650457 A CN 109650457A
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mangano
preparation
manganic oxide
added
ammonium
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CN109650457B (en
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丁晓锋
王以存
王军伟
刘阿朋
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SINOSTEEL ANHUI TIANYUAN TECHNOLOGY Co Ltd
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SINOSTEEL ANHUI TIANYUAN TECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00Compounds of manganese
    • C01G45/02Oxides; Hydroxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

Abstract

The invention belongs to anode LiMn2O4 raw material fields, more particularly to a kind of preparation method of spherical mangano-manganic oxide, this method includes that granularity≤100 μm manganese powder is made with disintegrating apparatus for 99wt.% or more manganese metal piece in purity, deionized water is added to be configured to the suspension of certain liquid-solid ratio, the ammonium salt of manganese powder weight 1%-3% and 0.2~1 ‰ surfactant of weight is added, control reaction temperature, oxidant is added, ammonium hydroxide is added and controls reaction process pH, a few hours are reacted under certain mixing speed, after reaction, slurry is by washing, expansion drying, spherical mangano-manganic oxide is made, it is less than normal that the present invention solves the meso-position radius in the presence of mangano-manganic oxide conventional preparation techniques, granule-morphology is irregular, it is easy to reunite, energy consumption for drying is higher, the problems such as biodiversity content is higher.

Description

A kind of preparation method of spherical mangano-manganic oxide
Technical field
The invention belongs to anode LiMn2O4 raw material fields, and in particular to a kind of system of spherical mangano-manganic oxide Preparation Method.
Background technique
Mangano-manganic oxide is the important source material of electronics industry production manganese-zinc ferrite soft magnetic materials, is also applied to temperature-sensitive on a small quantity The fields such as resistance, pigment, catalyst.In recent years, mangano-manganic oxide starts to apply in field of batteries, is mainly used for lithium-ion electric The preparation of pond manganate cathode material for lithium.Since lithium manganate material production process generallys use dry mixing, thus require four oxidations Three manganese product granule-morphologies are regular, are evenly distributed, and agglomerated particle without exception, powder dispersity is good, to guarantee that manganese source and lithium source are mixed The uniformity of conjunction.
Domestic manufacturer mainly uses electrolytic manganese metal suspension oxidizing process to produce mangano-manganic oxide at present, and the method is by manganese metal Piece is made into suspension after crushing, then blowing air aoxidizes to obtain mangano-manganic oxide slurry, and four oxygen are made in slurry after washing, drying Change three manganese.The mangano-manganic oxide meso-position radius of traditional handicraft preparation is less than normal, and granule-morphology is irregular, and uniformity is poor, it is difficult to directly use In battery industry;And spray drying process is generallyd use in drying process, principle is: air passes through filter and heater, Into the air distributor at the top of centrifugal spray drier, hot-air is in the shape of a spiral even into drier.Mangano-manganic oxide material Liquid is pumped into the centrifugal atomizer at the top of drier through filter by material fluid bath, and feed liquid is made to be sprayed into minimum misty liquid droplets, material Liquid and hot-air parallel flow contact, moisture evaporate rapidly, are dried to finished product in a very short period of time, finished product is by drying tower bottom and whirlwind Separator discharge, exhaust gas are discharged by blower.Mangano-manganic oxide is prepared using spray drying process, in order to guarantee that slurry is sufficiently atomized, Feed liquid mass percentage concentration is usually no more than 55%, and for ton product air consumption at 80 cubes or more, energy consumption is higher, in addition, preparation Mangano-manganic oxide powder granule is easy to reunite, and product moisture is not easy to control, and general biodiversity content is 0.3% or more.
The present invention is to propose a type to solve traditional soft magnetism mangano-manganic oxide the battery industry application difficult the problems such as Spherical mangano-manganic oxide preparation method, at the same solve present in preparation process meso-position radius is less than normal, particle is easy to reunite, pattern not Rule, the problems such as energy consumption is higher, biodiversity content is higher.The method by control manganese metal rusting rate in the solution and Trimanganese tetroxide particle reunion mode prepares spherical mangano-manganic oxide powder, in addition, this method drying process is dry using flash distillation Dry method.Expansion drying principle is: hot-air, which enters stirring crushing from dry motor spindle with suitable spout velocity by population pipe, to be done Dry room generates strong shearing to material, blows floating, turning effort, and material is centrifuged, sheared, collided, rubbed and by particle Change, enhances mass-and heat-transfer.In drying machine lower curtate, larger wetter cluster of grains under the action of blender by Mechanical Crushing, it is wet Content is lower, the lesser particle of granularity is risen by swirling eddy entrainment, is further dried in uphill process, at the top of hothouse Equipped with classifying cyclone, can to stock grading, make the powder reunited return to it is intracavitary be further crushed, to guarantee particle Uniformity and dispersibility.
The mangano-manganic oxide prepared by this method is suitable for being used in field of lithium ion battery to be used to prepare lithium manganate cathode material Material, on the one hand, product maintains the spherical pattern in reaction process, and good product dispersibility after dry, and there is no abnormal groups Poly- particle, product moisture is easily controllable, in addition, feed concentration can be improved to 80% or more, ton product air consumption can be reduced More than half.
Summary of the invention
D50Index refers to that cumulative particle sizes percentile reaches partial size corresponding when 50% in a kind of sample, also known as " in Position partial size " or " medium particle diameter ", usually indicate the granular size of the particle swarm with it.Lithium ion battery industry generally requires The D of manganate cathode material for lithium50At 10 μm or so, to take into account its chemical property and processing performance.Four oxygen of traditional handicraft preparation It is smaller to change three manganese partial sizes, meso-position radius D50Generally less than 3 μm, and granule-morphology is irregular, uniformity is poor, it is difficult in LiMn2O4 row Industry application.In addition, conventional method prepares mangano-manganic oxide using spray drying, feed liquid mass percentage concentration is usually no more than 55%, energy consumption is higher, moreover, the mangano-manganic oxide powder granule of preparation is easy to reunite.In addition, solving the preparation of mangano-manganic oxide tradition Product moisture in the presence of technique is not easy to control, and general biodiversity content is 0.3% or more.The present invention is for granulated The problems such as looks are irregular, easy to reunite, energy consumption is higher, biodiversity content is higher, proposes a kind of novel processing step.
The present invention relates to a kind of preparation method of spherical mangano-manganic oxide, method mangano-manganic oxide produced it is obvious Granularity, catalyst and surfactant types by controlling initial manganese powder are characterized in that regulate and control synthesis condition and react Journey, effectively to control and improve the microscopic appearance and structure of product.In addition, introducing expansion drying method, it is made to keep reacting In the process on the basis of trimanganese tetroxide particle pattern, energy consumption for drying is saved, reduces mangano-manganic oxide industrial products moisture content.
Specifically, the present invention relates to a kind of preparation methods of spherical mangano-manganic oxide, comprising:
(1) granularity≤100 μm manganese powder is made with disintegrating apparatus for 99wt.% or more manganese metal piece in purity;
(2) reaction kettle is added in manganese powder made from step (1), deionized water is added to be configured to suspension;Manganese powder weight is added 1%~3% ammonium salt and 0.2~1 ‰ surfactant of manganese powder weight;Control reaction temperature;Oxidant is added;Ammonia is added Water management reacts pH;It is stirred to react 10~20 hours, is filtered, washed;
(3) it will expect that cake is added to drying in flash drying equipment, is made spherical mangano-manganic oxide after washing.
Wherein, step (2), preferred:
The suspension liquid-solid ratio is (2~5): 1, preferably (2~4): 1;
The ammonium salt is one of ammonium chloride, ammonium sulfate, ammonium nitrate, ammonium formate, ammonium acetate, ammonium citrate or more Kind.
The surfactant is polyacrylic acid, in ammonium polyacrylate, polyethylene glycol, polyvinyl alcohol, polyacrylamide It is one or more.
The oxidant be oxygen, compressed air, hydrogen peroxide it is one or more.
The reaction temperature is 50~80 DEG C, preferably 60~80 DEG C.
The pH is 6.5~7.5, preferably 6.9~7.1.
The mixing speed is 200~500r/min, preferably 350~500r/min.
Washing eliminates impurity chlorine root, ammonium salt, calcium, magnesium etc..
Preferably, step (3) flash process parameter are as follows: 200~300 DEG C of inlet temperature, preferably 250~300 DEG C;Outlet temperature 100~120 DEG C, preferably 110~120 DEG C of degree;500~1000Pa of negative pressure, preferably 800~1000Pa;Broken mixing speed 50~ 150 revs/min, preferably 100~150 revs/min.
The invention further relates to a kind of spherical mangano-manganic oxides that any of the above-described method is prepared, it is characterised in that: Mangano-manganic oxide its granule-morphology for changing method preparation is spherical in shape or spherical, meso-position radius D50At 3~15 μm, preferably in 5~15 μ M, more preferably at 10~12 μm.
Preferably, in the mangano-manganic oxide product biodiversity content less than 0.3%.
Preferably, above-mentioned mangano-manganic oxide preparation method product per ton is using natural gas less than 40 cubes.
Detailed description of the invention
The following further describes the present invention with reference to the drawings.
Fig. 1 is expansion drying flow chart used by embodiment, in which: 1, air blower;2, heating furnace;3, host is flashed; 4, charger;5, cyclone separator;6, bag filter;7, air-introduced machine
Fig. 2 is the scanning electron microscope (SEM) photograph of mangano-manganic oxide product obtained by embodiment 1
Fig. 3 is the scanning electron microscope (SEM) photograph of mangano-manganic oxide product obtained by embodiment 2
Fig. 4 is the scanning electron microscope (SEM) photograph of mangano-manganic oxide product obtained by embodiment 3
Fig. 5 is the scanning electron microscope (SEM) photograph of mangano-manganic oxide product obtained by embodiment 4
Fig. 6 is the scanning electron microscope (SEM) photograph of mangano-manganic oxide product obtained by embodiment 5
Specific embodiment
The present invention will be further described with reference to the examples below.Described embodiment and its result are merely to illustrate The present invention, without the present invention described in detail in claims should will not be limited.
Embodiment 1
1000Kg high pure metal manganese piece is crushed within 100 μm using twin rollers, then is mixed 2 hours with Double cone mixer, It puts into later and 4m has been added3The reaction kettle of pure water is configured to suspension, and 25kg ammonium sulfate and 0.8kg ammonium polyacrylate is added, Reactor temperature is controlled at 60 DEG C, and under agitation, blowing air oxidation, wherein tolerance control is in 300m3/ h, mixing speed Control is added ammonium hydroxide and controls pH value in reaction 7 ± 0.1 in 350r/min, and reaction terminates after 15 hours, slurry filtration, washing, The material cake that aqueous mass ratio is 16% is obtained, material cake is added in flash drying equipment, air blower and air inducing fan delivery are controlled, Negative pressure in tower is set to control burner temperature in 800Pa, inlet temperature is made to maintain 250 DEG C, outlet temperature maintains 110 DEG C, breaks Spherical mangano-manganic oxide powder is made after dry in 100 revs/min of broken mixing speed.
Mangano-manganic oxide product particle good dispersion obtained by this, pattern is spherical in shape or spherical, and median is 10.8 μm, ton product is 33 cubes using natural gas, product moisture content 0.2%.
Embodiment 2
Technique is same as Example 1, and different is, by high pure metal manganese piece using twin rollers be crushed to 50 μm with It is interior.
Mangano-manganic oxide product particle good dispersion obtained by this, pattern is spherical in shape or spherical, and median is 5.8 μm, ton product is 37 cubes using natural gas, and product moisture content is 0.22%.
Embodiment 3
Technique is same as Example 1, and different is, surfactant 0.8kg polyvinyl alcohol.
Mangano-manganic oxide product median obtained by this is 12.5 μm, and ton product is 33 cubes using natural gas, Product moisture content is 0.19%.
Embodiment 4
Technique is same as Example 1, and different is, surfactant 0.8kg polyacrylamide.
Mangano-manganic oxide product median obtained by this is 4.7 μm, and ton product is 36 cubes using natural gas, is produced Product moisture content is 0.25%.
Embodiment 5
Technique is same as Example 1, and different is, adds deionized water to deploy the mangano-manganic oxide material cake after washing The slurry for being 50% at solid content, is dried using spray drying device, and atomization disk rotating speed is set as 15000 revs/min, control Charging rate makes 250 DEG C of inlet temperature, and outlet temperature maintains 110 DEG C, obtains mangano-manganic oxide powder.
Mangano-manganic oxide product median obtained by this is 10.2 μm, and ton product is 88 cubes using natural gas, Product moisture content is 0.35%.
Embodiment 6
Technique is same as Example 1, and different is, flash drying equipment is added in material cake, controls burner temperature, makes Inlet temperature maintains 200 DEG C, and outlet temperature maintains 110 DEG C, is crushed 100 revs/min of mixing speed, class ball is made after dry Shape mangano-manganic oxide powder.
Mangano-manganic oxide product median obtained by this is 10.1 μm, and ton product is 34 cubes using natural gas, Product moisture content is 0.25%.
Embodiment 7
Technique is same as Example 1, and different is, flash drying equipment is added in material cake, controls burner temperature, makes Inlet temperature maintains 300 DEG C, and outlet temperature maintains 110 DEG C, is crushed 100 revs/min of mixing speed, class ball is made after dry Shape mangano-manganic oxide powder.
Mangano-manganic oxide product median obtained by this is 10.5 μm, and ton product is 38 cubes using natural gas, Product moisture content is 0.15%.

Claims (11)

1. a kind of preparation method of spherical mangano-manganic oxide, comprising:
(1) granularity≤100 μm manganese powder is made with disintegrating apparatus for 99wt.% or more manganese metal piece in purity;
(2) reaction kettle is added in manganese powder made from step (1), deionized water is added to be configured to suspension;Addition manganese powder weight 1%~ 3% ammonium salt and 0.2~1 ‰ surfactant of manganese powder weight;Control reaction temperature;Oxidant is added;Ammonium hydroxide control is added System reaction pH;It is stirred to react 10~20 hours, is filtered, washed;
(3) it will expect that cake is added to drying in flash drying equipment, is made spherical mangano-manganic oxide after washing.
2. a kind of preparation method as described in claim 1, which is characterized in that suspension liquid-solid ratio described in step (2) is (2 ~5): 1, preferably (2~4): 1.
3. kind of preparation method as described in claim 1, which is characterized in that ammonium salt described in step (2) is ammonium chloride, sulfuric acid One of ammonium, ammonium nitrate, ammonium formate, ammonium acetate, ammonium citrate are a variety of.
4. a kind of preparation method as described in claim 1, which is characterized in that surfactant described in step (2) is poly- third One of olefin(e) acid, ammonium polyacrylate, polyethylene glycol, polyvinyl alcohol, polyacrylamide are a variety of.
5. a kind of preparation method as described in claim 1, which is characterized in that oxidant described in step (2) is oxygen, compression Air, hydrogen peroxide it is one or more.
6. a kind of preparation method as described in claim 1, which is characterized in that reaction temperature described in step (2) is 50~80 DEG C, preferably 60~80 DEG C.
7. a kind of preparation method as described in claim 1, which is characterized in that pH described in step (2) is 6.5~7.5, preferably 6.9~7.1.
8. a kind of preparation method as described in claim 1, which is characterized in that step (2) mixing speed is 200~500r/ Min, preferably 350~500r/min.
9. a kind of preparation method as described in claim 1, which is characterized in that step (3) flash process parameter are as follows: inlet temperature 200~300 DEG C, preferably 250~300 DEG C;100~120 DEG C of outlet temperature, preferably 110~120 DEG C;500~1000Pa of negative pressure, It is preferred that 800~1000Pa;Broken 50~150 revs/min of mixing speed, preferably 100~150 revs/min.
10. the spherical mangano-manganic oxide that a kind of the method according to claim 1 is prepared, feature exist In: its granule-morphology of the mangano-manganic oxide of this method preparation is spherical in shape or spherical, meso-position radius D50At 3~15 μm, preferably 5~ 15 μm, more preferably at 10~12 μm.
11. a kind of spherical mangano-manganic oxide as claimed in claim 10, it is characterised in that: the mangano-manganic oxide product Middle biodiversity content is less than 0.3%.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110759384A (en) * 2019-11-08 2020-02-07 中信大锰矿业有限责任公司 Method for preparing spheroidal manganous manganic oxide by manganese sulfate solution
CN110776015A (en) * 2019-11-05 2020-02-11 江西智锂科技有限公司 Synthesis method of battery-grade trimanganese tetroxide
CN111892091A (en) * 2020-08-27 2020-11-06 湖南特种金属材料有限责任公司 Preparation method of trimanganese tetroxide for drilling mud
CN113690011A (en) * 2021-07-13 2021-11-23 贵州金瑞新材料有限责任公司 Demagnetisation process for preparing battery-grade trimanganese tetroxide by manganese sheet method
CN113735175A (en) * 2021-08-17 2021-12-03 华中农业大学 Nano-mimetic enzyme, preparation method and seed soaking agent containing nano-mimetic enzyme
CN115959716A (en) * 2022-12-06 2023-04-14 中钢天源股份有限公司 Nickel-manganese binary precursor and preparation method thereof
CN115959710A (en) * 2022-12-06 2023-04-14 中钢天源股份有限公司 Preparation method of battery-grade manganese sesquioxide and product thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110776015A (en) * 2019-11-05 2020-02-11 江西智锂科技有限公司 Synthesis method of battery-grade trimanganese tetroxide
CN110759384A (en) * 2019-11-08 2020-02-07 中信大锰矿业有限责任公司 Method for preparing spheroidal manganous manganic oxide by manganese sulfate solution
CN111892091A (en) * 2020-08-27 2020-11-06 湖南特种金属材料有限责任公司 Preparation method of trimanganese tetroxide for drilling mud
CN113690011A (en) * 2021-07-13 2021-11-23 贵州金瑞新材料有限责任公司 Demagnetisation process for preparing battery-grade trimanganese tetroxide by manganese sheet method
CN113735175A (en) * 2021-08-17 2021-12-03 华中农业大学 Nano-mimetic enzyme, preparation method and seed soaking agent containing nano-mimetic enzyme
CN115959716A (en) * 2022-12-06 2023-04-14 中钢天源股份有限公司 Nickel-manganese binary precursor and preparation method thereof
CN115959710A (en) * 2022-12-06 2023-04-14 中钢天源股份有限公司 Preparation method of battery-grade manganese sesquioxide and product thereof

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