CN109052480A - A kind of high-purity mangano-manganic oxide and preparation method thereof - Google Patents
A kind of high-purity mangano-manganic oxide and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of high-purity mangano-manganic oxide: electrolytic manganese powder and water are tuned into manganese slurry；Ammonium salt solution is added in the manganese slurry, it stirs and is passed through oxidizing gas and reacted, reaction was completed when the pH value of reaction system reaches 5~7, and gained slurry is separated by solid-liquid separation, resulting solid is washed, is dried to get the high-purity mangano-manganic oxide is arrived after separation of solid and liquid.Preparation method of the invention, first sizes mixing to manganese powder, adds ammonium salt in catalysis agent, can overcome traditional safety that security risk present in ammonium salt in catalysis agent is added in manganese powder, guarantees in preparation process.Of the invention using electrolytic manganese as raw material, pilot process does not need any chemical subtraction, will not cause dedoping step bring secondary effect, and product purity is high, epigranular, microstructure rule, and consistency is good.
Description
Technical field
It is high, practical that the present invention relates to a kind of preparation methods of mangano-manganic oxide more particularly to a kind of security performance
High-purity mangano-manganic oxide and preparation method thereof.
Background technique
Mangano-manganic oxide is just to start by a kind of brand-new material concerned by people twentieth century the seventies and eighties.It first by
Walk the basic raw material for becoming soft magnetic ferrite instead of manganese carbonate, by development in more than 30 years, application field also by
Step is widened, and people are the study found that mangano-manganic oxide is the quality raw materials of synthesis of anode material of lithium-ion battery lithium manganese oxygen in recent years.
The method of industrial production mangano-manganic oxide at present, substantially there is manganese sulfate method and manganese powder method.Manganese sulfate method is to utilize
Mn2+Mn (OH) is precipitated under alkaline condition2, then pass through oxidant and it is carried out to aoxidize obtained mangano-manganic oxide；This method
Major defect is exactly that the mangano-manganic oxide purity for preparing is not high, and quality stability is poor, the reason is that usually containing in manganese sulfate raw material
More impurity is also difficult to remove completely, and is added to various other materials again in dedoping step even across removal of impurities, in addition manganese
When ion hydrolyzes, there are alkali formula manganese sulfate and sulfate to be mixed in precipitating, cause final products sulfur content higher, it is difficult to reduce.
Manganese powder method produces mangano-manganic oxide, has at home and abroad also carried out a large amount of research.Chinese patent application CN1252385A and
CN103058280A proposes to prepare mangano-manganic oxide using manganese powder two-step method, and manganese powder granularity substantially will be less than 50 μ
M, but manganese powder granularity is meticulous, activity is too strong, and manganese powder is directly thrown into catalyst solution reaction acutely, discharges a large amount of hydrogen,
It is careless slightly to explode, it is unfavorable for industrialized production, while first step conversion is eventually when two-step method prepares mangano-manganic oxide
Point is difficult to judge, in production process if it is determined that inaccurate, in the final product strip or cylindrical particle easy to form, thus
Cause mangano-manganic oxide microstructure uneven, it is difficult to be applied to other fields outside soft magnetism industry；Moreover, traditional preparation four
The process of Mn 3 O is that manganese powder is added in ammonium salt in catalysis agent, and the manganese powder being introduced into reacts rapidly with catalyst, generates hydrogen,
Manganese powder is continuously added, if friction generates spark between manganese powder or the external world brings Mars into, easily occurs to include that hydrogen is impure at this time
The major safety risks such as fire occur for explosion or combustion of hydrogen, are also no lack of therefore reason in industry and lead to serious accident
Enterprise.The clear 63-215521 of Japan Patent also proposed manganese powder and water, pass through two-step method preparation four without using catalyst
Mn 3 O, this method only can just react when temperature is higher than 90 DEG C, and large quantity of moisture evaporates when reaction, and high temperature is maintained to need
It is largely outer hot, it will increase energy consumption.
It prepares therefore, it is necessary to studying that a kind of processing step is simple, production cost is low, low energy consumption, security performance is high high-purity
Mangano-manganic oxide method.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
Kind of processing step is simple, without extraneous heating, production cost is low, security performance is high, is applicable in the one-step method preparation of industrialized production
The method of mangano-manganic oxide, and the mangano-manganic oxide of this method preparation is with high purity, activity is strong, microstructure is regular.
In order to solve the above technical problems, technical solution proposed by the present invention are as follows:
A kind of preparation method of high-purity mangano-manganic oxide, comprising the following steps:
Electrolytic manganese powder and water are tuned into manganese slurry；Ammonium salt solution is added in the manganese slurry, stirs and is passed through oxidizing gas
It is reacted, reaction was completed when the pH value of reaction system reaches 5~7, gained slurry is separated by solid-liquid separation, gained after separation of solid and liquid
Solid washed, dried to get to the high-purity mangano-manganic oxide.It is further preferred that the pH value to reaction system reaches
Reaction was completed when to 5.5, and applicant passes through the study found that when the pH value of reaction system reaches 5.5, then it represents that fully reacting is arrived
Up to terminal, at this time in product mangano-manganic oxide without miscellaneous, also without the complete manganese metal of unreacted or manganous hydroxide or manganese
Other compounds.
Manganese powder occurs to react as follows under the action of ammonium salt in catalysis agent solution:
Mn+2NH4 ++2H2O→Mn2++2NH3·H2O+H2↑；
Newly-generated Mn2+And NH3·H2O is also easy to produce basic salt complex:
Mn2++xNH3·H2O→Mn(NH3)x 2++xH2O；
A large amount of heat is discharged simultaneously, since the basic salt complex is unstable, is heated and generates Mn2+With NH3·H2O,
Mn2+With NH3·H2O reaction generates manganous hydroxide precipitating:
Mn2++2NH3·H2O→Mn(OH)2↓+2NH4 +。
Above-mentioned preparation method, it is preferred that the granularity of the electrolytic manganese powder is not higher than 380 μm；The electrolytic manganese powder be by
Any electrolytic manganese piece in model DJMnA, DJMnB, DJMnC is obtained through broken；The crumbling method is to roller.
Above-mentioned preparation method, it is preferred that the additional amount of ammonium salt makes 10~80g/L of ammonium salt concentration in reaction system；It is whole
In a reaction process, by into reaction system water supplement come to control in reaction system solid-liquid mass ratio be 1:(4~8).
Above-mentioned preparation method, it is preferred that the addition mass ratio of the addition quality of electrolytic metal manganese powder and ammonium salt be (2~
25): 1.
Above-mentioned preparation method, it is preferred that the temperature for controlling the reaction process is no more than 80 DEG C.
Above-mentioned preparation method, it is preferred that cold by supplementing water into reaction system, opening ventilation device or opening circulation
But the mode of water controls the temperature of reaction process.
Above-mentioned preparation method, it is preferred that the ammonium salt solution is a kind of or several in ammonium chloride, ammonium acetate and ammonium sulfate
Kind mixing salt solution；The oxidizing gas is air；The speed of agitator is 300~900rpm.The present invention is closed by control
Suitable speed of agitator can guarantee that manganese powder suspends completely in reactive tank, sufficiently occur with contacts such as catalyst, water and air anti-
It answers；Simultaneously by controlling suitable mixing speed, four oxidations that packet is attached to electrolytic manganese metal or manganous hydroxide outer layer are also helped
Three manganese peel off in time, expose inner layer unreacted completely fresh surface (electrolytic manganese metal or manganous hydroxide), connect fresh surface
Again react, to achieve the purpose that electrolytic manganese metal is prepared into mangano-manganic oxide.
Above-mentioned preparation method, it is preferred that the time of the reaction is 5~11h, is passed through oxidizing gas in reaction process
Rate be 30~100Nm3/h。
Above-mentioned preparation method, it is preferred that recycled in mother liquor Returning reacting system obtained after the separation of solid and liquid.
The inventive concept total as one, the present invention also provides a kind of high-purity mangano-manganic oxides, by above-mentioned preparation method
It is prepared.
Above-mentioned high-purity mangano-manganic oxide, it is preferred that Mn content >=71% in the high-purity mangano-manganic oxide, granularity D50For
0.5~10 μm, apparent density BD:0.5~1.3g/cm3, specific surface area BET:1~20m2/g。
Preparation method of the invention selects electrolytic manganese powder as raw material, and centre does not need any chemical subtraction, will not cause
Dedoping step bring secondary effect, manufactured product purity are high；The present invention first sizes mixing to manganese powder, and ammonium salt solution is added
It is reacted in manganese slurry, can overcome and manganese powder is directly added into security risk present in ammonium salt solution, various grains can be suitble to
The manganese powder of diameter；Simultaneously to the mixing speed of reaction system and the research of reaction end, it ensure that electrolytic manganese powder sufficiently reacts, and raw
At mangano-manganic oxide in without miscellaneous, purity is high.It can be seen that the preparation method is that an organic whole, from source
On head, in reaction process, by the selection of raw material and technological parameter, the common guarantee safety of preparation method of the invention
And the purity of obtained mangano-manganic oxide product.
Compared with the prior art, the advantages of the present invention are as follows:
(1) preparation method of the invention, first sizes mixing to manganese powder, adds ammonium salt in catalysis agent, can overcome traditional
Security risk present in ammonium salt in catalysis agent is added in manganese powder, guarantees the safety in preparation process.
(2) preparation method of the invention, first sizes mixing to manganese powder, can be suitble to various four oxidations three of partial size manganese powder preparation
Manganese, it is meticulous to overcome manganese powder granularity in traditional preparation methods, safety problem caused by activity is too strong.
(3) process flow of the invention is simple, highly-safe, and compared with two-step method, all reactions of the invention are one
It is completed in a reactive tank, ensure that the stabilization of reaction system, while eliminating intermediate turn trough link, the reaction time is short, production effect
Rate is high.
(4) the preparation method scope of application of the invention is broad, can not only be produced by technical arrangement plan and meet soft magnetism
The product of ferrite mangano-manganic oxide (GB/T21836-2008) any trade mark；But also it can be raw by controlling Fe content
Produce the spherical mangano-manganic oxide of high jolt ramming for being suitable for preparing LiMn2O4.
(5) present invention is crushed using to roller mode, is substantially reduced manganese piece and is crushed the time, and manganese powder granularity is up to standard, reduces
The bringing into of Fe content.
(6) of the invention using electrolytic manganese as raw material, pilot process does not need any chemical subtraction, will not cause to clean
Process bring secondary effect, product purity is high, epigranular, and microstructure rule, consistency is good, manufactured high-purity four oxidation
Mn content >=71% in three manganese, granularity D50It is 0.5~10 μm, apparent density BD:0.5~1.3g/cm3, specific surface area BET:1~
20m2/g。
Detailed description of the invention
Fig. 1 is the electron microscope of high-purity mangano-manganic oxide prepared by the embodiment of the present invention 1.
Fig. 2 is the electron microscope of high-purity mangano-manganic oxide prepared by the embodiment of the present invention 2.
Fig. 3 is the electron microscope of high-purity mangano-manganic oxide prepared by the embodiment of the present invention 3.
Fig. 4 is the electron microscope of high-purity mangano-manganic oxide prepared by the embodiment of the present invention 4.
Specific embodiment
To facilitate the understanding of the present invention, invention herein is done below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but protection scope of the present invention is not limited to following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, and it is of the invention to be not intended to limitation
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1:
A kind of preparation method of high-purity mangano-manganic oxide of the invention, comprising the following steps:
(1) 1.5m is chosen30.5m is added into the reactive tank in reactive tank3Pure water, open agitating device, revolving speed is
300rpm；
(2) 380 μm of granularity < of DJMnC manganese powder 250kg after taking roller pair breaking puts into reactive tank and manganese slurry is made,
Then 12Kg NH is added into reactive tank4Cl, and fill into pure water 0.7m3, ammonium chloride concentration is 10g/L at this time；
(3) after finishing manganese powder, ventilation device, air quantity 50Nm are opened3The speed of agitator of/h, agitating device are adjusted to
900rpm carries out moisturizing according to the liquid level not timing in reactive tank during the reaction, and maintenance system solid-liquid mass ratio is 1:
(4.5~4.8) open extractor fan, when the reaction system in reaction process when temperature rises to >=80 DEG C in reaction process
When pH value is to 5.5 (reaction time 7h), that is, reach reaction end, be separated by solid-liquid separation, washing, it is dry after obtain 330KgMn3O4；Gu
Liquid mother liquor obtained after separation can return to be recycled in the reaction system in next period.
The Mn that test the present embodiment obtains3O4Purity > 99%, wherein each element content is as follows: Mn:71.47%,
SiO2: 0.0068%, CaO:0.0010%, MgO:0.0061%, Cl:0.034%, Fe2O3: 0.013%, S:0.015%；It should
High-purity Mn3O4Apparent density BD:1.26g/cm3, BET specific surface area: 1.29m2/g；Mean particle size D50: 5.21 μm；Electron microscope
Piece Mn as shown in Figure 1:3O4Even particle size distribution, microstructure is similar spherical.
It can be seen that the Mn that the present embodiment obtains3O4Product F e content is low, purity is high, and apparent density is high, and size distribution is equal
Even, it is the desirable feedstock as dynamic lithium manganate that microstructure is similar spherical.
Embodiment 2:
A kind of preparation method of high-purity mangano-manganic oxide of the invention, comprising the following steps:
(1) 1.5m is chosen30.5m is added into the reactive tank in reactive tank3Pure water, open agitating device, revolving speed is
300rpm；
(2) 250 μm of granularity < of DJMnC manganese powder 250kg after taking roller pair breaking puts into reactive tank and manganese slurry is made,
Then 12Kg NH is added into reactive tank4Cl, and fill into pure water 0.7m3, ammonium chloride concentration is 10g/L at this time, agitating device
Speed of agitator is adjusted to 900rpm；
(3) it finishes after manganese powder after 1.5h, opens ventilation device, air quantity 30Nm3/ h, during the reaction according to reactive tank
In liquid level not timing carry out moisturizing, maintenance system solid-liquid mass ratio is 1:(4.5~4.8), in reaction process temperature rise to >=
At 80 DEG C, extractor fan is opened, when the pH value of the reaction system in reaction process is to 5.5 (reaction time 8h), that is, is reached
Reaction end is separated by solid-liquid separation, washs, obtains 330KgMn after drying3O4；The mother liquor obtained after separation of solid and liquid can return to next week
It is recycled in the reaction system of phase.
The Mn that test the present embodiment obtains3O4Purity > 99%, wherein each element content is as follows: Mn:71.62%,
SiO2: 0.0067%, CaO:0.0010%, MgO:0.0047%, Cl:0.034%, Fe2O3: 0.013%, S:0.017%；It should
Mn3O4Apparent density BD:0.744g/cm3, BET specific surface area: 5.46m2/g；Mean particle size D50: 2.31 μm；Electron microscopic picture is such as
Shown in Fig. 2: Mn3O4Even particle size distribution.
The Mn that the present embodiment is prepared3O4Product complies fully with manganor manganic oxide used for soft magnetic ferrite standard (GB/
T21826-2008) trade mark RM-06A requirement, if raw material is replaced with DJMnB manganese piece, the Mn of preparation3O4Product also complies with RM-
06B requirement.
Embodiment 3:
A kind of preparation method of high-purity mangano-manganic oxide of the invention, comprising the following steps:
(1) 1.5M is chosen30.4m is added into the reactive tank in reactive tank3Pure water, open agitating device, revolving speed is
300rpm；
(2) 250 μm of granularity < of DJMnB manganese powder 150kg after taking roller pair breaking puts into reactive tank and manganese slurry is made,
Then 35Kg ammonium acetate is added into reactive tank, and fills into pure water 0.7m3, the speed of agitator of agitating device is adjusted to 900rpm；
(3) 70min after manganese powder is finished, ventilation device, air quantity 100Nm are opened3/ h, while during the reaction according to anti-
The liquid level not timing in slot is answered to carry out moisturizing, maintenance system solid-to-liquid ratio 1:(7.5~8), when the reaction system in reaction process
When pH value is to 5.5 (reaction time 11h), that is, reach reaction end, be separated by solid-liquid separation, washing, it is dry after obtain 200KgMn3O4。
The Mn that test the present embodiment obtains3O4Purity > 99%, wherein each element content is as follows: Mn:71.42%, SiO2:
0.0078%, CaO:0.0010%, MgO:0.0026%, Fe2O3: 0.011%, S:0.017%, Se:0.0002%；The Mn3O4
Apparent density BD:0.762g/cm3, BET specific surface area: 15.72m2/g；Mean particle size D50: 0.92 μm；Electron microscopic picture such as Fig. 3
It is shown: Mn3O4Even particle size distribution；The mother liquor obtained after separation of solid and liquid can return to be recycled in the reaction system in next period
It utilizes.
The Mn that the present embodiment is prepared3O4Product complies fully with GB/T21826-2008 trade mark RM-15B index, reaches
The requirement of high activity high-specific surface area mangano-manganic oxide.
Embodiment 4:
A kind of preparation method of high-purity mangano-manganic oxide of the invention, comprising the following steps:
(1) by 150kgDJMnC manganese piece after ball milling, the manganese slurry of granularity≤15 μm is obtained；
(2) 1.5m is chosen3Reactive tank, it is 0.75m that volume is put into the reactive tank3, ammonium chloride that concentration is 72g/L
In solution, ammonium chloride concentration is 10g/L in reaction system at this time, and the manganese after step (1) ball milling is then added into the reactive tank
Slurry, and agitating device is opened, revolving speed 900rpm；
(3) ventilation device, air quantity 100Nm are opened after finishing manganese slurry 2h3/ h, and pure water is mended to 1.2m into reactive tank3Liquid
Position place, opens exhausting and cooling circulating water, carries out moisturizing according to liquid level not timing, maintenance reaction system solid-to-liquid ratio for 1:7.5~
8, temperature≤70 DEG C in reaction process are saved, (reaction time is when the pH value of the reaction system in reaction process is to 5.5
5h), that is, reach reaction end, be separated by solid-liquid separation, wash, obtain 200KgMn after drying3O4；The mother liquor obtained after separation of solid and liquid can be with
It returns and is recycled in the reaction system in next period.
The Mn that test the present embodiment obtains3O4Purity > 99%, wherein each element content is as follows: Mn:71.29%, SiO2:
0.0074%, CaO:0.0010%, MgO:0.0024%, Fe2O3: 0.38%, Cl:0.028%, S:0.015%；The Mn3O4's
Apparent density BD:0.668g/cm3, BET specific surface area: 15.51m2/g；Mean particle size D50: 1.34 μm；Electron microscopic picture such as Fig. 4 institute
Show: Mn3O4Even particle size distribution.
The Mn that the present embodiment is prepared3O4Product utilization manganese slurry does raw material, and ammonium chloride is catalyst, the Mn of preparation3O4's
Indices are also fully consistent with GB/T21826-2008 trade mark RM-15A high-specific surface area mangano-manganic oxide requirement.
Claims (10)
1. a kind of preparation method of high-purity mangano-manganic oxide, which comprises the following steps:
Electrolytic manganese powder and water are tuned into manganese slurry；Ammonium salt solution is added in the manganese slurry, stir and is passed through oxidizing gas progress
Reaction, reaction was completed when the pH value of reaction system reaches 5~7, and gained slurry is separated by solid-liquid separation, resulting solid after separation of solid and liquid
Body is washed, is dried to get the high-purity mangano-manganic oxide is arrived.
2. preparation method as described in claim 1, which is characterized in that the granularity of the electrolytic manganese powder is not higher than 380 μm；It is described
Electrolytic manganese powder is obtained after being crushed any electrolytic manganese piece in model DJMnA, DJMnB, DJMnC.
3. preparation method as described in claim 1, which is characterized in that ammonium salt concentration is 10~80g/L in reaction system；Entirely
In reaction process, by into reaction system water supplement come to control in reaction system solid-liquid mass ratio be 1:(4~8).
4. preparation method as described in claim 1, which is characterized in that the addition quality of electrolytic metal manganese powder and the addition of ammonium salt
Mass ratio is (2~25): 1.
5. preparation method as described in claim 1, which is characterized in that the temperature for controlling the reaction process is no more than 80 DEG C.
6. preparation method as claimed in any one of claims 1 to 5, which is characterized in that the ammonium salt solution is selected from ammonium chloride, vinegar
One or more of mixing salt solutions in sour ammonium and ammonium sulfate；The oxidizing gas is air；The speed of agitator be 300~
900rpm。
7. preparation method as claimed in any one of claims 1 to 5, which is characterized in that the time of the reaction is 5~11h, instead
The rate that oxidizing gas should be passed through in the process is 30~100Nm3/h。
8. preparation method as claimed in any one of claims 1 to 5, which is characterized in that mother liquor obtained after the separation of solid and liquid
It is recycled in Returning reacting system.
9. a kind of high-purity mangano-manganic oxide, which is characterized in that prepared by preparation method according to any one of claims 1 to 7
It obtains.
10. high-purity mangano-manganic oxide as claimed in claim 9, which is characterized in that Mn content in the high-purity mangano-manganic oxide
>=71%, granularity D50It is 0.5~10 μm, apparent density BD:0.5~1.3g/cm3, specific surface area BET:1~20m2/g。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110911653A (en) * | 2018-09-18 | 2020-03-24 | 天津理工大学 | Manganous manganic oxide/carbon nano tube composite material and preparation method and application thereof |
| CN114772649A (en) * | 2022-04-13 | 2022-07-22 | 贵州大龙汇成新材料有限公司 | Method for preparing mangano-manganic oxide by using lean manganese ore |
| CN115572220A (en) * | 2022-09-21 | 2023-01-06 | 宁夏天元锰材料研究院(有限公司) | Preparation method of high-purity manganese oxalate |
| WO2023108815A1 (en) * | 2021-12-16 | 2023-06-22 | 贵州大龙汇成新材料有限公司 | Preparation method for manganese hydroxide and use thereof |
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| CN110911653B (en) * | 2018-09-18 | 2021-10-15 | 天津理工大学 | Manganous manganic oxide/carbon nano tube composite material and preparation method and application thereof |
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| CN114772649A (en) * | 2022-04-13 | 2022-07-22 | 贵州大龙汇成新材料有限公司 | Method for preparing mangano-manganic oxide by using lean manganese ore |
| CN115572220A (en) * | 2022-09-21 | 2023-01-06 | 宁夏天元锰材料研究院(有限公司) | Preparation method of high-purity manganese oxalate |
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