CN106430330A - Preparation method of cobalt oxide powder - Google Patents

Preparation method of cobalt oxide powder Download PDF

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Publication number
CN106430330A
CN106430330A CN201610594957.2A CN201610594957A CN106430330A CN 106430330 A CN106430330 A CN 106430330A CN 201610594957 A CN201610594957 A CN 201610594957A CN 106430330 A CN106430330 A CN 106430330A
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cobalt
cobalt oxide
preparation
oxide powder
powder according
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王文祥
刘莹
李慧颖
方红生
黄玲
李腾
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Guangdong Vocational College of Environmental Protection Engineering
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/04—Oxides; Hydroxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • 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

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  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

A preparation method of cobalt oxide powder includes the following steps that A, during precipitating, an ammonium hydrogen carbonate solution is adopted as precipitator, a cobalt chloride solution is added in an ultrasonic atomization spraying mode with back titration, meanwhile, a surface active agent is added, and cobalt carbonate precipitate is obtained through a reaction, wherein the concentration of the cobalt chloride solution is 0.2 mol/L, and the concentration of the ammonium bicarbonate solution is 0.4 mol/L; B, during filtering and separating, the cobalt carbonate precipitate is filtered with water, then substances without a reaction are removed, then low-temperature drying is carried out for dewatering, and a cobalt oxide precursor is obtained; C, the cobalt oxide powder is obtained through thermal decomposition. The preparation method of the cobalt oxide powder is simple in technology, the pH is kept to be ranged from 7 to 8 during the reaction, and the generated cobalt oxide powder is high in purity and production efficiency and narrow in particle size distribution interval and does not contain impurity ions.

Description

A kind of preparation method of cobalt/cobalt oxide powder
Technical field
The present invention relates to alloy powder preparing technical field, more particularly to a kind of preparation method of cobalt/cobalt oxide powder.
Background technology
Cobalt/cobalt oxide powder is used widely in fields such as battery, catalyst, pottery, pigment, glass, while to cobalt oxide The granularity and performance of compound are it is also proposed that higher requirement.Due to granularity and pattern of the different applications to cobalt/cobalt oxide powder There is special requirement, the needle-like cobalt/cobalt oxide for such as being prepared with oxalate precipitation agent, be used in the field such as catalyst, pottery more；And conduct Additives for battery, then require that cobalt/cobalt oxide powder particle is mostly spherical, and the granularity to powder and granularity divide have special will Ask.Cobalt/cobalt oxide powder granularity heterogeneity prepared by traditional handicraft, and particle diameter is relatively large, the cobalt/cobalt oxide powder of generation is easily rolled into a ball Poly-, therefore which is difficult to meet in granularity and aspect of performance and requires.
Content of the invention
It is an object of the invention to a kind of preparation method of cobalt/cobalt oxide powder is proposed, and the process is simple of employing, pH is maintained In 7-8, the cobalt/cobalt oxide powder purity height of generation, ion free from foreign meter, production efficiency height, cobalt powder particle size distribution interval is narrow.
For reaching this purpose, the present invention is employed the following technical solutions：
A kind of preparation method of cobalt/cobalt oxide powder, comprises the following steps：
A, precipitation：
Using ammonium bicarbonate soln as precipitant, add cobaltous chloride molten with the ultrasonic atomization spray add mode of back titration Liquid, and surfactant is simultaneously introduced, reaction obtains cobalt carbonate precipitation；Wherein, the concentration of the cobalt chloride solution is 0.2mol/ L, the concentration of the ammonium bicarbonate soln is 0.4mol/L；
B, it is separated by filtration：
Cobalt carbonate sediment is carried out cold drying after the unreacted material of water filtration removal water is removed, obtain cobalt/cobalt oxide Presoma；
C, thermal decomposition：
The cobalt/cobalt oxide presoma that step B is obtained is calcined at 500-600 DEG C, obtains Co3O4Powder；
Or, the cobalt/cobalt oxide presoma for obtaining step B is calcined at 1100-1200 DEG C, CoO powder is obtained.
Further description, the surfactant is Tween 80.
Further description, the reaction temperature of step A is 20 DEG C.
Further description, the response time of step A is 30min.
Further description, the precipitant excess coefficient of step A is C2O4 2-/Co2+=2.
Further description, the preparation of CoO powder in step C is carried out in tube furnace.
Further description, the tube furnace used in step C is passed through nitrogen.
Further description, the calcination time of step C is 4h.
Further description, the cobalt/cobalt oxide presoma that step B is obtained is basic cobaltous carbonate.
Beneficial effects of the present invention：
1st, reaction solution is made to maintain 7-8 from ammonium hydrogen carbonate, without using pH adjusting agent, it is to avoid such as sodium ion, calcium The introducing of the other impurities ion of ion etc., the cobalt/cobalt oxide powder purity height of generation, ion free from foreign meter, and production efficiency High.
2nd, the cobalt powder particle size distribution interval for preparing is narrow, and dispersibility and nodularization effect are good, can be used for cell positive electrode Added material.
Description of the drawings
Fig. 1 is the SEM photograph that in embodiment of the present invention group 1, feed way is affected on cobalt/cobalt oxide precursor particle；
Fig. 2 is the laser particle size analysis result of cobalt/cobalt oxide powder body in embodiment of the present invention group 1；
Fig. 3 is the SEM photograph that in embodiment of the present invention group 2, surfactant is affected on cobalt/cobalt oxide powder；
Fig. 4 is the laser particle size analysis result that in embodiment of the present invention group 2, surfactant is affected on cobalt/cobalt oxide powder；
Fig. 5 is the cobalt/cobalt oxide presoma SEM photograph for testing acquisition in embodiment of the present invention group 3；
Fig. 6 is the laser particle size analysis result of the cobalt/cobalt oxide powder for testing acquisition in embodiment of the present invention group 3；
Fig. 7 is the SEM photograph that in embodiment of the present invention group 4, temperature is affected on cobalt/cobalt oxide precursor particle；
Fig. 8 is the SEM photograph that in embodiment of the present invention group 4, the response time is affected on cobalt/cobalt oxide precursor particle；
Fig. 9 is the X ray diffracting spectrum of cobalt/cobalt oxide presoma in one embodiment of the invention；
Figure 10 is the flow chart of the preparation method of one embodiment of the present of invention.
Specific embodiment
Technical scheme is further illustrated below in conjunction with the accompanying drawings and by specific embodiment.
A kind of preparation method of cobalt/cobalt oxide powder, comprises the following steps：
A, precipitation：
Using ammonium bicarbonate soln as precipitant, add cobaltous chloride molten with the ultrasonic atomization spray add mode of back titration Liquid, and surfactant is simultaneously introduced, reaction obtains cobalt carbonate precipitation；Wherein, the concentration of the cobalt chloride solution is 0.2mol/ L, the concentration of the ammonium bicarbonate soln is 0.4mol/L；
B, it is separated by filtration：
Cobalt carbonate sediment is carried out cold drying after the unreacted material of water filtration removal water is removed, obtain cobalt/cobalt oxide Presoma；
C, thermal decomposition：
The cobalt/cobalt oxide presoma that step B is obtained is calcined at 500-600 DEG C, obtains Co3O4Powder；
Or, the cobalt/cobalt oxide presoma for obtaining step B is calcined at 1100-1200 DEG C, CoO powder is obtained.
During the application sedimentation method prepare cobalt/cobalt oxide presoma, ammonium hydrogen carbonate is selected as the precipitant of heavy cobalt, On the one hand pass through NH3With Co2+Complexation, expand Co2+Stability region, prevent from generating the high Co of easy reunion, decomposition temperature (OH)2, ammonium hydrogen carbonate is on the other hand selected as precipitant, can be to the not conscientious regulation of pH value, than selecting ammonium oxalate to make precipitant Compare, select ammonium hydrogen carbonate to be not required to other foreign ions are introduced, this washing procedure to reducing production process, improves product Purity is all favourable.Further description, the rate of deposition during ammonium hydrogen carbonate prepares cobalt/cobalt oxide presoma is relatively low, generally 70%-80%.
Further description, solution ph is larger on the rate of deposition impact of carbonate system, when pH value is less than 6.5, Precipitate in reaction solution can decompose, and precipitate disappears, and solution is changed into transparent, the presoma that this explanation carbonate system is obtained Decompose in acid condition, therefore, reaction solution will maintain more than certain pH value.
This project is in the case of back titration, and the pH value of reaction solution declined before this, pH=8 when by titration or so PH=6.8 when being down to titration end-point or so, then pH value is raised slowly to pH=7.2 or so again, makes this from ammonium hydrogen carbonate Reaction solution in project can maintain 7-8, without using pH adjusting agent, it is to avoid the other impurities of such as sodium ion, calcium ion etc. The introducing of ion.
As shown in Figure 10, the process is simple that the application is adopted, can obtain different cobalt oxidations according to different calcining heats Thing, and the cobalt/cobalt oxide powder purity height for generating, ion free from foreign meter, production efficiency height, cobalt powder particle size distribution interval is narrow, is obtained Co3O4The granularity of powder is 0.1-10 μm, and the granularity of CoO powder is 1-10 μm (being determined using laser particle analyzer), and dispersibility Good with nodularization effect, can be used for the added material of cell positive electrode.
Specific embodiment is as follows：
This test be with CoCl2For raw material, ammonium hydrogen carbonate is to make reactor precipitant, with the beaker with baffle plate, reacts Carry out in constant temperature blender with magnetic force.CoCl2Solution is the stock solution of the various concentration for preparing, and prepares CoCl2To carry out during solution Filter.Ammonium hydrogen carbonate recrystallizes standby reagent after drying for dissolving, title sample preparation before test every time.Certain density CoCl2Molten Liquid and ammonium bicarbonate soln are reacted in assigned temperature according to the needs of each process conditions respectively as reaction mother liquor or Deca solution Under carry out, gained sediment through filter, 70 DEG C vacuum drying.
Embodiment group 1 investigates impact of the positive and negative titration to cobalt/cobalt oxide presoma
Reaction condition：CoCl2Solution 0.2mol/L, 100ml；NH4HCO3Solution 0.4mol/L, 100ml；T=30 DEG C； CO3 2-/Co2+=2；Response time：T=30min；In course of reaction, pH is not adjusted；Wherein just titrating as spray plus NH4HCO3 Solution, back titration is spray plus CoCl2Solution.Result of the test is shown in Table 1, Fig. 1, Fig. 2.
Table 1：Experimental condition
Analytical table 1, Fig. 1 and the result of the test of Fig. 2, it can be deduced that such as draw a conclusion：Before ammonium salt system prepares cobalt/cobalt oxide During driving body, the impact of the feed postition of material to precursor particle particle diameter is very big, in the case of just titrating, obtains Precursor particle particle diameter is larger, about 0.5 μm, and particle is reunited in loose.And the precursor particle particle diameter very little that back titration is obtained, Only 50nm or so, presoma is reunited seriously, the hard aggregation in tight collapse.Therefore can be obtained according to the difference of feed way The presoma of two kinds of particle diameters, a kind of for particle diameter compared with the thick but preferable submicron particle of dispersibility, another kind of is a 50nm left side for particle diameter Right nanometer particle, but seriously, therefore nanometer particle reunites in dry run, needs to add surface in titration process Activating agent is solving the agglomeration traits of particle.
Having for explanation is needed, surfactant can be polyethylene glycol 1500, polyethylene glycol 6000 or Tween 80.
Embodiment group 2
Checking surface active agent tween 80 (T-80) is to forerunner during carbonate system prepares cobalt/cobalt oxide presoma The impact of body particle.
Reaction condition：CoCl2Solution 0.2mol/L, 100ml；NH4HCO3Solution 0.4mol/L, 100ml；T=20 DEG C of (room Temperature)；CO3 2-/Co2+=2；Response time：T=30min；In course of reaction, pH is not adjusted；(spray plus NH are just titrated4HCO3Molten Liquid).Result of the test is shown in Table 2, Fig. 3, Fig. 4.
Table 2：Experimental condition
Knowable to the result of the test of table 2, Fig. 3 and Fig. 4, during carbonate system prepares cobalt/cobalt oxide presoma, add Plus surfactant T-80 can play a part of to disperse precursor particle.Laser particle size analysis result shows, obtains after calcining Co3O44.48 μm of the apparent particle diameter average out to of powder.T-80 is selected further to improve the dispersibility of precursor particle.
Embodiment group 3
In this test, investigated under the conditions of 20 DEG C, 40 DEG C and 60 DEG C each temperature respectively to cobalt/cobalt oxide presoma or The impact of cobalt/cobalt oxide powder.In analyzing influence degree, respectively to the microscopic appearance of cobalt/cobalt oxide presoma and calcining after Cobalt/cobalt oxide powder is studied, and the research to the microscopic appearance of cobalt/cobalt oxide presoma is mainly seen by scanning electron microscope Examine, the research to cobalt/cobalt oxide powder granularity mainly measures the size of its particle diameter using laser particle size analyzer, and combines forerunner Reunion situation, color of body etc. carry out comprehensive analysis.
Reaction condition：CoCl2Solution 0.2mol/L, 100ml；NH4HCO3Solution 0.4mol/L, 100ml；Material addition side Formula：Back titration, ultrasonic atomization spray plus CoCl2Solution；CO3 2-/Co2+=2；T=30min；In course of reaction, pH is not adjusted Section.Result of the test is shown in Table 3, Fig. 6 (a) and Fig. 6 (b).Wherein Fig. 6 (a) is calcined for cobalt/cobalt oxide presoma through 500 DEG C for 4 hours The Co for arriving3O4The laser particle size analysis result of powder, the lumps material warp that Fig. 6 (b) is obtained after calcining for presoma hard aggregation Laser particle size analysis result after underhand polish.
Table 3：Experimental condition
The result of the test of analytical table 3, Fig. 5 and Fig. 6 understands, the cobalt/cobalt oxide presoma for obtaining under carbonate system is class Spherical, particle diameter is less, and typically below 0.5 μm, but presoma reunion is more serious.Can be seen that 21 from the SEM photograph of Fig. 5 At DEG C, the grain diameter of obtained cobalt/cobalt oxide presoma is 0.4 μm.Its table is understood from the laser particle size analysis result of Fig. 6 (a) See particle diameter and be 0.1-16 μm, mean diameter is 4.26 μm.Under this explanation low temperature, obtained presoma is loose soft-agglomerated, through super Sound wave rapping can make soft-agglomerated dispersion.And knowable to the laser particle size analysis result of table 3 and Fig. 6 (b), obtained at high temperature What presoma was formed is hard aggregation, and ultrasound wave rapping can not be disperseed, the particle diameter of the powder particle for obtaining after underhand polish Distribution is wide, and particle size is uneven.As can be seen here, under the conditions of back titration, impact of the reaction temperature to precursor particle is very big, Improve temperature and increased the reunion of precursor particle, obtained at low temperature presoma be loose soft-agglomerated, and at high temperature Hard aggregation is then formed.Therefore, low temperature (room temperature) condition is conducive to obtaining loose cobalt/cobalt oxide precursor powder.
Further description, in principle, the response time is shorter, and particle diameter is less, and distribution is narrower, but in practical situation Under, particle size distribution enter quickly " self-insurance " distribution form (i.e. the apparent particle size distribution shape for different time is similar, and with initial Concentration distribution is unrelated), wayward.The catabiosis of colloidal particle are there are in real process, and the holding appropriate reaction time can Particle size distribution is made to narrow relatively.
Embodiment group 4
Under the conditions of back titration, the response time has been investigated respectively for the response time in the case of 10min and two kinds of 60min to front Drive the impact of body particle.
Reaction condition：CoCl2Solution 0.2mol/L, 100ml；NH4HCO3Solution 0.4mol/L, 100ml；Material addition side Formula：Back titration；CO3 2-/Co2+=2；T=40 DEG C；In course of reaction, pH is not adjusted.Result of the test is shown in Table 4, Fig. 7, Fig. 8.
Table 4：Experimental condition
As can be seen from Figure 7, the response time is longer, is more conducive to the growth of precursor particle.Can from the amplification picture of Fig. 7 Go out, granular precursor is formed by less small particles aggregation again, and when the response time is 10min, precursor particle is in 100nm Hereinafter, in random reunion (see Fig. 8 (a)).React and grow up for, after 60min, precursor particle is aggregated, form particle diameter about The spherical particle (see Fig. 8 (b)) of 0.5um.Therefore, it can control the grain of presoma by controlling the digestion time for reacting Footpath, so as to produce the presoma of different-grain diameter as needed.The result of the test of group 3 and 4 shows in conjunction with the embodiments, the response time pair The impact of precipitate particle sizes is little, and the impact to rate of deposition is more obvious, and the prolongation response time is conducive to the raising of rate of deposition, It is preferred that the time is 30min.
Further description, precipitant ((NH4)2C2O4·H2O) excess coefficient test is mainly investigation precipitant consumption Impact to cobalt/cobalt oxide precursor particle and rate of deposition.Show through overtesting, precipitant excess coefficient is to precipitate granularity Impact is less, and excess coefficient is little, and slightly beneficial to generating, particle diameter is little, good dispersion particle.But precipitant excess coefficient is to rate of deposition Impact very big, by testing the rate of deposition data that obtain, raising precipitant excess coefficient significantly enhances presoma Rate of deposition.In the industrial production, selected suitable precipitant excess coefficient is extremely important, and precipitant excess coefficient is less than normal, meeting Affect the response rate of main metal；Precipitant excess coefficient is bigger than normal, can not only increase the consumption of raw material, and can increase technical process Logistics capacity, so as to increase production cost, therefore, the preferred precipitant excess coefficient of this programme be C2O4 2-/Co2+=2.
Embodiment 5
A, precipitation：Using ammonium hydrogen carbonate (NH4HCO3) as precipitant, in the precipitant Deca mode of back titration, using super Sound wave atomization spray plus CoCl2Solution, is simultaneously introduced surfactant T-80,20 DEG C of reaction temperature, and the response time is 30min, to sink Agent excess coefficient in shallow lake is 2 (C2O4 2-/Co2+=2), obtained cobalt carbonate precipitation；
B, it is separated by filtration：The precipitation that step A is obtained removes unreacted material in precipitation through washing filtering, then through low temperature Dry and remove most moisture, prepared cobalt/cobalt oxide presoma；
C, thermal decomposition：With Muffle furnace at 600 DEG C, obtained presoma basic cobaltous carbonate in 4 hours calcining first steps, Prepare Co3O4Powder.In tube furnace, under the conditions of logical nitrogen is as protective atmosphere, 4 hours calcining first steps at 1200 DEG C In rapid, obtained presoma basic cobaltous carbonate, prepares CoO powder.
Embodiment 6
A, precipitation：Using ammonium hydrogen carbonate (NH4HCO3) as precipitant, in the precipitant Deca mode of back titration, using super Sound wave atomization spray plus CoCl2Solution, is simultaneously introduced surfactant T-80,20 DEG C of reaction temperature, and the response time is 30min, to sink Agent excess coefficient in shallow lake is 2 (C2O4 2-/Co2+=2), obtained cobalt carbonate precipitation；
B, it is separated by filtration：The precipitation that step A is obtained removes unreacted material in precipitation through washing filtering, then through low temperature Dry and remove most moisture, prepared cobalt/cobalt oxide presoma；
C, thermal decomposition：With Muffle furnace at 500 DEG C, obtained presoma basic cobaltous carbonate in 5 hours calcining first steps, Prepare Co3O4Powder.In tube furnace, under the conditions of logical nitrogen is as protective atmosphere, 5 hours calcining first steps at 1100 DEG C In rapid, obtained presoma basic cobaltous carbonate, prepares CoO powder.
Further description, the cobalt/cobalt oxide presoma that step B is obtained is basic cobaltous carbonate.Before the cobalt/cobalt oxide of acquisition It is spherical to drive body, and particle diameter is less, typically below 0.5 μm, analyzes the X-ray of cobalt/cobalt oxide presoma obtained in ammonium hydrogen carbonate Diffracting spectrum (see Fig. 9), it can be seen that the presoma for obtaining under the system is amorphous substance.Divide in conjunction with the thermogravimetric of presoma Analysis, it can be determined that the presoma is basic cobaltous carbonate.
The know-why of the present invention is described above in association with specific embodiment.These descriptions are intended merely to explain the present invention's Principle, and limiting the scope of the invention can not be construed to by any way.Based on explanation herein, the technology of this area Personnel associate other specific embodiments of the present invention by need not paying performing creative labour, these modes fall within Within protection scope of the present invention.

Claims (9)

1. a kind of preparation method of cobalt/cobalt oxide powder, it is characterised in that：Comprise the following steps：
A, precipitation：
Using ammonium bicarbonate soln as precipitant, cobalt chloride solution is added with the ultrasonic atomization spray add mode of back titration, and Surfactant is simultaneously introduced, reaction obtains cobalt carbonate precipitation；Wherein, the concentration of the cobalt chloride solution is 0.2mol/L, institute The concentration for stating ammonium bicarbonate soln is 0.4mol/L；
B, it is separated by filtration：
Cobalt carbonate sediment is carried out cold drying after the unreacted material of water filtration removal water is removed, obtain cobalt/cobalt oxide forerunner Body；
C, thermal decomposition：
The cobalt/cobalt oxide presoma that step B is obtained is calcined at 500-600 DEG C, obtains Co3O4Powder；
Or, the cobalt/cobalt oxide presoma for obtaining step B is calcined at 1100-1200 DEG C, CoO powder is obtained.
2. the preparation method of a kind of cobalt/cobalt oxide powder according to claim 1, it is characterised in that：The surfactant For Tween 80.
3. the preparation method of a kind of cobalt/cobalt oxide powder according to claim 1, it is characterised in that：Step A anti- Temperature is answered for 20 DEG C.
4. the preparation method of a kind of cobalt/cobalt oxide powder according to claim 1, it is characterised in that：Step A anti- It is 30min between seasonable.
5. the preparation method of a kind of cobalt/cobalt oxide powder according to claim 1, it is characterised in that：Step A heavy Agent excess coefficient in shallow lake is C2O4 2-/Co2+=2.
6. the preparation method of a kind of cobalt/cobalt oxide powder according to claim 1, it is characterised in that：CoO in step C The preparation of powder is carried out in tube furnace.
7. the preparation method of a kind of cobalt/cobalt oxide powder according to claim 6, it is characterised in that：Make in step C Tube furnace is passed through nitrogen.
8. the preparation method of a kind of cobalt/cobalt oxide powder according to claim 1, it is characterised in that：The forging of step C The burning time is 4h.
9. the preparation method of a kind of cobalt/cobalt oxide powder according to claim 1, it is characterised in that：The cobalt that step B is obtained Oxide precursor is basic cobaltous carbonate.
CN201610594957.2A 2016-07-26 2016-07-26 Preparation method of cobalt oxide powder Pending CN106430330A (en)

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Cited By (4)

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CN111132932A (en) * 2019-12-30 2020-05-08 东江环保股份有限公司 Preparation method of basic copper carbonate
CN113617346A (en) * 2021-08-18 2021-11-09 珠海市科立鑫金属材料有限公司 Preparation method of small-particle cobaltosic oxide
CN115710022A (en) * 2022-11-17 2023-02-24 科立鑫(珠海)新能源有限公司 Preparation method of high-density cobalt carbonate
CN116789184A (en) * 2023-07-12 2023-09-22 科立鑫(珠海)新能源有限公司 Environment-friendly process for producing cobaltous oxide

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