CN103071807A - Preparation method of ultra-fine spherical cobalt powder - Google Patents
Preparation method of ultra-fine spherical cobalt powder Download PDFInfo
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- CN103071807A CN103071807A CN2012104751424A CN201210475142A CN103071807A CN 103071807 A CN103071807 A CN 103071807A CN 2012104751424 A CN2012104751424 A CN 2012104751424A CN 201210475142 A CN201210475142 A CN 201210475142A CN 103071807 A CN103071807 A CN 103071807A
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Abstract
The invention relates to a preparation method of ultra-fine spherical cobalt powder, which adopts a solvent synchronizing method and a hydrogen reduction method to prepare ultra-fine spherical cobalt powder. The method comprises the following steps of adopting urea or ammonium carbonate as precipitating agent, adopting ethylene glycol, 1,2-propylene glycol or water as solvent, utilizing the solvent synchronizing method to transfer a solution or slurry prepared from cobalt salt and the precipitating agent into a reaction kettle, heating the reaction kettle to a proper temperature in an oven, and preserving the temperature for proper time, cooling the reaction kettle to a room temperature to obtain precipitate; washing, filtering and drying the precipitate to obtain precursors; reducing the precursor powder in argon/nitrogen mixed gases to finally obtain the ultra-fine spherical cobalt powder, wherein the particle granularity is less than 1 micron. The preparation method provided by the invention has the advantages that the process is simple, the production efficiency is high, the distribution area of the cobalt powder granularity is narrow, the particle granularity is less than 1 micron, and the scattering and spherodization effects are good.
Description
Technical field
The invention belongs to the superfine powder preparation field, be specifically related to a kind of preparation method of the superfine spherical cobalt powder that evenly, disperses.
Background technology
The magnetic cobalt powder has good physical property, chemical property and mechanical performance, is widely used in the industries such as battery material, carbide alloy, diamond instrument, cermet.And the fields such as battery material, carbide alloy and diamond instrument are to the cobalt powder basic demand: the cobalt powder particle is tiny, and (particle diameter＜1.5um), favorable dispersibility and pattern are that sphere or class are spherical, and chemical purity is high.Its reason is: superfine spherical cobalt powder has good flowability, and therefore higher compactedness and the stronger characteristics such as permeability, have important engineering significance to the development of superfine spherical cobalt powder.
At present, the method for preparing super-fine cobalt powder both at home and abroad is a lot, mainly contains the high-pressure water spray method, electrolysis, gamma-radiation radiation method, polyol reduction method, precipitation-thermal dissociation method, cobalt oxide or cobalt oxalate hydrogen reduction method etc.The high-pressure water spray method is a kind of physical method, and production technology is simple, and is pollution-free, but the cobalt powder particle of its preparation is thick, and particle diameter is at 20～50um; Electrolysis can only prepare the cobalt powder of general performance; The cobalt powder particle that the gamma-radiation radiation method makes is little, and mostly is α-Co, but is difficult to realize suitability for industrialized production; Polyol reduction method, wherein polyalcohol both had been solvent, was reducing agent again, and reduction temperature is low, and the cobalt powder particle is little and the nodularization rate high, but polyalcohol is unstable, easily decomposes; The baking temperature of precipitation-thermal dissociation method is wayward, and the atmosphere that needs protection; The hydrogen reduction method of the oxide of cobalt oxalate or cobalt is one of domestic main production cobalt powder method, and its technological process is simple, productive rate and efficient are high, be suitable for suitability for industrialized production, but the cobalt powder of the method preparation mainly is dendroid from morphology analysis, and dispersion effect is poor; From the chemical purity analysis, to compare with the cobalt powder of advanced manufacturer production, its chemical purity is lower, and impurity is more; From grain size analysis, be generally 1.0um～3.0um, and 1.0um following be difficult to large-scale production.If such cobalt powder is applied in battery, the carbide alloy, can reduce its combination property, make troubles to practical application.
Comparatively speaking, prepare superfine spherical cobalt powder, and can realize that the effective method of suitability for industrialized production is hydrogen reduction method, because the predecessor granule-morphology determines the pattern of final reduction cobalt powder, therefore, the scientific research personnel is devoted to the presoma of hydrogen reduction method is studied both at home and abroad.Number of patent application is 200410068855.4 to adopt air-flow supersonic sprayings to prepare＜presoma of the CoOx of 60nm, through roasting, and shearing-crushing, centrifugal, air-dry, again through tube furnace H
2Reduction preparation nano-cobalt powder, but operation is tediously long, and control is complicated; Number of patent application is that 200610067164.1 employing Freeze Drying Techniques are directly carried out the pre-freeze processing to the cobalt oxalate that does not add any surfactant, and then passes into H
2Reduction obtains superfine spherical cobalt powder, but drying time is long and efficient is low; Number of patent application is 200710075929.0 cobalt carbonate or cobalt oxalate to be carried out high-energy ball milling, thereby obtains ultra-fine cobalt carbonate or the presoma of cobalt oxalate, and then uses H
2Reduction preparation superfine spherical cobalt powder, but in ball milling, easily introduce impurity, and particle is easily grown up during reduction; Number of patent application is 201010196228.4 take carbonic hydroammonium as precipitating reagent, adds with cobalt salt solution and stream mode and prepares Cobalt carbonate sediment in the reactor, and then use H
2The cobalt powder of the subsphaeroidal focusing shape of reduction preparation, but during the preparation Cobalt carbonate sediment, influence factor is more such as temperature, charging rate, concentration etc., and the cobalt powder nodularization effect that makes is not ideal.
Summary of the invention
The defective that exists in order to overcome prior art, the invention provides a kind of method for preparing superfine spherical cobalt powder, the method is in conjunction with the advantage of solvent synthetic method and hydrogen reduction method, and its purpose is to prepare that particle is tiny, the super-fine cobalt powder of nodularization rate height and good dispersion, and concrete steps are as follows:
(1) presses the precipitating reagent weighing of 1.05～1.3 times of cobalt salt and theoretical reacting doses, take by weighing again the surfactant of gross mass 2wt%～6wt%; First cobalt salt is dissolved in a certain amount of solvent, be mixed with the A solution of 0.25mol/l～0.8mol/l, surfactant and precipitating reagent are joined respectively in the A solution again, strong agitation forms B solution or slip; Its described cobalt salt is CoCL2 6H2O, cobalt sulfate or cobalt nitrate hexahydrate; Described precipitating reagent is urea or ammonium carbonate; Described surfactant is lauryl sodium sulfate (SDS), PVP (PVP), neopelex (SDBS), polyethylene glycol (PEG); Described solvent is ethylene glycol, 1,2-PD or water;
(2) leave standstill ten minutes after, above-mentioned B solution or slip are transferred in the reactor, again reactor is put in the drying box, temperature is 150 ℃～220 ℃, temperature retention time is 8 ~ 24h, carries out corresponding chemical reaction, generates sediment; (the solvent synthetic method prepares presoma)
(3) by to sedimentary suction filtration, washing, drying, obtain presoma;
(4) presoma that obtains is calcined under reducing atmosphere, calcining heat is 500～700 ℃, and calcination time is the spherical cobalt powder that 1.5 ~ 5h obtains granularity＜1um;
Compared with prior art, the present invention has following useful effect:
(1) this reaction system is to carry out at airtight reactor (reactor), by to reactor heating, thereby creates the environment of a HTHP, so that chemical reaction velocity is fast, reactivity is high;
(2) the present invention adopts the solvent synthetic method to prepare presoma, uses hydrogen reducing again, prepared cobalt powder, and its dispersion effect is relatively good, and pattern is more even;
(3) adopt the present invention to prepare the spherical cobaltous carbonate presoma, its particle is little, good dispersion, and it is few to introduce impurity, and this gives security for the high spherical cobalt powder of preparation purity.
Description of drawings
Fig. 1 is process chart of the present invention;
Fig. 2 is the SEM collection of illustrative plates of the super-fine cobalt powder of embodiment 1;
Fig. 3 is the SEM collection of illustrative plates of the super-fine cobalt powder of embodiment 2;
Fig. 4 is the SEM collection of illustrative plates of the super-fine cobalt powder of embodiment 3;
Fig. 5 is the SEM collection of illustrative plates of the super-fine cobalt powder of embodiment 4;
Fig. 6 is the XRD collection of illustrative plates of the cobalt powder of 600 ℃ of reduction 3h.
The specific embodiment
Embodiment 1
N (CoCl in molar ratio
2.6H
2O): n (CON
2H
4)=1:1.05 takes by weighing respectively the CoCl of 0.02mol
2.6H
2O, the CON of 0.21mol
2H
4Take by weighing again the lauryl sodium sulfate (SDS) of above medicine gross mass 6wt%; Measure the ethylene glycol (EG) of 25ml as solvent; Under the room temperature, with CoCl
2.6H
2O is dissolved among the EG, is mixed with the A solution of 0.8mol/l, again with SDS and CON
2H
4Add in the A solution, strong agitation is until form B solution, leave standstill ten minutes after, B solution is transferred in the 40ml reactor, and is heated to 150 ℃, behind the insulation 24h, be cooled to room temperature, respectively water and ethanol washing, suction filtration obtains the cobalt carbonate presoma after the drying; Presoma is reduced under the mist by argon/hydrogen, and reduction temperature is 580 ℃, and the recovery time is 3h, namely gets superfine spherical cobalt powder, and its pattern as shown in Figure 2.
Embodiment 2
N (CoCl in molar ratio
2.6H
2O): n (CON
2H
4)=1:1.1 takes by weighing respectively the CoCl of 0.01mol
2.6H
2O, the CON of 0.11mol
2H
4Take by weighing again the lauryl sodium sulfate (SDS) of above medicine gross mass 5wt%; Measure the ethylene glycol (EG) of 20ml as solvent; First EG is heated to 30 ℃ and insulation, with CoCl
2.6H
2O is dissolved among the EG, is mixed with the A solution of 0.5mol/l, again with SDS and CON
2H
4Add in the A solution, strong agitation is until form B solution, leave standstill ten minutes after, B solution is transferred in the reactor of 40ml, and is heated to 160 ℃, behind the insulation 18h, be cooled to room temperature, water and ethanol wash respectively, suction filtration obtains presoma after the drying; Presoma is reduced under the mist by argon/hydrogen, and reduction temperature is 600 ℃, and the recovery time is 3h, namely gets superfine spherical cobalt powder, and its pattern as shown in Figure 3.
Embodiment 3
N (CoCl in molar ratio
2.6H
2O): n (CON
2H
4)=1:1.2 takes by weighing respectively the CoCl of 0.01mol
2.6H
2O, the CON of 0.12mol
2H
4Take by weighing again the lauryl sodium sulfate (SDS) of above medicine gross mass 4wt%; Measure the ethylene glycol (EG) of 25ml as solvent; First EG is heated to 50 ℃ and insulation, with CoCl
2.6H
2O is dissolved among the EG, is mixed with the A solution of 0.4mol/l, again with SDS and CON
2H
4Add in the A solution, strong agitation is until form B solution, leave standstill ten minutes after, B solution is transferred in the reactor of 40ml, and is heated to 170 ℃, behind the insulation 15h, be cooled to room temperature, water and ethanol wash respectively, suction filtration obtains presoma after the drying; Presoma is reduced under the mist by argon/hydrogen, and reduction temperature is 630 ℃, and the recovery time is 2.5h, namely gets superfine spherical cobalt powder, and its pattern as shown in Figure 4.
Embodiment 4
N (Co (NO in molar ratio
3)
2.6H
2O): n (CON
2H
4)=1:1.1 takes by weighing respectively 0.01mol Co (NO
3)
2.6H
2O, the CON of 0.11mol
2H
4Take by weighing again the lauryl sodium sulfate (SDS) of above medicine gross mass 3wt%; Measure the ethylene glycol (EG) of 40ml as solvent; First EG is heated to 70 ℃ and insulation, with CoCl
2.6H
2O is dissolved among the EG, is mixed with the A solution of 0.25mol/l, again with SDS and CON
2H
4Add in the A solution, strong agitation is until form B solution, leave standstill ten minutes after, B solution is transferred in the reactor of 50ml, and is heated to 180 ℃, behind the insulation 13h, be cooled to room temperature, water and ethanol wash respectively, suction filtration obtains presoma after the drying; Presoma is reduced under the mist by argon/hydrogen, and reduction temperature is 650 ℃, and the recovery time is 2.5h, namely gets superfine spherical cobalt powder, and its pattern as shown in Figure 5.
Embodiment 5
N (Co (NO in molar ratio
3)
2.6H
2O): n (CON
2H
4)=1:1.2 takes by weighing respectively 0.02mol Co (NO
3)
2.6H
2O, the CON of 0.24mol
2H
4Take by weighing again the lauryl sodium sulfate (SDS) of above medicine gross mass 2wt%; Measure the ethylene glycol (EG) of 40ml as solvent; First EG is heated to 30 ℃ and insulation, again with CoCl
2.6H
2O is dissolved among the EG, is mixed with the A solution of 0.5mol/l, again with SDS and CON
2H
4Add in the A solution, strong agitation is until form B solution, leave standstill ten minutes after, B solution is transferred in the reactor of 50ml, and is heated to 200 ℃, behind the insulation 10h, be cooled to room temperature, water and ethanol wash respectively, suction filtration obtains presoma after the drying; Presoma is reduced under the mist by argon/hydrogen, and reduction temperature is 700 ℃, and the recovery time is 1.5h, namely obtains superfine spherical cobalt powder.
Embodiment 6
N (CoSO in molar ratio
4.7H
2O): n (CON
2H
4)=1:1.1 takes by weighing respectively the CoSO of 0.02mol
4.7H
2O, the CON of 0.22mol
2H
4Take by weighing again the lauryl sodium sulfate (SDBS) of above medicine gross mass 4wt%; Measure the ethylene glycol (EG) of 40ml as solvent; First EG is heated to 30 ℃ and insulation, again with CoCl
2.6H
2O is dissolved among the EG, is mixed with the A solution of 0.5mol/l, again with SDS and CON
2H
4Add in the A solution, strong agitation is until form B solution, leave standstill ten minutes after, B solution is transferred in the reactor of 50ml, and is heated to 220 ℃, behind the insulation 8h, be cooled to room temperature, water and ethanol wash respectively, suction filtration obtains presoma after the drying; Presoma is reduced under the mist by argon/hydrogen, and reduction temperature is 580 ℃, and the recovery time is 3h, namely obtains superfine spherical cobalt powder.
Embodiment 7
N (CoSO in molar ratio
4.7H
2O): n (CON
2H
4)=1:1.2 takes by weighing respectively the CoSO of 0.02mol
4.7H
2O, the CON of 0.24mol
2H
4Take by weighing again the PVP (PVP) of above medicine gross mass 3wt%; Measure the ethylene glycol of 40ml as solvent; First solvent is heated to 30 ℃ and insulation, again with CoCl
2.6H
2O is dissolved in the solvent, is mixed with the A solution of 0.5mol/l, again with SDS and CON
2H
4Add in the A solution, strong agitation is until form B solution, leave standstill ten minutes after, B solution is transferred in the reactor of 50ml, and is heated to 190 ℃, behind the insulation 11h, be cooled to room temperature, water and ethanol wash respectively, suction filtration obtains presoma after the drying; Presoma is reduced under the mist by argon/hydrogen, and reduction temperature is 500 ℃, and the recovery time is 5h, namely gets superfine spherical cobalt powder.
Example 8
N (CoCl in molar ratio
2.6H
2O): n (CON
2H
4)=1:1.1 takes by weighing respectively the CoCl of 0.02mol
2.6H
2O, the CON of 0.22mol
2H
4Take by weighing again the lauryl sodium sulfate (SDS) of above medicine gross mass 4wt%; Measure the 1,2-PD (EG) of 40ml as solvent; First EG is heated to 30 ℃ and insulation, again with CoCl
2.6H
2O is dissolved among the EG, is mixed with the A solution of 0.5mol/l, again with SDS and CON
2H
4Add in the A solution, strong agitation is until form B solution, leave standstill ten minutes after, B solution is transferred in the reactor of 50ml, and is heated to 180 ℃, behind the insulation 13h, be cooled to room temperature, water and ethanol wash respectively, suction filtration obtains presoma after the drying; Presoma is reduced under the mist by argon/hydrogen, and reduction temperature is 600 ℃, and the recovery time is 3h, namely obtains superfine spherical cobalt powder.
Embodiment 9
N (CoSO in molar ratio
4.7H
2O): n (CON
2H
4)=1:1.3 takes by weighing respectively the CoSO of 0.02mol
4.7H
2O, (the NH of 0.26mol
4)
2CO
3Take by weighing again the polyethylene glycol (PEG) of above medicine gross mass 4wt%; Measure the water of 40ml as solvent; Under the room temperature, with CoSO
4.7H
2O is soluble in water, is mixed with the A solution of 0.5mol/l, again with PEG and (NH
4)
2CO
3Add A solution, stir until the B slip that forms, leave standstill ten minutes after, the B slip is transferred in the reactor of 50ml, and is heated to 160 ℃, behind the insulation 18h, be cooled to room temperature, water and ethanol wash respectively, suction filtration obtains presoma after the drying; Presoma is reduced under the mist by argon/hydrogen, and reduction temperature is 550 ℃, and the recovery time is 3.5h, namely gets superfine spherical cobalt powder.
Claims (2)
1. superfine spherical cobalt powder preparation method is characterized in that it may further comprise the steps:
(1) presses the weighing of cobalt salt and 1.05～1.3 times of precipitating reagents of theoretical reacting dose, take by weighing again the surfactant of gross mass 2wt%～6wt%; First cobalt salt is dissolved in a certain amount of solvent, be mixed with the A solution of 0.25mol/l～0.8mol/l; Surfactant and precipitating reagent are joined respectively in the A solution, and strong agitation forms B solution or slip; Its described cobalt salt is CoCL2 6H2O, cobalt sulfate or cobalt nitrate hexahydrate; Described precipitating reagent is urea or ammonium carbonate; Described surfactant is lauryl sodium sulfate, PVP (PVP), neopelex (SDBS), polyethylene glycol (PEG); Described solvent is ethylene glycol, 1,2-PD or water;
(2) leave standstill ten minutes after, the above-mentioned B of obtaining solution or slip are transferred in the reactor, again reactor is put in the drying box, temperature is 150～220 ℃, temperature retention time is 8～24h, carries out corresponding chemical reaction, generates sediment; (solvent method prepares presoma)
(3) by to sedimentary suction filtration, washing, drying, obtain presoma;
(4) presoma that obtains is calcined under reducing atmosphere, calcining heat is 500～700 ℃, and calcination time is the spherical cobalt powder that 1.5-5h obtains granularity＜1um; Described reducing atmosphere is argon/hydrogen gas mixture.
2. the preparation method of a kind of superfine spherical cobalt powder according to claim 1 is characterized in that forming in B solution or the slip process in preparation described in the step (1), and its solvent temperature is room temperature～70 ℃ scopes.
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| CN103752820A (en) * | 2014-02-19 | 2014-04-30 | 南京林业大学 | Method for preparing modified nanometer cobalt powder |
| CN106077694A (en) * | 2016-08-08 | 2016-11-09 | 南昌大学 | A kind of preparation method of spherical cobalt powder |
| CN106270554A (en) * | 2016-09-28 | 2017-01-04 | 广州凯耀资产管理有限公司 | A kind of preparation method of super-fine cobalt powder |
| CN106964784A (en) * | 2017-05-27 | 2017-07-21 | 湘潭大学 | A kind of preparation method of cobalt powder |
| CN108526476A (en) * | 2018-04-08 | 2018-09-14 | 南京寒锐钴业股份有限公司 | A kind of preparation method of diamond tool cobalt powder |
| CN111727932A (en) * | 2020-06-30 | 2020-10-02 | 倪仲周 | Organic black pig breeding method |
| CN112846213A (en) * | 2021-01-05 | 2021-05-28 | 有研工程技术研究院有限公司 | Preparation method of low-oxygen high-dispersion nano spherical cobalt powder |
| CN113909485A (en) * | 2021-10-11 | 2022-01-11 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
| CN114230456A (en) * | 2021-12-24 | 2022-03-25 | 马鞍山昂扬新材料科技有限公司 | Synthesis process of cobalt acetate |
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| CN108526476A (en) * | 2018-04-08 | 2018-09-14 | 南京寒锐钴业股份有限公司 | A kind of preparation method of diamond tool cobalt powder |
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| CN112846213A (en) * | 2021-01-05 | 2021-05-28 | 有研工程技术研究院有限公司 | Preparation method of low-oxygen high-dispersion nano spherical cobalt powder |
| CN113909485A (en) * | 2021-10-11 | 2022-01-11 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
| CN113909485B (en) * | 2021-10-11 | 2023-11-17 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
| CN114230456A (en) * | 2021-12-24 | 2022-03-25 | 马鞍山昂扬新材料科技有限公司 | Synthesis process of cobalt acetate |
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Application publication date: 20130501 |