CN107680768A - A kind of preparation method of cobalt nano magnetic material - Google Patents
A kind of preparation method of cobalt nano magnetic material Download PDFInfo
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- CN107680768A CN107680768A CN201710917496.2A CN201710917496A CN107680768A CN 107680768 A CN107680768 A CN 107680768A CN 201710917496 A CN201710917496 A CN 201710917496A CN 107680768 A CN107680768 A CN 107680768A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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Abstract
The invention discloses a kind of preparation method of cobalt nano magnetic material, prepares NaOH solution and CoCl respectively first2Solution, by CoCl2Solution is slowly dropped into NaOH solution, is stirred continuously to being uniformly dispersed, and obtains blue-tinted transparent solution；95wt% aqueous povidone solutions and 35wt% hydrazine hydrates is added dropwise successively again, obtains blue mixed solution；Blue mixed solution is transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, reactor is put into vacuum drying chamber and reacted；Autoclave is taken out after the completion of reaction, obtains colourless transparent solution and black precipitate；Centrifugation, the black precipitate in reaction product is washed with absolute ethyl alcohol and deionized water successively, then by black precipitate material drying to constant weight, that is, obtains cobalt nano magnetic material.Present invention process is simple, obtained cobalt nano magnetic material uniform particle diameter, good dispersion, crystalline in branch, has excellent magnetic property.
Description
Technical field
The invention belongs to field of magnetic material, is related to a kind of cobalt nano magnetic material, and in particular to a kind of cobalt nano-magnetic
The preparation method of material.
Background technology
Cobalt nano magnetic material is widely used in hard with its special physics, chemical property and magnetic property and closed
An industries such as gold, battery, permanent-magnet material, diamond tool manufacture, however, the property of magnetic nanoparticle depends on
Grain size and scattered degree.Therefore, single dispersing is prepared, the nano-particle of uniform particle diameter turns into the heat that nano magnetic material is studied
Point.At present, preparing the method for cobalt nano magnetic material both at home and abroad has electrolysis, high-pressure water spray method, oxalates thermal decomposition method, super
Sound atomization thermal decomposition method, polyol process, gas phase hydrogen reduction method, high pressure hydrogen reduction method, cobalt oxalate hydrogen reduction method, hydrazine hydrate liquid phase
Reducing process etc..Wherein, hydrazine hydrate liquid phase reduction is applied relatively broad, and it is passed through using hydrazine hydrate as reducing agent in aqueous medium
Thermal reduction is made, but obtained product has the problem of particle diameter is uneven, particle diameter is big.
The content of the invention
It is an object of the invention to provide a kind of preparation method of cobalt nano magnetic material, step is simple, and particle size is made
Uniformly.
To achieve these goals, the present invention adopts the following technical scheme that：A kind of preparation method of cobalt nano magnetic material,
Comprise the following steps：
(1) NaOH and ethylene glycol are weighed respectively, prepare the NaOH ethylene glycol solutions that 20mL concentration is 10~15mol/L, and
It is cooled to room temperature；
(2) CoCl is weighed respectively2·6H2O and glycerine, prepare the CoCl that 10mL concentration is 0.05~0.15mol/L2Third
Three alcoholic solutions；
(3) CoCl of 1mL steps 2 preparation is pipetted with pipette2Glycerin solution, it is slowly dropped into what is prepared in step 1
In NaOH ethylene glycol solutions, it is stirred continuously to being uniformly dispersed, obtains blue-tinted transparent solution；
(4) under same mixing speed, 95wt% aqueous povidone solutions and 35wt% hydrations are added dropwise successively
Hydrazine, obtain blue mixed solution；
(5) the blue mixed solution obtained in step 4 is transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, tightened anti-
Kettle is answered, and repeated multiple times concussion is shaken, and then reactor is put into vacuum drying chamber, sets reaction temperature as 120~200
DEG C, the reaction time is 2~5h；
(6) after the completion of reacting, treat that vacuum drying chamber is cooled to room temperature, take out autoclave, obtain colourless transparent solution and black
Color precipitates；
(7) centrifuge, the black precipitate in reaction product is washed 3~5 times with absolute ethyl alcohol and deionized water successively, then
Black precipitate material is placed in vacuum drying chamber and dried to constant weight, that is, obtains cobalt nano magnetic material.
Preferably, the volume ratio of the aqueous povidone solution in described step 4 and hydrazine hydrate is 1:1~2:5.
Preferably, the reaction temperature in described step 5 is 180 DEG C, reaction time 2h.
Preferably, mode of washing uses supersound washing in described step 7, and ultrasonic time is 3~5min.
Preferably, the drying temperature in described step 7 is 50~60 DEG C, and drying time is 6~8h.
The preparation technology of the present invention is simple, using hydrazine hydrate as reducing agent, using polyvinylpyrrolidone as complexant, with second two
Alcohol and glycerine replace water as medium, and obtained cobalt nano magnetic material uniform particle diameter, good dispersion are crystalline in branch, have
Excellent magnetic property.
Embodiment
The present invention is described in further detail with reference to specific embodiment.
Embodiment 1
A kind of preparation method of cobalt nano magnetic material, comprises the following steps：
(1) NaOH and ethylene glycol are weighed respectively, are prepared 20mL concentration and are 15mol/L NaOH ethylene glycol solutions, and cool down
To room temperature；
(2) CoCl is weighed respectively2·6H2O and glycerine, prepare the CoCl that 10mL concentration is 0.1mol/L2Glycerine is molten
Liquid；
(3) CoCl of 1mL steps 2 preparation is pipetted with pipette2Glycerin solution, it is slowly dropped into what is prepared in step 1
In NaOH ethylene glycol solutions, it is stirred continuously to being uniformly dispersed, obtains blue-tinted transparent solution；
(4) under same mixing speed, 95wt% aqueous povidone solutions and 35wt% hydrations are added dropwise successively
The volume ratio of hydrazine, aqueous povidone solution and hydrazine hydrate is 1:1, obtain blue mixed solution；
(5) the blue mixed solution obtained in step 4 is transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, tightened anti-
Kettle is answered, and repeated multiple times concussion is shaken, and then reactor is put into vacuum drying chamber, sets reaction temperature as 180 DEG C, is reacted
Time is 2h；
(6) after the completion of reacting, treat that vacuum drying chamber is cooled to room temperature, take out autoclave, obtain colourless transparent solution and black
Color precipitates；
(7) centrifuge, by the black precipitate in reaction product successively with absolute ethyl alcohol and deionized water supersound washing 3~5 times,
Each ultrasonic 3min, then black precipitate material is placed in vacuum drying chamber and dried to constant weight, drying temperature is 60 DEG C, is dried
Time is 6h, that is, obtains cobalt nano magnetic material.
Embodiment 2
A kind of preparation method of cobalt nano magnetic material, comprises the following steps：
(1) NaOH and ethylene glycol are weighed respectively, are prepared 20mL concentration and are 10mol/L NaOH ethylene glycol solutions, and cool down
To room temperature；
(2) CoCl is weighed respectively2·6H2O and glycerine, prepare the CoCl that 10mL concentration is 0.15mol/L2Glycerine is molten
Liquid；
(3) CoCl of 1mL steps 2 preparation is pipetted with pipette2Glycerin solution, it is slowly dropped into what is prepared in step 1
In NaOH ethylene glycol solutions, it is stirred continuously to being uniformly dispersed, obtains blue-tinted transparent solution；
(4) under same mixing speed, 95wt% aqueous povidone solutions and 35wt% hydrations are added dropwise successively
The volume ratio of hydrazine, aqueous povidone solution and hydrazine hydrate is 2:5, obtain blue mixed solution；
(5) the blue mixed solution obtained in step 4 is transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, tightened anti-
Kettle is answered, and repeated multiple times concussion is shaken, and then reactor is put into vacuum drying chamber, sets reaction temperature as 200 DEG C, is reacted
Time is 2h；
(6) after the completion of reacting, treat that vacuum drying chamber is cooled to room temperature, take out autoclave, obtain colourless transparent solution and black
Color precipitates；
(7) centrifuge, by the black precipitate in reaction product successively with absolute ethyl alcohol and deionized water supersound washing 3~5 times,
Each ultrasonic 4min, then black precipitate material is placed in vacuum drying chamber and dried to constant weight, drying temperature is 50 DEG C, is dried
Time is 8h, that is, obtains cobalt nano magnetic material.
Embodiment 3
A kind of preparation method of cobalt nano magnetic material, comprises the following steps：
(1) NaOH and ethylene glycol are weighed respectively, are prepared 20mL concentration and are 15mol/L NaOH ethylene glycol solutions, and cool down
To room temperature；
(2) CoCl is weighed respectively2·6H2O and glycerine, prepare the CoCl that 10mL concentration is 0.05mol/L2Glycerine is molten
Liquid；
(3) CoCl of 1mL steps 2 preparation is pipetted with pipette2Glycerin solution, it is slowly dropped into what is prepared in step 1
In NaOH ethylene glycol solutions, it is stirred continuously to being uniformly dispersed, obtains blue-tinted transparent solution；
(4) under same mixing speed, 95wt% aqueous povidone solutions and 35wt% hydrations are added dropwise successively
The volume ratio of hydrazine, aqueous povidone solution and hydrazine hydrate is 1:1, obtain blue mixed solution；
(5) the blue mixed solution obtained in step 4 is transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, tightened anti-
Kettle is answered, and repeated multiple times concussion is shaken, and then reactor is put into vacuum drying chamber, sets reaction temperature as 120 DEG C, is reacted
Time is 5h；
(6) after the completion of reacting, treat that vacuum drying chamber is cooled to room temperature, take out autoclave, obtain colourless transparent solution and black
Color precipitates；
(7) centrifuge, by the black precipitate in reaction product successively with absolute ethyl alcohol and deionized water supersound washing 3~5 times,
Each ultrasonic 5min, then black precipitate material is placed in vacuum drying chamber and dried to constant weight, drying temperature is 60 DEG C, is dried
Time is 6h, that is, obtains cobalt nano magnetic material.
Claims (5)
1. a kind of preparation method of cobalt nano magnetic material, it is characterised in that comprise the following steps：
(1) NaOH and ethylene glycol are weighed respectively, are prepared 20mL concentration and are 10~15mol/L NaOH ethylene glycol solutions, and cool down
To room temperature；
(2) CoCl is weighed respectively2·6H2O and glycerine, prepare the CoCl that 10mL concentration is 0.05~0.15mol/L2Glycerine
Solution；
(3) CoCl of 1mL steps 2 preparation is pipetted with pipette2Glycerin solution, it is slowly dropped into the NaOH second two prepared in step 1
In alcoholic solution, it is stirred continuously to being uniformly dispersed, obtains blue-tinted transparent solution；
(4) under same mixing speed, 95wt% aqueous povidone solutions and 35wt% hydrazine hydrates is added dropwise successively, obtains
To blue mixed solution；
(5) the blue mixed solution obtained in step 4 is transferred in polytetrafluoroethyllining lining hydrothermal reaction kettle, tightens reaction
Kettle, and repeated multiple times concussion is shaken up, and then reactor is put into vacuum drying chamber, sets reaction temperature as 120~200 DEG C,
Reaction time is 2~5h；
(6) after the completion of reacting, treat that vacuum drying chamber is cooled to room temperature, take out autoclave, obtain colourless transparent solution and black sinks
Form sediment；
(7) centrifuge, the black precipitate in reaction product is washed 3~5 times with absolute ethyl alcohol and deionized water successively, then will be black
Color deposit is placed in vacuum drying chamber and dried to constant weight, that is, obtains cobalt nano magnetic material.
A kind of 2. preparation method of cobalt nano magnetic material according to claim 1, it is characterised in that described step 4
In aqueous povidone solution and hydrazine hydrate volume ratio be 1:1~2:5.
A kind of 3. preparation method of cobalt nano magnetic material according to claim 1 or 2, it is characterised in that described step
Reaction temperature in rapid 5 is 180 DEG C, reaction time 2h.
A kind of 4. preparation method of cobalt nano magnetic material according to claim 1 or 2, it is characterised in that described step
Mode of washing uses supersound washing in rapid 7, and ultrasonic time is 3~5min.
A kind of 5. preparation method of cobalt nano magnetic material according to claim 1 or 2, it is characterised in that described step
Drying temperature in rapid 7 is 50~60 DEG C, and drying time is 6~8h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108380899A (en) * | 2018-04-04 | 2018-08-10 | 陕西理工大学 | A kind of preparation method of cobalt nano magnetic material |
| CN111790288A (en) * | 2020-07-21 | 2020-10-20 | 金华职业技术学院 | Preparation method and equipment of magnetic nano composite material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1973003A (en) * | 1929-07-12 | 1934-09-11 | Gen Aniline Works Inc | Dehalogenation of cyclic halogen compounds |
| CN1261565A (en) * | 1999-01-21 | 2000-08-02 | 中国科学技术大学 | Method for preparing nanometre metal cobalt powder or nickel powder |
-
2017
- 2017-09-30 CN CN201710917496.2A patent/CN107680768A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1973003A (en) * | 1929-07-12 | 1934-09-11 | Gen Aniline Works Inc | Dehalogenation of cyclic halogen compounds |
| CN1261565A (en) * | 1999-01-21 | 2000-08-02 | 中国科学技术大学 | Method for preparing nanometre metal cobalt powder or nickel powder |
Non-Patent Citations (1)
| Title |
|---|
| 胡文斌: "钴纳米磁性材料的合成及性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108380899A (en) * | 2018-04-04 | 2018-08-10 | 陕西理工大学 | A kind of preparation method of cobalt nano magnetic material |
| CN111790288A (en) * | 2020-07-21 | 2020-10-20 | 金华职业技术学院 | Preparation method and equipment of magnetic nano composite material |
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Application publication date: 20180209 |