CN105562704A - Method for preparing cobalt nanometer magnetic material through hydrothermal synthesis method - Google Patents
Method for preparing cobalt nanometer magnetic material through hydrothermal synthesis method Download PDFInfo
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- CN105562704A CN105562704A CN201410547024.9A CN201410547024A CN105562704A CN 105562704 A CN105562704 A CN 105562704A CN 201410547024 A CN201410547024 A CN 201410547024A CN 105562704 A CN105562704 A CN 105562704A
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Abstract
The invention discloses a method for preparing a cobalt nanometer magnetic material through a hydrothermal synthesis method. The method for preparing the cobalt nanometer magnetic material through the hydrothermal synthesis method includes the steps that firstly, a NaOH solution and a CoC12 solution with the concentration of 0.05-0.15 mol/L are prepared; the CoC12 solution is slowly dripped into the NaOH solution, the mixture is stirred continuously till the CoC12 solution is evenly dispersed, and a blue transparent solution is obtained; ethidene diamine and hydrazine hydrate are dripped in sequence, and a blue mixed solution is obtained; the mixed solution is transferred into a polytetrafluoroethylene container and put into a vacuum drying box to be heated to generate a reaction; after the reaction is completed, the mixed solution is cooled to the room temperature, and a colorless and transparent solution and black precipitates are obtained; and finally, a centrifugal separator is used for separating the black precipitates in the reaction product, washing is conducted, the black precipitate matter is dried in the vacuum drying box, and the cobalt nanometer magnetic material is obtained. The method for preparing the cobalt nanometer magnetic material through the hydrothermal synthesis method solves the problems that the requirement for powder performance cannot be met in the prior art, and products are uneven in particle diameter and large in particle size.
Description
Technical field
The invention belongs to magnetic Nano material technical field, relate to a kind of method that hydrothermal synthesis method prepares cobalt nano magnetic material.
Background technology
Cobalt nano magnetic material has special physics, chemical property and magnetic property, and its Application comparison is extensive, has had a lot of research both at home and abroad to metallic cobalt nano magnetic material.At present, the method much preparing cobalt nano magnetic material is had both at home and abroad.As oxide, oxalates hydrogen reduction method, oxalates thermal decomposition method, high-pressure water spray method, electrolysis, polyol process, hydrazine hydrate liquid phase reduction etc.Wherein some method realizes industrialization, and some is also in laboratory exploration and conceptual phase.Along with the developing of cobalt nano magnetic material application, present existing technique can not meet the requirement of powder property, and the particle diameter that there is product is uneven, the problem that particle diameter is larger.
Summary of the invention
The object of this invention is to provide a kind of method that hydrothermal synthesis method prepares cobalt nano magnetic material, solve the requirement that existing technique can not meet powder property, and the particle diameter that there is product is uneven, the problem that particle diameter is larger.
The technical solution adopted in the present invention is, a kind of hydrothermal synthesis method prepares the method for cobalt nano magnetic material, specifically implements according to following steps:
Step 1, preparation NaOH solution, is that 1:1 ~ 2 take NaOH and distilled water according to mass ratio, is then mixed with distilled water by NaOH, and be cooled to room temperature;
Step 2, compound concentration is the CoCl of 0.05 ~ 0.15mol/L
2solution;
Step 3, by the CoCl in step 2
2solution slowly drips in NaOH solution obtained in progressive rapid 1, and is constantly stirred to and is uniformly dispersed, and obtains blue-tinted transparent solution;
Step 4, under same mixing speed, instills ethylenediamine and hydrazine hydrate successively, obtains blue mixed solution;
Step 5, transfers in polytetrafluoroethylcontainer container by the mixed solution obtained in step 4, container is put into autoclave, and repeated multiple times concussion is shaken all, then autoclave is put into vacuum drying chamber and adds thermal response;
Step 6, after having reacted, is cooled to room temperature, takes out autoclave, obtains colourless transparent solution and black precipitate;
Step 7, uses whizzer the black precipitate in product to be separated, then uses absolute ethyl alcohol and deionized water cyclic washing 3 ~ 5 times, then black precipitate material is carried out drying in vacuum drying chamber, namely obtain as cobalt nano magnetic material.
Feature of the present invention is also,
Wherein, the mass concentration of the ethylenediamine in step 4 is 99%, and the mass concentration of hydrazine hydrate is 35%.
Wherein, the reaction temperature in step 5 is 100 ~ 180 DEG C, and the reaction time is 3 ~ 7h.
Wherein, the baking temperature in step 7 is 45 ~ 60 DEG C, and drying time is 3 ~ 5 hours.
The invention has the beneficial effects as follows, utilize hydrothermal synthesis method to select hydrazine hydrate as reducing agent, and use ethylenediamine as complexant, prepare uniform particle sizes, good dispersion and the cobalt nano magnetic material of function admirable.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
A kind of hydrothermal synthesis method of the present invention prepares the method for cobalt nano magnetic material, specifically implements according to following steps:
Step 1, preparation NaOH solution, is that 1:1 ~ 2 take NaOH and distilled water according to mass ratio, is then mixed with distilled water by NaOH, and be cooled to room temperature;
Step 2, compound concentration is the CoCl of 0.05 ~ 0.15mol/L
2solution;
Step 3, by the CoCl in step 2
2solution slowly drips in NaOH solution obtained in progressive rapid 1, and is constantly stirred to and is uniformly dispersed, and obtains blue-tinted transparent solution;
Step 4, under same mixing speed, instills ethylenediamine (EDA, 99wt%) and mass concentration is 35wt% hydrazine hydrate (N successively
2h
4h
2o), blue mixed solution is obtained;
Step 5, transfers in polytetrafluoroethylcontainer container by above-mentioned blue solution, container is put into autoclave, and repeated multiple times concussion is shaken all, then autoclave is put into vacuum drying chamber and adds thermal response.Temperature 100 ~ 180 DEG C, the reaction time is 3 ~ 7h
Step 6, after having reacted, is cooled to room temperature, takes out autoclave, obtains colourless transparent solution and black precipitate;
Step 7, whizzer is used black precipitate to be isolated, use absolute ethyl alcohol and deionized water cyclic washing more respectively repeatedly, then by black precipitate material in vacuum drying chamber at 40 ~ 60 DEG C dry 3 ~ 5 hours, the atrament obtained is cobalt nano magnetic material.
In preparation method of the present invention, utilize hydrothermal synthesis method to select hydrazine hydrate as reducing agent, and use ethylenediamine as complexant, prepare uniform particle sizes, good dispersion and the cobalt nano magnetic material of function admirable.Molecule in the hydrazine hydrate wherein used is associated by strong hydrogen bonding, is widely used as reducing agent.Great advantage as reducing agent is that reducing power is strong in the basic conditions, and its oxidation product is N
2, foreign metal ion can not be introduced to product.
Embodiment 1
Hydrothermal synthesis method prepares a method for cobalt nano magnetic material, specifically implements according to following steps:
Step 1, preparation NaOH solution, is that 1:1 takes NaOH and distilled water according to mass ratio, is then mixed with distilled water by NaOH, and be cooled to room temperature;
Step 2, compound concentration is the CoCl of 0.05mol/L
2solution;
Step 3, by the CoCl in step 2
2solution slowly drips in NaOH solution obtained in progressive rapid 1, and is constantly stirred to and is uniformly dispersed, and obtains blue-tinted transparent solution;
Step 4, under same mixing speed, instills ethylenediamine (EDA, 99wt%) and mass concentration is 35wt% hydrazine hydrate (N successively
2h
4h
2o), blue mixed solution is obtained;
Step 5, transfers in polytetrafluoroethylcontainer container by above-mentioned blue solution, container is put into autoclave, and repeated multiple times concussion is shaken all, then autoclave is put into vacuum drying chamber and adds thermal response.Temperature 100 DEG C, the reaction time is 3h
Step 6, after having reacted, is cooled to room temperature, takes out autoclave, obtains colourless transparent solution and black precipitate;
Step 7, uses whizzer black precipitate to be isolated, then uses absolute ethyl alcohol and deionized water cyclic washing respectively repeatedly, and then by black precipitate material in vacuum drying chamber at 40 DEG C dry 3 hours, the atrament obtained is cobalt nano magnetic material.
Embodiment 2
Hydrothermal synthesis method prepares a method for cobalt nano magnetic material, specifically implements according to following steps:
Step 1, preparation NaOH solution, is that 1:2 takes NaOH and distilled water according to mass ratio, is then mixed with distilled water by NaOH, and be cooled to room temperature;
Step 2, compound concentration is the CoCl of 0.15mol/L
2solution;
Step 3, by the CoCl in step 2
2solution slowly drips in NaOH solution obtained in progressive rapid 1, and is constantly stirred to and is uniformly dispersed, and obtains blue-tinted transparent solution;
Step 4, under same mixing speed, instills ethylenediamine (EDA, 99wt%) and mass concentration is 35wt% hydrazine hydrate (N successively
2h
4h
2o), blue mixed solution is obtained;
Step 5, transfers in polytetrafluoroethylcontainer container by above-mentioned blue solution, container is put into autoclave, and repeated multiple times concussion is shaken all, then autoclave is put into vacuum drying chamber and adds thermal response.Temperature 180 DEG C, the reaction time is 7h
Step 6, after having reacted, is cooled to room temperature, takes out autoclave, obtains colourless transparent solution and black precipitate;
Step 7, uses whizzer black precipitate to be isolated, then uses absolute ethyl alcohol and deionized water cyclic washing respectively repeatedly, and then by black precipitate material in vacuum drying chamber at 60 DEG C dry 5 hours, the atrament obtained is cobalt nano magnetic material.
Embodiment 3
Hydrothermal synthesis method prepares a method for cobalt nano magnetic material, specifically implements according to following steps:
Step 1, preparation NaOH solution, is that 1:1.5 takes NaOH and distilled water according to mass ratio, is then mixed with distilled water by NaOH, and be cooled to room temperature;
Step 2, compound concentration is the CoCl of 0.1mol/L
2solution;
Step 3, by the CoCl in step 2
2solution slowly drips in NaOH solution obtained in progressive rapid 1, and is constantly stirred to and is uniformly dispersed, and obtains blue-tinted transparent solution;
Step 4, under same mixing speed, instills ethylenediamine (EDA, 99wt%) and mass concentration is 35wt% hydrazine hydrate (N successively
2h
4h
2o), blue mixed solution is obtained;
Step 5, transfers in polytetrafluoroethylcontainer container by above-mentioned blue solution, container is put into autoclave, and repeated multiple times concussion is shaken all, then autoclave is put into vacuum drying chamber and adds thermal response.Temperature 150 DEG C, the reaction time is 5h
Step 6, after having reacted, is cooled to room temperature, takes out autoclave, obtains colourless transparent solution and black precipitate;
Step 7, uses whizzer black precipitate to be isolated, then uses absolute ethyl alcohol and deionized water cyclic washing respectively repeatedly, and then by black precipitate material in vacuum drying chamber at 50 DEG C dry 4 hours, the atrament obtained is cobalt nano magnetic material.
Claims (4)
1. hydrothermal synthesis method prepares a method for cobalt nano magnetic material, it is characterized in that, specifically implements according to following steps:
Step 1, preparation NaOH solution, is that 1:1 ~ 2 take NaOH and distilled water according to mass ratio, is then mixed with distilled water by NaOH, and be cooled to room temperature;
Step 2, compound concentration is the CoCl of 0.05 ~ 0.15mol/L
2solution;
Step 3, by the CoCl in step 2
2solution slowly drips in NaOH solution obtained in progressive rapid 1, and is constantly stirred to and is uniformly dispersed, and obtains blue-tinted transparent solution;
Step 4, under same mixing speed, instills ethylenediamine and hydrazine hydrate successively, obtains blue mixed solution;
Step 5, transfers in polytetrafluoroethylcontainer container by the mixed solution obtained in step 4, container is put into autoclave, and repeated multiple times concussion is shaken all, then autoclave is put into vacuum drying chamber and adds thermal response.
Step 6, after having reacted, is cooled to room temperature, takes out autoclave, obtains colourless transparent solution and black precipitate;
Step 7, uses whizzer the black precipitate in product to be separated, then uses absolute ethyl alcohol and deionized water cyclic washing 3 ~ 5 times, then black precipitate material is carried out drying in vacuum drying chamber, namely obtain as cobalt nano magnetic material.
2. a kind of hydrothermal synthesis method according to claim 1 prepares the method for cobalt nano magnetic material, it is characterized in that, the mass concentration of the ethylenediamine in described step 4 is 99%, and the mass concentration of hydrazine hydrate is 35%.
3. a kind of hydrothermal synthesis method according to claim 1 prepares the method for cobalt nano magnetic material, it is characterized in that, the reaction temperature in described step 5 is 100 ~ 180 DEG C, and the reaction time is 3 ~ 7h.
4. a kind of hydrothermal synthesis method according to claim 1 prepares the method for cobalt nano magnetic material, it is characterized in that, the baking temperature in described step 7 is 45 ~ 60 DEG C, and drying time is 3 ~ 5 hours.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106493354A (en) * | 2016-10-24 | 2017-03-15 | 兰州大学 | The preparation method of the composite nano powder of oxide coated by zinc magnetic metal nano particle |
| CN108169978A (en) * | 2018-01-03 | 2018-06-15 | 京东方科技集团股份有限公司 | Electronic Paper and preparation method thereof, hand-written electric paper device |
| CN108380899A (en) * | 2018-04-04 | 2018-08-10 | 陕西理工大学 | A kind of preparation method of cobalt nano magnetic material |
| CN108746656A (en) * | 2018-06-15 | 2018-11-06 | 威海职业学院 | Prealloy powder and preparation method thereof for diamond composition |
| CN113059179A (en) * | 2021-03-17 | 2021-07-02 | 电子科技大学 | Preparation method of magnetic cobalt particles |
| CN115555575A (en) * | 2022-09-21 | 2023-01-03 | 安徽格派锂电循环科技有限公司 | Method for preparing nano cobalt particles by utilizing thermal spraying method |
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2014
- 2014-10-15 CN CN201410547024.9A patent/CN105562704A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106493354A (en) * | 2016-10-24 | 2017-03-15 | 兰州大学 | The preparation method of the composite nano powder of oxide coated by zinc magnetic metal nano particle |
| CN106493354B (en) * | 2016-10-24 | 2018-11-16 | 兰州大学 | The preparation method of the composite nano powder of oxide coated by zinc magnetic metal nano particle |
| CN108169978A (en) * | 2018-01-03 | 2018-06-15 | 京东方科技集团股份有限公司 | Electronic Paper and preparation method thereof, hand-written electric paper device |
| CN108169978B (en) * | 2018-01-03 | 2021-08-17 | 京东方科技集团股份有限公司 | Electronic paper, preparation method thereof and handwriting electronic paper device |
| CN108380899A (en) * | 2018-04-04 | 2018-08-10 | 陕西理工大学 | A kind of preparation method of cobalt nano magnetic material |
| CN108746656A (en) * | 2018-06-15 | 2018-11-06 | 威海职业学院 | Prealloy powder and preparation method thereof for diamond composition |
| CN108746656B (en) * | 2018-06-15 | 2021-11-26 | 威海职业学院 | Pre-alloyed powder for diamond products and preparation method thereof |
| CN113059179A (en) * | 2021-03-17 | 2021-07-02 | 电子科技大学 | Preparation method of magnetic cobalt particles |
| CN113059179B (en) * | 2021-03-17 | 2022-06-03 | 电子科技大学 | Preparation method of magnetic cobalt particles |
| CN115555575A (en) * | 2022-09-21 | 2023-01-03 | 安徽格派锂电循环科技有限公司 | Method for preparing nano cobalt particles by utilizing thermal spraying method |
| CN115555575B (en) * | 2022-09-21 | 2024-03-29 | 安徽格派锂电循环科技有限公司 | Method for preparing nano cobalt particles by using thermal spraying method |
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Application publication date: 20160511 |