CN113184916B - Ferroferric oxide magnetic powder and preparation method thereof - Google Patents
Ferroferric oxide magnetic powder and preparation method thereof Download PDFInfo
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- CN113184916B CN113184916B CN202110598190.1A CN202110598190A CN113184916B CN 113184916 B CN113184916 B CN 113184916B CN 202110598190 A CN202110598190 A CN 202110598190A CN 113184916 B CN113184916 B CN 113184916B
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- alkaline precipitant
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- ferroferric oxide
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000006247 magnetic powder Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 239000002244 precipitate Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 81
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 238000005086 pumping Methods 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 230000002572 peristaltic effect Effects 0.000 description 9
- 239000012153 distilled water Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- 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
- C01P2006/42—Magnetic properties
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a preparation method of ferroferric oxide magnetic powder, which comprises the following steps: (1) Adding water and an alkaline precipitant into a reaction vessel, and adjusting the pH value; (2) continuously charging inert gas into the reaction vessel; (3) Under the condition of continuous stirring and specific reaction temperature, the mixture is introduced into a reaction containerAdding Fe at a certain flow rate 2+ Solution and Fe 3+ Adding an alkaline precipitant into the solution at the same time according to a certain flow rate, and stabilizing the pH value to be equal to the pH value in the step (1); (4) Stopping the addition of Fe 2+ Solution and Fe 3+ Continuously adding an alkaline precipitant into the solution, stabilizing the pH value to be equal to the pH value in the step (1), and stopping adding the alkaline precipitant after the precipitate is not increased any more; (5) removing the supernatant and washing the precipitate; and (6) filtering and drying to obtain the product. The ferroferric oxide magnetic powder prepared by the preparation method has better uniformity and fluidity, and has better definition when being applied to magnetic mark detection.
Description
Technical Field
The invention belongs to the technical field of magnetic material preparation, and particularly relates to ferroferric oxide magnetic powder and a preparation method thereof.
Background
Ferroferric oxide is an important non-destructive inspection magnetic powder material, and has attracted great attention in recent years due to its unique electromagnetic properties. It is well known that magnetic powder material properties are related to the morphology of the material, in particular to the crystal growth and size of the material. The nano ferroferric oxide has the characteristics of good magnetic properties, easiness in preparing composite materials and the like, and can be used as a magnetic powder material and has good application prospect in the aspects of magnetic mark detection of aviation, ships and the like, but the ferroferric oxide prepared by the existing preparation method is not uniform in granularity, and meanwhile, has poor fluidity, so that the definition is poor when the ferroferric oxide is applied to magnetic mark detection.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides the ferroferric oxide magnetic powder and the preparation method thereof, and the ferroferric oxide magnetic powder prepared by the preparation method has better uniformity and fluidity, and has better definition when being applied to magnetic mark detection.
The technical aim of the invention is realized by the following technical scheme:
a preparation method of ferroferric oxide magnetic powder comprises the following steps:
(1) Adding water and alkaline precipitant into the reaction vessel, and regulating pH value
(2) Continuously filling inert gas into the reaction vessel;
(3) Under the condition of continuous stirring and specific reaction temperature, adding Fe into a reaction container at a certain flow rate 2+ Solution and Fe 3+ Adding an alkaline precipitant into the solution at the same time according to a certain flow rate, and stabilizing the pH value to be equal to the pH value in the step (1);
(4) Stopping the addition of Fe 2+ Solution and Fe 3+ Continuously adding an alkaline precipitant into the solution, stabilizing the pH value to be equal to the pH value in the step (1), and stopping adding the alkaline precipitant after the precipitate is not increased any more;
(5) Removing supernatant fluid, and washing precipitate;
(6) Filtering, and drying.
Preferably, the pH value in the step (1) is 9-11.
Preferably, the alkaline precipitant is a NaOH solution or an aqueous ammonia solution.
Preferably, the alkaline precipitant is a NaOH solution, and the concentration of the NaOH solution is 0.8-1.2mol/l.
Preferably, the reaction temperature in step (3) is 55-65 ℃.
Preferably, the Fe 2+ Fe in solution 2+ The concentration of Fe is 0.8-1.2mol/l 3+ Fe in solution 3+ The concentration of (2) is 0.8-1.2mol/l.
Preferably, the alkaline precipitant is mixed with a surfactant.
Preferably, the surfactant is sodium dodecyl sulfate.
Preferably, the Fe 2+ Solution and Fe 3+ The solution is filtered by an ion filter membrane with the aperture of 0.01-0.02 mu m and then enters a reaction container.
Another object of the present invention is to provide a ferroferric oxide magnetic powder:
a ferroferric oxide magnetic powder prepared by the preparation method.
The beneficial effects of the invention are as follows: the ferroferric oxide magnetic powder has better uniformity and fluidity, and has better definition when being applied to nondestructive detection.
Detailed Description
The invention will be further illustrated with reference to specific examples.
Example 1:
a preparation method of ferroferric oxide magnetic powder comprises the following steps:
(1) Preparing a solution: 100ml of NaOH solution with the concentration of 0.8mol/l and FeCl with the concentration of 0.8mol/l are respectively prepared 2 50ml of solution and FeCl with concentration of 0.8mol/l 3 50ml of a solution, wherein the NaOH solution is mixed with 0.3g/l of sodium dodecyl sulfate by mass fraction, and the NaOH solution and FeCl are mixed 2 Solution and FeCl 3 The solution was placed in a water bath at 55 ℃ through 3 conical flasks;
(2) Mounting and preparing a reaction vessel: a four-necked flask is adopted as a reaction vessel, a certain amount of distilled water with the temperature of 55 ℃ is firstly added into the four-necked flask, then a pH meter probe and a nitrogen gas inlet rubber tube are arranged on the four-necked flask, and NaOH solution and FeCl are respectively filled into the four-necked flask through 3 peristaltic pumps and a plurality of rubber tubes 2 Solution and FeCl 3 The conical flask of the solution was connected to a four-necked flask, in which FeCl was attached 2 Solution and FeCl 3 An ion filter membrane fiber pipe with the aperture of 0.01 mu m is arranged at the tail end of a rubber pipe of the solution, naOH solution is pumped into the rubber pipe through a peristaltic pump for the first time, the pH value is regulated to 9, then a stirrer is assembled, and a stirring rod needs to extend below the liquid level;
(3) Continuously filling nitrogen into the reaction vessel;
(4) FeCl is pumped in by peristaltic pump under continuous stirring 2 Solution, feCl 3 Solution and NaOH solution, keeping pH value at 9, wherein FeCl 2 Solution and FeCl 3 The pumping speed of the solution is 2ml/min;
(5) After a period of time, the FeCl pumping is stopped 2 Solution and FeCl 3 Continuously pumping NaOH solution, keeping the pH value at 9, and stopping pumping the NaOH solution after the precipitate is not increased any more;
(6) Removing supernatant, washing the precipitate with distilled water, and washing with absolute ethyl alcohol;
(7) Filtering, and drying.
The ferroferric oxide magnetic powder is prepared by the preparation method.
The magnetization intensity of the prepared ferroferric oxide magnetic powder is 68.6emu/g, the flow property reaches 16.3s/50g, and better definition can be obtained when the ferroferric oxide magnetic powder is used for preparing 5% concentration magnetic suspension for magnetic mark detection.
Example 2:
a preparation method of ferroferric oxide magnetic powder comprises the following steps:
(1) Preparing a solution: 100ml of NaOH solution with the concentration of 1.0mol/l and FeCl with the concentration of 1.0mol/l are respectively prepared 2 50ml of solution, feCl with concentration of 1.0mol/l 3 50ml of a solution, wherein the NaOH solution is mixed with 0.3g/l of sodium dodecyl sulfate by mass fraction, and the NaOH solution and FeCl are mixed 2 Solution and FeCl 3 The solution was placed in a water bath at 60 ℃ through 3 conical flasks;
(2) Mounting and preparing a reaction vessel: a four-necked flask is adopted as a reaction vessel, a certain amount of distilled water with the temperature of 60 ℃ is firstly added into the four-necked flask, then a pH meter probe and a nitrogen gas inlet rubber tube are arranged on the four-necked flask, and NaOH solution and FeCl are respectively filled into the four-necked flask through 3 peristaltic pumps and a plurality of rubber tubes 2 Solution and FeCl 3 The conical flask of the solution was connected to a four-necked flask, in which FeCl was attached 2 Solution and FeCl 3 An ion filter membrane fiber pipe with the aperture of 0.015 mu m is arranged at the tail end of a rubber pipe of the solution, naOH solution is pumped into the rubber pipe through a peristaltic pump for the first time, the pH value is regulated to 10, then a stirrer is assembled, and a stirring rod needs to extend below the liquid level;
(3) Continuously filling nitrogen into the reaction vessel;
(4) FeCl is pumped in by peristaltic pump under continuous stirring 2 Solution, feCl 3 Solution and NaOH solution, keeping pH value at 10, wherein FeCl 2 Solution and FeCl 3 The pumping speed of the solution is 2ml/min;
(5) After a period of time, the FeCl pumping is stopped 2 Solution and FeCl 3 Continuously pumping NaOH solution, keeping the pH value at 10, and stopping pumping the NaOH solution after the precipitate is not increased any more;
(6) Removing supernatant, washing the precipitate with distilled water, and washing with absolute ethyl alcohol;
(7) Filtering, and drying.
The ferroferric oxide magnetic powder is prepared by the preparation method.
The magnetization intensity of the prepared ferroferric oxide magnetic powder is 73.5emu/g, the flow property reaches 22.8s/50g, and better definition can be obtained when the ferroferric oxide magnetic powder is used for preparing 5% concentration magnetic suspension for magnetic mark detection.
Example 3:
a preparation method of ferroferric oxide magnetic powder comprises the following steps:
(1) Preparing a solution: 100ml of NaOH solution with the concentration of 1.2mol/l and FeCl with the concentration of 1.2mol/l are respectively prepared 2 50ml of solution, feCl with concentration of 1.2mol/l 3 50ml of a solution, wherein the NaOH solution is mixed with 0.3g/l of sodium dodecyl sulfate by mass fraction, and the NaOH solution and FeCl are mixed 2 Solution and FeCl 3 The solution was placed in a water bath at 65 ℃ through 3 conical flasks;
(2) Mounting and preparing a reaction vessel: a four-necked flask is adopted as a reaction vessel, a certain amount of distilled water with the temperature of 65 ℃ is firstly added into the four-necked flask, then a pH meter probe and a nitrogen gas inlet rubber tube are arranged on the four-necked flask, and NaOH solution and FeCl are respectively filled into the four-necked flask through 3 peristaltic pumps and a plurality of rubber tubes 2 Solution and FeCl 3 The conical flask of the solution was connected to a four-necked flask, in which FeCl was attached 2 Solution and FeCl 3 An ion filter membrane fiber pipe with the aperture of 0.02 mu m is arranged at the tail end of a rubber pipe of the solution, naOH solution is pumped into the rubber pipe through a peristaltic pump for the first time, the pH value is regulated to 11, then a stirrer is assembled, and a stirring rod needs to extend below the liquid level;
(3) Continuously filling nitrogen into the reaction vessel;
(4) FeCl is pumped in by peristaltic pump under continuous stirring 2 Solution, feCl 3 Solution and NaOH solution, keeping pH value at 11, wherein FeCl 2 Solution and FeCl 3 The pumping speed of the solution is 2ml/min;
(5) After a period of time, the FeCl pumping is stopped 2 Solution and FeCl 3 Continuously pumping NaOH solution, keeping the pH value at 11, and stopping pumping the NaOH solution after the precipitate is not increased any more;
(6) Removing supernatant, washing the precipitate with distilled water, and washing with absolute ethyl alcohol;
(7) Filtering, and drying.
The ferroferric oxide magnetic powder is prepared by the preparation method.
The magnetization intensity of the prepared ferroferric oxide magnetic powder is 69.2emu/g, the flow property reaches 18.7s/50g, and better definition can be obtained when the ferroferric oxide magnetic powder is used for preparing 5% concentration magnetic suspension for magnetic mark detection.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (1)
1. The preparation method of the ferroferric oxide magnetic powder is characterized by comprising the following steps:
(1) Adding water and an alkaline precipitant into a reaction vessel, and adjusting the pH value;
(2) Continuously filling inert gas into the reaction vessel;
(3) Under the condition of continuous stirring and specific reaction temperature, adding Fe into a reaction container at a certain flow rate 2+ Solution and Fe 3+ Adding an alkaline precipitant into the solution at the same time according to a certain flow rate, and stabilizing the pH value to be equal to the pH value in the step (1);
(4) Stopping the addition of Fe 2+ Solution and Fe 3+ Continuously adding an alkaline precipitant into the solution, stabilizing the pH value to be equal to the pH value in the step (1), and stopping adding the alkaline precipitant after the precipitate is not increased any more;
(5) Removing supernatant fluid, and washing precipitate;
(6) Filtering, and drying to obtain the final product;
the pH value in the step (1) is 9-11; the alkaline precipitant is NaOH solution, and the concentration of the NaOH solution is 0.8-1.2mol/l; the reaction temperature in the step (3) is 55-65 ℃;the Fe is 2+ Fe in solution 2+ The concentration of Fe is 0.8-1.2mol/l 3+ Fe in solution 3+ The concentration of (2) is 0.8-1.2mol/l; the alkaline precipitant is mixed with a surfactant; the surfactant is sodium dodecyl sulfate; the Fe is 2+ Solution and Fe 3+ The solution is filtered by an ion filter membrane with the aperture of 0.01-0.02 mu m and then enters a reaction container.
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| CN113184916B true CN113184916B (en) | 2023-05-23 |
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| CN104229901B (en) * | 2014-10-11 | 2016-05-11 | 中南林业科技大学 | A kind of preparation method of magnetic ferroferric oxide nano-particles |
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