CN102765761B - Method for preparing ferroferric oxide at room temperature - Google Patents
Method for preparing ferroferric oxide at room temperature Download PDFInfo
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- CN102765761B CN102765761B CN201210227631.8A CN201210227631A CN102765761B CN 102765761 B CN102765761 B CN 102765761B CN 201210227631 A CN201210227631 A CN 201210227631A CN 102765761 B CN102765761 B CN 102765761B
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- room temperature
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- deionized water
- ferroferric oxide
- ferrous
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Abstract
The invention comprises a method for preparing ferroferric oxide at room temperature and belongs to the technical field of chemical industry. The method comprises the steps of: 1, preparing a ferrous solution with mass concentration of 0.5-1% by ferrous salt; 2, adding strong reducing agent powder into the ferrous solution in the step 1, wherein the mass ratio of the strong reducing agent and the ferrous salt is 1:0.5 to 1:6; 3, cleaning black magnetic zero valent iron obtained with deionized water after reaction in the steps 1 and 2, immersing the zero valent iron at room temperature into the deionized water of a container for 24-36 hours, wherein the container is provided with an air layer above and the container is sealed; and 4, obtaining stable ferroferric oxide after 24-36 hours, ultrasonically cleaning the ferroferric oxide with deionized water and ethanol for three times, wherein each time last for 2-3 minutes. The method for preparing ferroferric oxide provided by the invention is low in preparation cost and energy consumption, small in environmental pollution, simple to operate, easy to control processes, short in preparation period, and is convenient for production in a large scale.
Description
Technical field
The invention belongs to chemical technology field, is a kind of preparation method of Fe 3 O 4 magnetic powder.Be specifically related to a kind of room temperature and prepare the method for Z 250.
Background technology
Z 250, another name iron oxide black, magnet, magnetite, magnet, natural mineral type is magnetite.For the magnetic black crystals of tool, therefore be called again martial ethiops, there is good electroconductibility.Be dissolved in acid, the organic solvent such as water insoluble, alkali and ethanol, ether.Z 250 is a kind of conventional magneticsubstance, is typically used as pigment and rumbling compound, also can be used for manufacturing the starting material of mrt and telecommunication apparatus.
The preparation method of magnetic nanometer particles mainly contains physical method and chemical process.Physical method is prepared nanoparticle and is generally adopted vacuum condensation method, physical pulverization method, mechanical ball milling method etc.But the sample common product purity of preparing with physical method is low, size distribution is inhomogeneous,
The particle run-of-the-mill of the nanoparticle that employing chemical process obtains is better, and working method is also comparatively easy, and production cost is also lower, is the main method adopting in current research, production.
The chemical preparation process of Z 250, comprises comparison coprecipitation method, sol-gel method, microemulsion method, hydrolysis method, hydrothermal method etc.Aforesaid method all must be through reaction or heat treated under high temperature, and energy consumption is larger, method complexity.
Summary of the invention
The object of the present invention is to provide a kind of simple to operate, production cost is low, be convenient to scale operation, prepare the method for Z 250 under the room temperature condition of energy-conserving and environment-protective.
The present invention includes the following step:
(1) the ferrous iron solution that is 0.5%-1% by divalent iron salt configuration quality concentration;
(2) strong reductant powder is joined in the ferrous iron solution of step (1), the mass ratio of strong reductant and divalent iron salt is 1:0.5 to 1:6;
(3) after the reacting completely of step ((1)) and ((2)), by the black magnetic fe washed with de-ionized water obtaining, at room temperature evenly be immersed to 24--36 hour in the deionized water that is loaded on container, gas cloud sealed vessel are left in container top.
(4) after 24--36 hour, obtain the Z 250 of stable existence, with deionized water and ethanol ultrasonic cleaning three times, carry out 2-3 minutes at every turn.
The described strong reductant powder of step (2) is the strong reducing substance of sodium borohydride class.
The described ferrous iron of step (2) is the one in iron protochloride, Iron nitrate and ferrous sulfate.
Process in the ferrous iron solution that strong reductant powder is joined to step (1) described in step (2) is carried out under 150W power ultrasonic condition.
The present invention adopts fe is evenly immersed in to the mode in deionized water in last preparation process, makes fe and deionized water and trace oxygen carry out chemical reaction:
2Fe+O
2+2H
2O→2Fe(OH)
2 (1)
4Fe(OH)
2+O
2+2H
2O→4Fe(OH)
3 (2)
Under air-proof condition, in container, the not enough so that reaction (2) of oxygen is fully carried out, and then: result Fe (OH)
2and Fe (OH)
3dehydration reaction generates Fe simultaneously
3o
4:
Fe(OH)
2+2Fe(OH)
3→Fe
3O
4+4H
2O (3)
The diffraction peak of all X-ray diffraction spectrums of ferroferric oxide powder prepared by the present invention can be according to JCPDS card No.19-0629, corresponding to the Fe of face-centred cubic structure
3o
4ferrite standard spectrum.
The present invention compared with prior art tool has the following advantages:
1, it is synthetic under room temperature condition that method of the present invention is prepared Z 250, and reactant is at room temperature carried out to reduction reaction, has overcome the last handling process of complexity in chemosynthesis, and has needed the problems such as high temperature power consumption.
2, in preparation method of the present invention, adopt raw material simple, and be all primary chemical raw material, thereby preparation cost is low, environmental pollution is little.
3, simple to operate, technique is easy to control, and preparation cycle is short, is convenient to carry out scale operation.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of the Z 250 for preparing according to present method
Wherein: ordinate zou represents the intensity at X-ray diffraction peak; X-coordinate represents X-ray diffraction spectrometer scanning angle.
Embodiment
Embodiment 1
A kind of room temperature is prepared the method for ferroferric oxide powder: 0.15g ferrous sulfate is dissolved in 15mL deionized water, obtains mass concentration and be 1% ferrous salt solution.Under 150W power ultrasonic condition, add 0.025g SODIUM BOROHYDRIDE POWDER.After question response completes, with washed with de-ionized water black magnetic powder several, be placed in 100mL beaker, add 30mL deionized water, sealed vessel; After 24 hours, use deionized water and ethanol ultrasonic cleaning three times, carry out 2-3 minutes at every turn, obtain black magnetic powder.X-ray diffraction is accredited as pure phase Fe
3o
4.
Embodiment 2
A kind of room temperature is prepared the method for ferroferric oxide powder: 0.15g Iron nitrate salt is dissolved in 30mL deionized water, obtains mass concentration and be 0.5% ferrous salt solution.Under 150W power ultrasonic condition, add 0.075g SODIUM BOROHYDRIDE POWDER.After question response completes, with washed with de-ionized water black magnetic powder several, be placed in 100mL beaker, add 30mL deionized water, sealed vessel; After 36 hours, use deionized water and ethanol ultrasonic cleaning three times, carry out 2-3 minutes at every turn, obtain black magnetic powder.X-ray diffraction is accredited as pure phase Fe
3o
4.
Claims (3)
1. a method of preparing Z 250 under room temperature condition, is characterized in that comprising the following steps:
(1) the ferrous iron solution that is 0.5%-1% by divalent iron salt configuration quality concentration;
(2) strong reductant powder is joined in the ferrous iron solution of step (1), the mass ratio of strong reductant and divalent iron salt is 1:0.5 to 1:6, and described strong reductant powder is the strong reducing substance of sodium borohydride;
(3) after the reacting completely of step (1) and (2), by the black magnetic fe washed with de-ionized water obtaining, at room temperature evenly be immersed to 24--36 hour in the deionized water that is loaded on container, gas cloud sealed vessel are left in container top;
(4) after 24--36 hour, obtain the Z 250 of stable existence, with deionized water and ethanol ultrasonic cleaning three times, carry out 2-3 minutes at every turn.
2. by the method for preparing Z 250 under room temperature condition claimed in claim 1, it is characterized in that the described ferrous iron of step (2) is the one in iron protochloride, Iron nitrate and ferrous sulfate.
3. by the method for preparing Z 250 under room temperature condition claimed in claim 1, it is characterized in that the process in the described ferrous iron solution that strong reductant powder is joined to step (1) of step (2) is carried out under 150W power ultrasonic condition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210227631.8A CN102765761B (en) | 2012-07-03 | 2012-07-03 | Method for preparing ferroferric oxide at room temperature |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210227631.8A CN102765761B (en) | 2012-07-03 | 2012-07-03 | Method for preparing ferroferric oxide at room temperature |
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| Publication Number | Publication Date |
|---|---|
| CN102765761A CN102765761A (en) | 2012-11-07 |
| CN102765761B true CN102765761B (en) | 2014-05-21 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058283B (en) * | 2013-02-01 | 2014-07-02 | 济南大学 | Preparation method of iron oxides with adjustable size, appearance and compositions |
| CN104953113B (en) * | 2014-06-11 | 2016-06-15 | 佛山市南海新力电池有限公司 | A kind of manufacture method of battery carbon cladding nano ferriferrous oxide |
| CN107986337B (en) * | 2017-11-03 | 2020-05-05 | 浙江华源颜料股份有限公司 | Easily-dispersible high-tinting-strength iron oxide black and preparation method thereof |
| CN107694510B (en) * | 2017-11-14 | 2020-04-24 | 南昌大学 | Method for removing methylene blue in printing and dyeing wastewater by two-dimensional magnetic MXene |
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|---|---|---|---|---|
| JPS57175734A (en) * | 1981-04-21 | 1982-10-28 | Res Inst For Prod Dev | Preparation of ultrafine particle of fe3o4 |
| CN102259192B (en) * | 2011-07-27 | 2013-07-31 | 南京师范大学 | Method for preparing nanometer zero-valent iron based on liquid-phase complexation reduction method |
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2012
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