CN102765761A - Method for preparing ferroferric oxide at room temperature - Google Patents
Method for preparing ferroferric oxide at room temperature Download PDFInfo
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- CN102765761A CN102765761A CN2012102276318A CN201210227631A CN102765761A CN 102765761 A CN102765761 A CN 102765761A CN 2012102276318 A CN2012102276318 A CN 2012102276318A CN 201210227631 A CN201210227631 A CN 201210227631A CN 102765761 A CN102765761 A CN 102765761A
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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, be a kind of preparation method of Fe 3 O 4 magnetic powder.Be specifically related to a kind of method of room temperature preparation Z 250.
Background technology
Z 250, another name iron oxide black, magnet, magnetite, magnet, the natural mineral type is a magnetite.For having the black crystals of magnetic,, has good electroconductibility so be called martial ethiops again.Be dissolved in acid, organic solvent such as water insoluble, alkali and ethanol, ether.Z 250 is a kind of magneticsubstance commonly used, usually as pigment and rumbling compound, also can be used for making the starting material of mrt and telecommunication apparatus.
The preparation method of magnetic nanometer particles mainly contains physical method and chemical process.The nanoparticle for preparing physical method generally adopts vacuum condensation method, physical pulverization method, mechanical ball milling method etc.But the sample common product purity with the physical method preparation is low, size distribution is inhomogeneous,
The particle run-of-the-mill of the nanoparticle that the employing chemical process obtains is better, and working method is also more or less freely, and production cost is also lower, is the main method that adopts in present research, the production.
The chemical prepn process of Z 250 comprises comparison coprecipitation method, sol-gel method, microemulsion method, hydrolysis method, hydrothermal method etc.Aforesaid method all must react down or heat treated through high temperature, and energy consumption is bigger, and method is complicated.
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, the room temperature condition of energy-conserving and environment-protective prepares Z 250 down method.
The present invention includes the following step:
(1) use divalent iron salt configuration quality concentration is 0.5%-1% ferrous iron solution;
(2) the 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) treat the reacting completely of step ((1)) and ((2)) after, the black magnetic fe that obtains is used washed with de-ionized water, at room temperature evenly be immersed in the deionized water that is loaded on container 24--36 hour, gas cloud and sealed vessel are left in the container top.
(4) obtain the Z 250 of stable existence after 24--36 hour,, carried out 2-3 minutes at every turn with deionized water and ethanol ultrasonic cleaning three times.
The described strong reductant powder of step (2) is the strong reducing substance of Peng Qinghuana class.
The described ferrous iron of step (2) is a kind of in iron protochloride, Iron nitrate and the ferrous sulfate.
The process that step (2) is described to join the strong reductant powder in the ferrous iron solution of step (1) is carried out under 150W power ultrasonic condition.
The present invention adopts in last preparation process fe evenly is immersed in the mode in the deionized water, 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, the not enough so that reaction (2) of oxygen is fully carried out in the container, and then: Fe (OH) as a result
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 of the present invention's preparation can be according to JCPDS card No.19-0629, corresponding to the Fe of face-centred cubic structure
3O
4The ferrite standard spectrum.
The present invention compared with prior art has following advantage:
1, it is synthetic under the room temperature condition that method of the present invention prepares Z 250, and reactant is at room temperature carried out reduction reaction, has overcome last handling process complicated in the chemosynthesis, and needs problem such as high temperature power consumption.
2, adopt raw material simple among the preparation method of the present invention, and all be the primary chemical raw material, thereby preparation cost is low, environmental pollution is little.
3, simple to operate, technology is easy to control, and preparation cycle is short, is convenient to carry out scale operation.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the Z 250 for preparing according to present method
Wherein: ordinate zou is represented the intensity at X-ray diffraction peak; X-coordinate is represented X-ray diffraction spectrometer scanning angle.
Embodiment
Embodiment 1
A kind of method of room temperature preparation ferroferric oxide powder: the 0.15g ferrous sulfate is dissolved in the 15mL deionized water, obtains mass concentration and be 1% ferrous salt solution.Under 150W power ultrasonic condition, add 0.025g Peng Qinghuana powder.After question response is accomplished, with washed with de-ionized water black magnetic powder for several times, place the 100mL beaker, add the 30mL deionized water, sealed vessel; After 24 hours, use deionized water and ethanol ultrasonic cleaning three times, carried out 2-3 minutes at every turn, obtain the black magnetic powder.X-ray diffraction is accredited as pure phase Fe
3O
4
Embodiment 2
A kind of method of room temperature preparation ferroferric oxide powder: 0.15g Iron nitrate salt is dissolved in the 30mL deionized water, obtains mass concentration and be 0.5% ferrous salt solution.Under 150W power ultrasonic condition, add 0.075g Peng Qinghuana powder.After question response is accomplished, with washed with de-ionized water black magnetic powder for several times, place the 100mL beaker, add the 30mL deionized water, sealed vessel; After 36 hours, use deionized water and ethanol ultrasonic cleaning three times, carried out 2-3 minutes at every turn, obtain the black magnetic powder.X-ray diffraction is accredited as pure phase Fe
3O
4
Claims (4)
1. the following method for preparing Z 250 of room temperature condition is characterized in that comprising the following steps:
(1) use divalent iron salt configuration quality concentration is 0.5%-1% ferrous iron solution;
(2) the 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) treat the reacting completely of step (1) and (2) after, the black magnetic fe that obtains is used washed with de-ionized water, at room temperature evenly be immersed in the deionized water that is loaded on container 24--36 hour, gas cloud and sealed vessel are left in the container top;
(4) obtain the Z 250 of stable existence after 24--36 hour,, carried out 2-3 minutes at every turn with deionized water and ethanol ultrasonic cleaning three times.
2. by the method for preparing Z 250 under the described room temperature condition of claim 1, it is characterized in that the described strong reductant powder of step (2) is the strong reducing substance of Peng Qinghuana class.
3. the method for preparing down Z 250 by the described room temperature condition of claim 1 is characterized in that the described ferrous iron of step (2) is a kind of in iron protochloride, Iron nitrate and the ferrous sulfate.
4. the method for preparing down Z 250 by the described room temperature condition of claim 1 is characterized in that the process in the described ferrous iron solution that the strong reductant powder is joined step (1) of step (2) is carried out under 150W power ultrasonic condition.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058283A (en) * | 2013-02-01 | 2013-04-24 | 济南大学 | Preparation method of iron oxides with adjustable size, appearance and compositions |
| WO2015188744A1 (en) * | 2014-06-11 | 2015-12-17 | 佛山市南海新力电池有限公司 | Manufacturing method for carbon-coated nano-ferroferric oxide for battery |
| CN107694510A (en) * | 2017-11-14 | 2018-02-16 | 南昌大学 | A kind of two-dimensional magnetic MXene is to dyeing waste water Methylene Blue minimizing technology |
| CN107986337A (en) * | 2017-11-03 | 2018-05-04 | 浙江华源颜料股份有限公司 | A kind of easily scattered high coloring power iron oxide black and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57175734A (en) * | 1981-04-21 | 1982-10-28 | Res Inst For Prod Dev | Preparation of ultrafine particle of fe3o4 |
| CN102259192A (en) * | 2011-07-27 | 2011-11-30 | 南京师范大学 | Method for preparing nanometer zero-valent iron based on liquid-phase complexation reduction method |
-
2012
- 2012-07-03 CN CN201210227631.8A patent/CN102765761B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57175734A (en) * | 1981-04-21 | 1982-10-28 | Res Inst For Prod Dev | Preparation of ultrafine particle of fe3o4 |
| CN102259192A (en) * | 2011-07-27 | 2011-11-30 | 南京师范大学 | Method for preparing nanometer zero-valent iron based on liquid-phase complexation reduction method |
Non-Patent Citations (2)
| Title |
|---|
| 周永平等: "磷酸氢二钠器械消毒液的防锈试验", 《中国医院药学杂志》, vol. 14, no. 3, 31 December 1994 (1994-12-31), pages 141 * |
| 王晓辉: "铁的化合价呈现规律", 《中学课程辅导(初三版)》, no. 10, 31 December 2003 (2003-12-31), pages 43 - 3 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058283A (en) * | 2013-02-01 | 2013-04-24 | 济南大学 | Preparation method of iron oxides with adjustable size, appearance and compositions |
| WO2015188744A1 (en) * | 2014-06-11 | 2015-12-17 | 佛山市南海新力电池有限公司 | Manufacturing method for carbon-coated nano-ferroferric oxide for battery |
| JP2016534512A (en) * | 2014-06-11 | 2016-11-04 | ロンヂョウ ワンファー トレーディング カンパニー リミテッド | Method for producing carbon-coated nano-triiron tetraoxide for batteries |
| CN107986337A (en) * | 2017-11-03 | 2018-05-04 | 浙江华源颜料股份有限公司 | A kind of easily scattered high coloring power iron oxide black and preparation method thereof |
| 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 |
| CN107694510A (en) * | 2017-11-14 | 2018-02-16 | 南昌大学 | A kind of two-dimensional magnetic MXene is to dyeing waste water Methylene Blue minimizing technology |
| 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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| CN102765761B (en) | 2014-05-21 |
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