CN102390872A - Preparation method of micrometer-scale cubic ultrodispersed ferroferric oxide particles - Google Patents
Preparation method of micrometer-scale cubic ultrodispersed ferroferric oxide particles Download PDFInfo
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- CN102390872A CN102390872A CN2011102266063A CN201110226606A CN102390872A CN 102390872 A CN102390872 A CN 102390872A CN 2011102266063 A CN2011102266063 A CN 2011102266063A CN 201110226606 A CN201110226606 A CN 201110226606A CN 102390872 A CN102390872 A CN 102390872A
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Abstract
The invention discloses a preparation method of micrometer-scale cubic ultrodispersed ferroferric oxide particles. The preparation method comprises the following steps of: 101, dissolving a trivalent ferric salt and a divalent ferric salt in deionized water to form reaction liquid; 102, adding hydrogen peroxide to the reaction liquid, dropwise adding an alkaline solution, and regulating the pH value of the reaction liquid to 9-10 to form suspension liquid; 103, feeding the suspension liquid to a stainless steel reaction kettle with a tetrafluoroethylene base pad, putting the stainless steel reaction kettle into a drying box, reacting for 12h, and then cooling to room temperature to obtain ferroferric oxide particles; 104, washing the ferroferric oxide particles by using deionized water and drying the particles; and 105, putting the ferroferric oxide particles obtained in the step 104 in a muffle furnace to obtain the ferroferric oxide particles. The ferroferric oxide particles prepared by using the preparation method disclosed by the invention have micrometer-scale size, regular cubic shape and good dispersibility.
Description
Technical field
The invention belongs to the technical field of preparation ultrafine powder, specifically, relate to a kind of preparation method who is the cubical ultra-dispersed ferriferrous oxide particles of micron order.
Background technology
Z 250 superfine powder particle is made starting material and is easy to get because its chemicalstability is good at present, and making processes is easier relatively, has been widely used in magnetic functional material, like functional materialss such as magnetic recording material, magnetic parting material and magnetic paints.Yet the dispersiveness of magneticsubstance directly has influence on its application prospect, and therefore, it is even to prepare particle diameter, and shape is regular, and the research of the magneticsubstance that magnetic is stronger becomes the focus of magneticsubstance research.The preparation method of ferriferrous oxide particles is numerous, and the method for common employing has two kinds, and a kind of is to be trivalent iron salt and divalent iron salt mixed solution and the strong alkaline aqueous solution direct reaction of 2:1 with mol ratio directly.This method needs to feed nitrogen as protective gas in the preparation process, thereby the renders operation process is complicated, and production cost is high, is difficult to large-scale production.Second kind of domestic method is that hydrothermal method is synthetic.The synthetic Z 250 of hydrothermal method is widely used at present.Temperature is higher in the hydrothermal preparation process, generates ferroferric oxide nano granules and is prone to reunite, and causes hydrothermal method synthesis of nano Z 250 dispersing property not good.Yet simple to operate being easy to of hydrothermal method accomplished scale production.More than two kinds of methods be the preparation that under alkaline environment, realizes Z 250, the ferriferrous oxide particles that under alkaline environment, prepares is little, generally at 100-5 nm, is difficult to prepare the bigger ferriferrous oxide particles of particle.Because the need usefulness of using, the preparation pattern is regular, and finely disseminated uniform particle diameter magnetic-particle will help expanding the utilization of magneticsubstance.
Summary of the invention
Technical problem:Technical problem to be solved by this invention is: a kind of preparation method who is the cubical ultra-dispersed ferriferrous oxide particles of micron order; The size of the ferriferrous oxide particles that this preparation method processes reaches micron order; Shape is the cubes of rule; And can not reunite good dispersivity between the ferriferrous oxide particles.
Technical scheme:For solving the problems of the technologies described above, the technical scheme that the present invention adopts is:
The preparation method who is the cubical ultra-dispersed ferriferrous oxide particles of micron order of the present invention is characterized in that, this preparation method may further comprise the steps:
101. with mol ratio is that trivalent iron salt and the divalent iron salt of 2:1 is dissolved in the deionized water, forms reaction solution;
102. in the reaction solution that step 101 obtains, add ydrogen peroxide 50, react after 30 minutes, in this reaction solution, splash into basic soln, reacting liquid pH value is transferred to 9-10, form suspension-s;
103. the suspension-s that step 102 is obtained places the stainless steel cauldron of tetrafluoroethylene heelpiece, and this stainless steel cauldron is inserted in 120-180 ℃ the baking oven, reacts after 12 hours, is cooled to room temperature, obtains being cubical ferriferrous oxide particles;
104., remove the iron ion that remains in the ferriferrous oxide particles surface, dry then ferriferrous oxide particles with the ferriferrous oxide particles that deionized water cleaning step 103 obtains;
105. the ferriferrous oxide particles that step 104 is obtained places 300-600 ℃ muffle furnace calcination 4-12 hour, obtains ferriferrous oxide particles.
Beneficial effect:Compared with prior art, the present technique scheme has following beneficial effect:
1. the ferriferrous oxide particles size is micron order, and shape is the cubes of rule.The ferriferrous oxide particles size of prior art for preparing is nano level generally at 200-300 nm, and complex-shaped.And the ferriferrous oxide particles size of present technique scheme preparation is micron order, and shape is the cubes that length all equates.
2. can not reunite between the ferriferrous oxide particles, good dispersivity, magnetic is good.Adopt present technique scheme gained ferriferrous oxide particles to belong to micron order.Adopt water or ethanol to do evengranular being dispersed in the dispersion agent that dispersion agent just can be prepared with this programme under less external force effect.Good dispersivity between the particle can not reunited.Because particle is big,, help expanding its range of application at the sedimentation speed of dispersion agent ferriferrous oxide particles greater than existing hydrothermal preparation.
3. reduce the influence of alkaline matter to environment.In the present technique scheme, in the step 102, add ydrogen peroxide 50, make the iron ion oxidation generate as oxygenant.Rely in the prior art and add alkaline matter as oxygenant.Therefore, in the present technique scheme, replace alkaline matter as oxygenant, reduced the influence of alkaline matter environment through ydrogen peroxide 50.
4. the preparation method is simple to operate, is easy to suitability for industrialized production.The step of the preparation ferriferrous oxide particles that the present technique scheme provides is simple, and easy handling can be realized the industrial production of mass-producing.
Description of drawings
Fig. 1 is the ESEM picture of the ferriferrous oxide particles of the embodiment of the invention 1 preparation.
Fig. 2 is the X-ray diffraction picture of the ferriferrous oxide particles of the embodiment of the invention 1 preparation.
Embodiment
A kind of preparation method who is the cubical ultra-dispersed ferriferrous oxide particles of micron order of the present invention may further comprise the steps:
101. with mol ratio is that trivalent iron salt and the divalent iron salt of 2:1 is dissolved in the deionized water, forms reaction solution.
102. in the reaction solution that step 101 obtains, add ydrogen peroxide 50, react after 30 minutes, in this reaction solution, splash into basic soln, pH transfers to 9-10 with reaction solution, forms suspension-s.
In this step, the concentration of the hydrogen peroxide in the ydrogen peroxide 50 is 30%, and promptly to account for the mass fraction of ydrogen peroxide 50 be 30% to hydrogen peroxide.The volume percent of ydrogen peroxide 50 and reaction solution is 0.6%-4%.
103. the suspension-s that step 102 is obtained places the stainless steel cauldron of tetrafluoroethylene heelpiece, and this stainless steel cauldron is inserted in 120-180 ℃ the baking oven, reacts after 12 hours, is cooled to room temperature, obtains being cubical ferriferrous oxide particles.
This step is to produce the hydro-thermal reaction of ferriferrous oxide particles.Tetrafluoroethylene is a high temperature material.The pad that the tetrafluoroethylene material is processed can provide the seal inside environment of hydro-thermal reaction.Stainless steel cauldron places 120-180 ℃ baking oven, the temperature that provides ferriferrous oxide particles to form.Water forms a kind of internal medium of HTHP under 120-180 ℃ of situation, the formation that utilizes ferriferrous oxide particles is arranged.In reaction solution; After adding ydrogen peroxide 50 and basic soln successively; Ydrogen peroxide 50 and basic soln common and ferric ion and ferrous ion reaction, generation is the cubes ferriferrous oxide particles in 120-180 ℃ baking oven then, and this particulate size is a micron level.
104., remove the iron ion that remains in the ferriferrous oxide particles surface, dry then ferriferrous oxide particles with the ferriferrous oxide particles that deionized water cleaning step 103 obtains.
In this step, deionized water can be removed the iron ion on ferriferrous oxide particles surface.Preferred three times of the number of times of washed with de-ionized water ferriferrous oxide particles.Wash number very little, then the iron ion on ferriferrous oxide particles surface is residual just more.Wash number is too many, and then the iron ion in the ferriferrous oxide particles will be cleaned, and influences the shape of ferriferrous oxide particles itself.In addition, dry ferriferrous oxide particles carries out in vacuum environment, and be 2-3 hour time of drying.Dry ferriferrous oxide particles in vacuum environment can be saved time of drying, improves preparation efficiency.
105. the ferriferrous oxide particles that step 104 is obtained places 300-600 ℃ muffle furnace calcination 4-12 hour, obtains ferriferrous oxide particles.
In this step, ferriferrous oxide particles is carried out high-temperature calcination, make the magnetic responsiveness of ferriferrous oxide particles strengthen, make ferriferrous oxide particles can satisfy the requirement of magneticsubstance.
Generally speaking, this preparation method comprises hydro-thermal reaction and high-temperature calcination, and hydro-thermal reaction is a step 103, generates through hydro-thermal reaction to be cubical ferriferrous oxide particles.High-temperature calcination is a step 105, strengthens the magnetic responsiveness of ferriferrous oxide particles through high-temperature calcination.So-called ultra-dispersed ferriferrous oxide particles is meant between the ferriferrous oxide particles agglomeration can not occur, can contact between the particle, but can not bond together.Ferriferrous oxide particles in the present technique scheme is the micron order monocrystalline.Through increasing the size of ferriferrous oxide particles, improve the dispersiveness of ferriferrous oxide particles.
Through three embodiment technical scheme of the present invention is specified below.
Embodiment 1
2.7 gram iron(ic)chloride and 1 gram iron protochloride are dissolved in the 100 mL deionized waters; Add ydrogen peroxide 50 1 mL then, react after 30 minutes, splash into ammoniacal liquor 1 mL; Reaction solution is placed the stainless steel cauldron of 50 mL tetrafluoroethylene heelpieces; Reaction kettle is inserted 120 ℃ of reactions after 12 hours, be cooled to room temperature, obtain being cubical ferriferrous oxide particles; With washed with de-ionized water ferriferrous oxide particles three times, remove the iron ion that remains in particle surface, vacuum-drying placed 300 ℃ of muffle furnace calcination after 12 hours after 2 hours, was cooled to room temperature, obtained ferriferrous oxide particles.Adopt sem to characterize to the ferriferrous oxide particles that finally obtains, its magnification is 1500 times, and is as shown in Figure 1; The particle diameter of ferriferrous oxide particles is 3 μ m, and the gap between the particle is big, good dispersivity; Can not reunite, ferriferrous oxide particles is cubes.Adopt X-ray diffractometer to characterize to the ferriferrous oxide particles that finally obtains simultaneously.Sweep limit is 2 θ, spends to 80 degree from 20.As shown in Figure 2, X-coordinate is an angle of diffraction, and ordinate zou is a diffraction peak intensity, and ferriferrous oxide particles demonstrates the Z 250 crystalline phase of standard, and percent crystallinity is better, so the magnetic of ferriferrous oxide particles is stronger.
5.4 gram iron(ic)chloride and 2 gram iron protochlorides are dissolved in the 100 mL deionized waters, add ydrogen peroxide 50 1 mL, react after 30 minutes; Splash into 1mol/L NaOH solution 1 mL, reaction solution is placed the stainless steel cauldron of 50 mL tetrafluoroethylene heelpieces, reaction kettle is inserted in 160 ℃ the baking oven reaction after 12 hours; Be cooled to room temperature, obtain being cubical ferriferrous oxide particles, with washed with de-ionized water ferriferrous oxide particles three times; Remove the iron ion that remains in the ferriferrous oxide particles surface; After the vacuum-drying 2 hours, place 500 ℃ of muffle furnace calcination 6 hours, obtain ferriferrous oxide particles.The testing method that adopts with embodiment 1 is identical, adopts sem and X-ray diffractometer to characterize to the ferriferrous oxide particles that finally obtains, and this ferriferrous oxide particles is cubes; Simultaneously, the particle diameter of ferriferrous oxide particles is 4 μ m, good dispersivity; Better crystallinity degree, magnetic is strong.
Embodiment 3
4 gram ferric sulfate and 2.7 gram ferrous sulfate are dissolved in the 100 mL deionized waters, add ydrogen peroxide 50 1 mL, react after 30 minutes; Splash into ammoniacal liquor 1 mL, reaction solution is placed the stainless steel cauldron of 50 mL tetrafluoroethylene heelpieces, reaction kettle is inserted in 140 ℃ the baking oven reaction after 12 hours; Be cooled to room temperature, obtain being cubical ferriferrous oxide particles, with washed with de-ionized water ferriferrous oxide particles three times; Remove the iron ion that remains in the ferriferrous oxide particles surface; After the vacuum-drying 2 hours, place 600 ℃ of muffle furnace calcination 6 hours, obtain ferriferrous oxide particles.Adopt sem and X-ray diffractometer to characterize to the ferriferrous oxide particles that finally obtains, this ferriferrous oxide particles is cubes, and simultaneously, the particle diameter of ferriferrous oxide particles is 4 μ m, good dispersivity.
Claims (4)
1. a preparation method who is the cubical ultra-dispersed ferriferrous oxide particles of micron order is characterized in that, this preparation method may further comprise the steps:
101. with mol ratio is that trivalent iron salt and the divalent iron salt of 2:1 is dissolved in the deionized water, forms reaction solution;
102. in the reaction solution that step 101 obtains, add ydrogen peroxide 50, react after 30 minutes, in this reaction solution, splash into basic soln, reacting liquid pH value is transferred to 9-10, form suspension-s;
103. the suspension-s that step 102 is obtained places the stainless steel cauldron of tetrafluoroethylene heelpiece, and this stainless steel cauldron is inserted in 120-180 ℃ the baking oven, reacts after 12 hours, is cooled to room temperature, obtains being cubical ferriferrous oxide particles;
104., remove the iron ion that remains in the ferriferrous oxide particles surface, dry then ferriferrous oxide particles with the ferriferrous oxide particles that deionized water cleaning step 103 obtains;
105. the ferriferrous oxide particles that step 104 is obtained places 300-600 ℃ muffle furnace calcination 4-12 hour, obtains ferriferrous oxide particles.
2. according to the described preparation method who is the cubical ultra-dispersed ferriferrous oxide particles of micron order of claim 1; It is characterized in that; The concentration of the hydrogen peroxide in the ydrogen peroxide 50 in the described step 102 is 30%, and the volume percent of ydrogen peroxide 50 and reaction solution is 0.6%-4%.
3. according to the described preparation method who is the cubical ultra-dispersed ferriferrous oxide particles of micron order of claim 1, it is characterized in that, in the described step 104, washed with de-ionized water ferriferrous oxide particles three times.
4. according to the described preparation method who is the cubical ultra-dispersed ferriferrous oxide particles of micron order of claim 1, it is characterized in that in the described step 104, dry ferriferrous oxide particles carries out in vacuum environment, be 2-3 hour time of drying.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103204551A (en) * | 2013-04-12 | 2013-07-17 | 陕西科技大学 | Controllable preparation method of micron-order Fe3O4 |
| CN107162063A (en) * | 2017-07-05 | 2017-09-15 | 合肥学院 | A kind of size tunable Fe3O4The preparation method of nano powder and its application in water-oil separating |
| CN111187065A (en) * | 2020-01-15 | 2020-05-22 | 湖南航天磁电有限责任公司 | Microwave oven magnetic slurry containing ammonium polyacrylate dispersant and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204551A (en) * | 2013-04-12 | 2013-07-17 | 陕西科技大学 | Controllable preparation method of micron-order Fe3O4 |
| CN103204551B (en) * | 2013-04-12 | 2014-08-27 | 陕西科技大学 | Controllable preparation method of micron-order Fe3O4 |
| CN107162063A (en) * | 2017-07-05 | 2017-09-15 | 合肥学院 | A kind of size tunable Fe3O4The preparation method of nano powder and its application in water-oil separating |
| CN107162063B (en) * | 2017-07-05 | 2018-08-17 | 合肥学院 | A kind of size tunable Fe3O4The preparation method of nano powder and its application in water-oil separating |
| CN111187065A (en) * | 2020-01-15 | 2020-05-22 | 湖南航天磁电有限责任公司 | Microwave oven magnetic slurry containing ammonium polyacrylate dispersant and preparation method thereof |
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