CN108455682B - Water-based Fe3O4Preparation method of nano powder - Google Patents
Water-based Fe3O4Preparation method of nano powder Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
Water-based Fe3O4A method for preparing nano powder, which relates to the technical field of magnetic nano powder preparation. Under the condition of room temperature, adding soluble ferric salt and potassium sodium tartrate into deionized water to prepare a reaction solution, adjusting the pH value of the reaction system to 6-14, transferring the reaction solution into reaction equipment to perform hydrothermal synthesis reaction, and obtaining the aqueous Fe3O4And (3) nano powder. The pH of the reaction solution and the type of iron salt play a key role in the formation and morphology of the final product. In systems with pH greater than 7, FeCl is used3.6H2In case of O, sodium potassium tartrate plays a role in reduction, and FeSO is used4.7H2And when O is contained, the potassium sodium tartrate plays a role of a template. Fe obtained by the invention3O4The nano particles and the nano sheets have higher saturation magnetization, have the quasi-superparamagnetic characteristic, and the two products have good dispersibility in water, so the nano particles and the nano sheets are expected to be used as carriers of biomedicine and various catalysts.
Description
Technical Field
The invention relates to the technical field of magnetic nano powder preparation, in particular to aqueous Fe3O4A method for preparing nano powder.
Background
Fe3O4The nano powder has excellent magnetic performance and can be used as an adsorbent, a catalyst and magnetic fluid. Further, Fe3O4The nano material can be used as a magnetic carrier, forms a composite magnetic material with a series of non-magnetic nano materials, and is widely applied to the aspects of pollutant treatment, catalytic reaction, drug targeted delivery and the like.
As is well known, Fe3O4Can be regarded as being made of FeO and Fe2O3A composite oxide of the above composition. According to this feature, Fe is produced3O4There are generally two main types of processes, namely partial reduction or partial oxidation and coprecipitation. For example, with Fe3+Selecting some reducing agents as raw materials, and adopting a partial reduction method to obtain high-purity Fe3O4. The method generally relies onThe like reducing agent can control Fe in a water system3+Partially reduced to Fe2+Then two kinds of iron ions are coprecipitated and dehydrated to form Fe3O4A phase. For example, the subject group has been treated with FeCl3.6H2O is used as a raw material, sodium citrate, triethanolamine, mannitol and other reducing agents are adopted to prepare Fe with various forms through hydrothermal success3O4And (3) nano materials. The method is simple to operate, low in cost and very wide in application. Secondly, with Fe2+Fe can also be prepared by partial oxidation method as raw material3O4. However, since Fe is present at room temperature2+Is easily oxidized in advance in air or water, and thus, high purity Fe is obtained3O4The method generally adopts special measures to prevent Fe2+And (3) early-stage oxidation of the raw materials. Likewise, if Fe is used3+And Fe2+Preparing Fe by coprecipitation method as raw material3O4In the aspect of experimental control, Fe is controlled2+Or else the purity of the product obtained will be affected.
The invention uses FeCl respectively3.6H2O and FeSO4.7H2O is iron source, and potassium sodium tartrate (KNaC) is adopted for the first time4H4O6.4H2O) is used as a coordination agent and a reducing agent, and two forms of Fe are successfully prepared by a hydrothermal method3O4High purity nano powder, solves Fe2+Pre-oxide problems. The method has the advantages of simple operation, low cost, environmental friendliness and the like, and is expected to be popularized and applied.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides water-based Fe3O4The preparation method of the nano-powder adopts sodium potassium tartrate as a complexing agent and a reducing agent for the first time, and successfully prepares two forms of Fe by a hydrothermal method3O4High purity nano powder, solves Fe2+Pre-oxide problems.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: water-based Fe3O4The preparation method of the nano-powder comprises the steps of adding soluble ferric salt and potassium sodium tartrate into deionized water to prepare a reaction solution at room temperature, adjusting the pH value of the reaction system to 6-14, transferring the reaction solution into reaction equipment, and carrying out hydrothermal synthesis reaction to obtain aqueous Fe3O4And (3) nano powder. The reaction temperature of the hydrothermal synthesis reaction is 180 ℃, and the reaction time is 4-24 h.
The use amount of potassium sodium tartrate and NaOH and FeCl3.6H2The O concentration is related to the pH requirement of the reaction solution, and under normal conditions, Fe3+When the concentration is constant, the using amount of the potassium sodium tartrate is determined according to that Fe is contained in a solution with the pH value of 7-143+It is preferable that no precipitate is generated. To Fe2+-KNaC4H4O6.4H2O-H2O reaction system, KNaC4H4O6.4H2The amount of O is such that Fe is present at room temperature2+The precondition is that no precipitation and no oxidation occur in the alkaline system.
Aqueous Fe as the invention3O4According to the preferable technical scheme of the preparation method of the nano powder, the soluble ferric salt is ferric chloride, and the molar ratio of the ferric chloride to the potassium sodium tartrate is 0.5-4: 1, the pH value of the reaction system is 7-14. The microstructure of the prepared product is irregular Fe3O4And (3) nanoparticles.
Aqueous Fe as the invention3O4According to another preferable technical scheme of the preparation method of the nano powder, the soluble ferric salt is ferrous sulfate, and the molar ratio of the ferrous sulfate to the potassium sodium tartrate is 0.5-2: 1, the pH value of the reaction system is 6-14. The microstructure of the prepared product is hexagonal flaky Fe3O4And (3) nanoparticles.
The invention relates to (FeCl)3.6H2O and FeSO4.7H2O, etc.) as iron source, KNaC4H4O6.4H2O is a green cheap reducing agent and a template agent. Experimental studies have found that the pH of the reaction solution and the type of iron salt play a key role in the formation and morphology of the final product. In systems with a pH greater than 7, Fe is usedCl3.6H2In case of O, sodium potassium tartrate plays a role in reduction, and FeSO is used4.7H2And when O is contained, the potassium sodium tartrate plays a role of a template. Therefore, the method can obtain the required target product only by controlling the pH value of the reaction solution and using the type of the ferric salt. Meanwhile, Fe obtained by the invention3O4The nano particles and the nano sheets have higher saturation magnetization, have the quasi-superparamagnetic characteristic, and the two products have good dispersibility in water, so the nano particles and the nano sheets are expected to be used as carriers of biomedicine and various catalysts.
Compared with the prior art, the invention also has the following beneficial effects:
1) and realize Fe3O4The purity and the form of the nano powder are simple and controllable, and the nano powder is high-performance Fe3O4The preparation and application of the nano material provide a new method.
2) The method has the advantages of simple experimental operation, low cost, environmental friendliness, large amount of obtained products and excellent physical and chemical properties of the products.
Drawings
FIG. 1 is a graph showing the influence of pH of the reaction system on the final reaction product in example 1;
FIGS. 2a to 2d are the morphological, phase and magnetic property analyses of the product of example 2;
FIGS. 3a to 3d are phase, morphology, composition and magnetic property analyses of the product of example 3;
FIGS. 4a to 4c show KNaC in example 44H4O6.4H2The effect of the amount of O used on the morphology of the product.
Detailed Description
The following example and attached drawing are combined to obtain the water-based Fe3O4The preparation method of the nano powder is further detailed. The structure, morphology and magnetic performance of the product obtained by the method are respectively characterized and analyzed by X-ray powder diffraction (XRD, D3500), a field emission scanning electron microscope (FE-SEM, SU8010) and a magnetic intensity vibration meter (VSM).
Example 1: influence of different pH systems on the product after reaction.
FeCl is added3.6H2O and KNaC4H4O6.4H2O is mixed according to the mass ratio of 1: 3 weighing the components, putting the components into 60mL of deionized water, stirring the mixture to dissolve the components, adjusting the pH of the solution by using a NaOH solution with the concentration of 2mol/L, transferring the solution into a reaction kettle, carrying out hydrothermal reaction for 16 hours at 180 ℃ and then inspecting the influence of different pH systems on the product after the reaction.
FIG. 1 is a graph showing the relationship between the pH of the reaction system and the final reaction product. As can be seen from FIG. 1, at a pH of less than 7, the reaction product was only a small amount of dark green Fe (OH)2Precipitating; when the pH value is about 7, a small amount of black magnetic product is obtained after the reaction, and the solution is brown, which indicates that iron ions which are not precipitated exist in the solution; when the pH value is more than 7, a large amount of black magnetic products are obtained after the reaction, and no iron ions exist in the solution.
Example 2: fe3O4And (4) preparing and characterizing the nano particles.
FeCl is added3.6H2O and KNaC4H4O6.4H2O is mixed according to the mass ratio of 1: 3, putting the weighed mixture into 60mL of deionized water, stirring the mixture to dissolve the mixture, adjusting the pH value of the mixture to 9 by using a NaOH solution with the concentration of 2mol/L, transferring the mixture into a reaction kettle, and carrying out hydrothermal reaction for 16 hours at 180 ℃ to obtain irregular Fe3O4And (3) nanoparticles.
After observing a large number of black products by using SEM, the product is in the form of irregular nano particles (shown in figure 2a and figure 2b), and the result of XRD phase analysis is combined to obtain that the irregular black product is Fe3O4(see FIG. 2 c). The room temperature magnetic property of the product is characterized by VSM, and the irregular Fe is known3O4Saturation magnetization (M) of nanopowders) About 65emu/g, coercive force (H)c) About 7Oe, with quasi-supersequence characteristics (see FIG. 2d) (coercivity H of the product)cAt 0, often referred to as super-ordered particles).
Based on the experimental results of examples 1 and 2, it can be considered that Fe is irregular3O4Nano meterThe powder formation process is as follows: first, the iron tartrate complex anion formed at room temperature destabilizes upon heating, with Fe therein3+Will be partially reduced to Fe by tartrate2+. Then, Fe in the reaction system2+And Fe3+According to the following steps of 1: 2 in an alkaline system to form Fe by coprecipitation reaction3O4The above two processes can be represented by equations (1) and (2), respectively.
Example 3: fe3O4And (3) preparation and characterization of the nanosheet.
With FeSO4·7H2O is an iron source, FeSO4·7H2O and KNaC4H4O6.4H2The mass ratio of O is 1: 1, weighing the solids according to a proportion, putting the solids into 60mL of deionized water, stirring to dissolve the solids, adjusting the pH value to 9 by using a NaOH solution with the concentration of 2mol/L, transferring the solution into a reaction kettle, and carrying out hydrothermal reaction for 16 hours at 180 ℃ to obtain hexagonal flaky Fe3O4And (3) nanoparticles.
First, as a result of analyzing the morphology and composition of the obtained product by SEM, the product obtained under the experimental conditions was hexagonal plate-shaped particles, the thickness of the plate was about 25nm, and the product was mainly composed of Fe and O elements (see fig. 3b and 3 c). Then, the phase analysis of the product by X-ray diffraction showed that the flaky product was Fe3O4(see FIG. 3 a). Finally, VSM test results further show that the hexagonal flaky Fe3O4The saturation magnetization of the nano powder is about 78emu/g, the coercive force is about 74Oe, the nano powder has a ferrimagnetic characteristic, and stable magnetic particles uniformly dispersed in a water system are quickly enriched under the action of an external magnetic field (see fig. 3 d).
Example 4: varying KNaC4H4O6.4H2Influence of the amount of O on the product after the reaction.
The reaction conditions were the same as in example 3, except that KNaC was not added4H4O6.4H2O、FeSO4·7H2O and KNaC4H4O6.4H2The mass ratio of O is 1: 2. FeSO4·7H2O and KNaC4H4O6.4H2The mass ratio of O is 1: investigation of Change KNaC4H4O6.4H2Influence of the amount of O on the product after the reaction.
After experiments, the KNaC is not added in the reaction system4H4O6.4H2O, except Fe at room temperature2+Fe can be obtained in addition to partial oxidation in alkaline system3O4Product, but product is Fe3O4Polyhedral large particles (see FIG. 4a), when FeSO4·7H2O and KNaC4H4O6.4H2The mass ratio of O is 1: 2 and 1: at 3 time, i.e. KNaC4H4O6.4H2When the amount of O is large, Fe is obtained3O4Will change in morphology: under optimum conditions (FeSO)4·7H2O and KNaC4H4O6.4H2The mass ratio of O is 1: 1) obtained hexagonal flaky Fe3O4Fe in large flakes gradually irregular3O4Transition (see fig. 4b and 4 c). It can be seen that KNaC4H4O6.4H2The amount of O to be used is such that Fe is finally formed3O4Has a great influence on the morphology of (2).
Based on the experimental results of examples 3 and 4, we believe that Fe2+-KNaC4H4O6.4H2O-H2O-system flaky Fe3O4The formation process of the nano powder is as follows: firstly, at room temperature, the stable ferrous tartrate coordinated anions are destabilized to release Fe when being heated2+And tartrate; then, Fe in the reaction system2+Will be reacted with OH-Formation of Fe (OH)2A metastable phase; finally, Fe (OH)2Oxidation reaction in alkaline system to form Fe3O4The above three processes can be represented by equations (3), (4) and (5), respectively.
It should be noted that the presence of a certain amount of tartrate in the reaction system not only stabilizes Fe2+May also function as a soft template, allowing the formation of Fe of different forms3O4And (3) nano materials.
Example 5: fe3O4And (4) preparing nanoparticles.
FeCl is added3.6H2O and KNaC4H4O6.4H2O is mixed according to the mass ratio of 1: 1, putting the weighed mixture into 60mL of deionized water, stirring the mixture to dissolve the mixture, adjusting the pH value of the mixture to 11 by using a NaOH solution with the concentration of 2mol/L, transferring the mixture into a reaction kettle, and carrying out hydrothermal reaction for 8 hours at 180 ℃ to obtain irregular Fe3O4And (3) nanoparticles.
Example 6: fe3O4And (3) preparing the nano sheet.
With FeSO4·7H2O is an iron source, FeSO4·7H2O and KNaC4H4O6.4H2The mass ratio of O is 2: 1, weighing the solids according to a proportion, putting the solids into 60mL of deionized water, stirring to dissolve the solids, adjusting the pH value to 14 by using a NaOH solution with the concentration of 2mol/L, transferring the solution into a reaction kettle, and carrying out hydrothermal reaction at 180 ℃ for 24 hours to obtain hexagonal flaky Fe3O4And (3) nanoparticles.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (1)
1. Water-based Fe3O4The preparation method of the nano powder is characterized in that FeSO is used4·7H2O and KNaC4H4O6· 4H2The mass ratio of O is 1: 1, weighing the solids according to a proportion, putting the solids into 60mL of deionized water, stirring to dissolve the solids, adjusting the pH value to 9 by using a NaOH solution with the concentration of 2mol/L, transferring the solution into a reaction kettle, and carrying out hydrothermal reaction for 16 hours at 180 ℃ to obtain hexagonal flaky Fe3O4A nanoparticle; the obtained product is hexagonal flaky particles, the thickness of the sheet is 25nm, the saturation magnetization is about 78emu/g, the coercive force is about 74Oe, and the product has ferrimagnetic characteristics.
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