CN111410236A - Preparation method of needle-shaped nano zinc ferrite powder - Google Patents
Preparation method of needle-shaped nano zinc ferrite powder Download PDFInfo
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- CN111410236A CN111410236A CN202010235702.3A CN202010235702A CN111410236A CN 111410236 A CN111410236 A CN 111410236A CN 202010235702 A CN202010235702 A CN 202010235702A CN 111410236 A CN111410236 A CN 111410236A
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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
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
Abstract
A preparation method of needle-shaped nano zinc ferrite powder comprises the following steps: (1) under the condition of stirring, adding an additive, ethanol, sodium salicylate, soluble starch and carbamide into water in sequence, and continuously stirring uniformly; (2) dropwise adding a zinc citrate solution into the reaction solution under the stirring condition, and then dropwise adding a ferrous acetate solution to obtain a precursor suspension; (3) ultrasonically dispersing the precursor suspension, and filtering; washing the solid phase with water and heating to 400-500 ℃. The needle-shaped nano zinc ferrite powder obtained by the method has good dispersibility, is not easy to agglomerate, and has simple and convenient preparation method and environmental protection.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of needle-shaped nano zinc ferrite powder.
Background
Nano zinc ferrite (ZnFe)2O4) Is an important functional material, and is widely used in the fields of environmental materials, magnetic materials, new energy materials and the like in recent years. At present, methods for preparing nano zinc ferrite include a coprecipitation method, a solid phase method, a solvothermal method, a sol-gel method, a template method, an electrostatic spinning method and the like. The patent with publication number CN101525156A discloses a preparation method of nano zinc ferrite, which comprises the following steps: uniformly mixing ferric salt, zinc salt and cyclodextrin solution at normal temperature and normal pressure, filtering after magnetic stirring, drying the product at 50-150 ℃ for 10-48 h, and roasting the dried product at 500-900 ℃ for 1-5 h. Publication No. CN109090139A discloses a method for preparing antibacterial zinc ferrite nanoparticles and its application, wherein the zinc ferrite nanoparticles are prepared by simple coprecipitation method at room temperature, and the prepared powder has the problems of easy agglomeration and large particle size. Patent publication No. CN110339813A discloses a nano-composite magnetic material for air purification and a preparation method thereof, and although nano-zinc ferrite can also be prepared, the preparation process is complicated. Patent publication No. CN110198783A discloses a method for preparing a zinc ferrite catalyst, in which a zinc precursor solution is brought into contact with an alkaline solution to obtain a first precipitate, an iron precursor solution is added to the first precipitate to obtain a second precipitate, and the second precipitate is dried and fired. The patent of publication No. CN109806876A discloses a magnetic zinc ferrite/graphene nano composite photocatalyst, and a preparation method and application thereof, wherein the preparation method of zinc ferrite adopts diethylene glycol as a solvent, polyethylene glycol as a morphology control agent, sodium dodecyl sulfate as a dispersing agent, and sodium acetate hydrolysis is utilized to provide an alkaline condition, so that zinc ferrite uniformly nucleates and grows on the surface of graphene, and the prepared zinc ferrite has good dispersibility, but the graphene is expensive, thereby restricting the wide application thereof. The patent of publication No. CN109455766A discloses a superfine zinc ferrite nano-particle and a preparation method and gas-sensitive application thereof, wherein the preparation method of the zinc ferrite comprises the steps of firstly weighing zinc nitrate hexahydrate and ferric nitrate nonahydrate to be mixed with an ethanol solution, after the mixture is uniformly mixed, dropwise adding ammonia water into the mixed solution, adjusting the pH value of the solution, stirring for water bath and ultrasonic treatment for 10-60 min, then transferring the mixed solution into a high-pressure reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle in an oven at 150-230 ℃ for reaction for 12h, centrifugally drying and the like; although zinc ferrite nanoparticles can also be prepared, the process is cumbersome and requires a long time.
According to a plurality of research reports, the morphology influences the nano ZnFe2O4The photocatalytic performance, the bactericidal performance, the magnetic performance, the adsorption performance and other important influencing factorsThe medium-needle-shaped nano zinc ferrite has excellent performance in the fields of environmental purification and catalysis; at present, low-cost preparation methods of needle-shaped and good-dispersibility nano zinc ferrite are rarely reported.
Disclosure of Invention
The invention aims to provide a preparation method of needle-shaped nano zinc ferrite powder, which prepares needle-shaped zinc ferrite powder with good dispersibility and difficult agglomeration by a simple process in a mode of preparing multi-component reaction solution and dripping a zinc source and an iron source.
The method of the invention is carried out according to the following steps:
1. adding an additive, ethanol, sodium salicylate, soluble starch and carbamide into water in sequence under the condition of stirring, and continuously stirring uniformly to prepare a reaction solution; wherein the additive accounts for 0.03-0.08% of the mass of water, the ethanol accounts for 5-20% of the mass of water, the sodium salicylate accounts for 3-11% of the mass of water, the soluble starch accounts for 4-12% of the mass of water, and the carbamide accounts for 3-16% of the mass of water;
2. dropwise adding a zinc citrate solution into the reaction solution under the stirring condition, after dropwise adding is finished for 2-6 min, continuously dropwise adding a ferrous acetate solution under the stirring condition, and obtaining a precursor suspension after dropwise adding is finished;
3. ultrasonically dispersing the precursor suspension for 5-18 min under the standing condition, and then filtering and separating out a solid phase; washing the solid phase with water until the washing solution is neutral, and then heating to 400-500 ℃ to obtain needle-shaped nano zinc ferrite powder; wherein the heating speed is controlled to be 15-19 ℃/min during heating.
In the step 1, the additive is a mixture of sodium glutamate and allyl polyoxyethylene ether, wherein the sodium glutamate accounts for 19-34% of the total mass of the additive.
In the step 1, the stirring speed is 900-1200 rpm, and the continuous stirring time is 2-8 min.
In the step 2, the concentration of the zinc citrate solution is 0.2-0.6M, and the adding amount of the zinc citrate solution is 3-6 by the molar ratio of the carbonic amide to the zinc citrate in the reaction solution; the concentration of the ferrous acetate solution is 0.2-0.8M, and the addition amount of the ferrous acetate is 0.5 according to the molar ratio of the zinc citrate to the ferrous acetate in all the materials.
In the step 2, the stirring speed during stirring is 1200-1800 rpm.
In the step 2, when the zinc citrate solution and the ferrous acetate solution are dripped, the dripping speed is controlled to be 10-16 drops/min.
In the step 3, the heating is performed by microwave heating.
The average particle size of the acicular nano zinc ferrite powder is 12-30 nm, and the average length is 1-4 mu m.
The method of the invention prepares a reaction solution based on specific additive components, and finishes the preparation of zinc ferrite by utilizing the catalytic action of carbamide regulated by an additive through a short flow reaction based on specific zinc source and iron source; the obtained needle-shaped nano zinc ferrite powder has good dispersibility, is not easy to agglomerate, and has simple preparation method and environmental protection.
Detailed Description
The water used in the examples of the present invention is deionized water.
Sodium glutamate, allyl polyoxyethylene ether, ethanol, sodium salicylate, soluble starch and carbamide (urea) which are adopted in the embodiment of the invention are commercially available analytical pure reagents.
The zinc citrate solution and the ferrous acetate solution adopted in the embodiment of the invention are prepared from commercially available analytical pure reagents and water.
The ultrasonic frequency in the ultrasonic dispersion in the embodiment of the invention is 28 kHz.
In the embodiment of the invention, the water washing is carried out for three times after the solid phase is soaked in water and filtered.
In the embodiment of the invention, when the zinc citrate solution and the ferrous acetate solution are dripped, the dripping speed is controlled to be 10-16 drops/min
The following examples are intended only to illustrate the invention in detail and are not intended to limit the scope of the invention in any way.
Example 1
Adding additive, ethanol, sodium salicylate, soluble starch and carbamide into water (100g) in sequence under the condition of stirring speed of 900rpm, and continuously stirring for 2min to prepare reaction solution; wherein the additive accounts for 0.03 percent of the mass of water, the ethanol accounts for 5 percent of the mass of water, the sodium salicylate accounts for 3 percent of the mass of water, the soluble starch accounts for 4 percent of the mass of water, and the carbamide accounts for 3.6 percent of the mass of water; the additive is a mixture of sodium glutamate and allyl polyoxyethylene ether, wherein the sodium glutamate accounts for 19% of the total mass of the additive;
dropwise adding a zinc citrate solution into the reaction solution under the condition of a stirring speed of 1200rpm, after dropwise adding is finished within 2min, continuously dropwise adding a ferrous acetate solution under the condition of stirring, and obtaining a precursor suspension after dropwise adding is finished; the concentration of the zinc citrate solution is 0.2M, and the adding amount of the zinc citrate solution is 3 according to the molar ratio of the carbonic amide to the zinc citrate in the reaction solution; the concentration of the ferrous acetate solution is 0.2M, and the adding amount of the ferrous acetate is 0.5 according to the molar ratio of the zinc citrate to the ferrous acetate in all the materials;
ultrasonically dispersing the precursor suspension for 5min under the standing condition, and then filtering and separating out a solid phase; washing the solid phase with water until the washing solution is neutral, and then heating the solid phase to 400 ℃ by microwave to obtain needle-shaped nano zinc ferrite powder; wherein the heating speed is controlled to be 15 ℃/min during heating;
the average particle size of the needle-shaped nano zinc ferrite powder is 12nm, and the average length is 1 mu m.
Example 2
The method is the same as example 1, except that:
(1) adding an additive, ethanol, sodium salicylate, soluble starch and carbamide into water in sequence under the condition of a stirring speed of 1100rpm, and continuously stirring for 4min to prepare a reaction solution; wherein the additive accounts for 0.04 percent of the mass of water, the ethanol accounts for 10 percent of the mass of water, the sodium salicylate accounts for 6 percent of the mass of water, the soluble starch accounts for 9 percent of the mass of water, and the carbamide accounts for 7.5 percent of the mass of water; the additive is a mixture of sodium glutamate and allyl polyoxyethylene ether, wherein the sodium glutamate accounts for 34% of the total mass of the additive;
(2) dropwise adding a zinc citrate solution into the reaction solution under the condition of a stirring speed of 1400rpm, and finishing dropwise adding within 4 min; the concentration of the zinc citrate solution is 0.4M, and the adding amount of the zinc citrate solution is 4 according to the molar ratio of the carbonic amide to the zinc citrate in the reaction solution; the concentration of the ferrous acetate solution is 0.4M;
(3) ultrasonic dispersing for 10 min; heating to 420 ℃ by microwave, wherein the heating speed is 16 ℃/min;
(4) the average particle size of the needle-shaped nano zinc ferrite powder is 18nm, and the average length is 2 mu m.
Example 3
The method is the same as example 1, except that:
(1) adding an additive, ethanol, sodium salicylate, soluble starch and carbamide into water in sequence under the condition of stirring speed of 1000rpm, and continuously stirring for 5min to prepare a reaction solution; wherein the additive accounts for 0.06 percent of the mass of water, the ethanol accounts for 15 percent of the mass of water, the sodium salicylate accounts for 8 percent of the mass of water, the soluble starch accounts for 6 percent of the mass of water, and the carbamide accounts for 16 percent of the mass of water; the additive is a mixture of sodium glutamate and allyl polyoxyethylene ether, wherein the sodium glutamate accounts for 23% of the total mass of the additive;
(2) dropwise adding a zinc citrate solution into the reaction solution under the condition of stirring speed of 1600rpm, and finishing dropwise adding within 5 min; the concentration of the zinc citrate solution is 0.6M, and the adding amount of the zinc citrate solution is 5 according to the molar ratio of the carbonic amide to the zinc citrate in the reaction solution; the concentration of the ferrous acetate solution is 0.6M;
(3) ultrasonic dispersing for 16 min; heating to 460 ℃ by microwave, wherein the heating speed is 18 ℃/min;
(4) the average particle size of the needle-shaped nano zinc ferrite powder is 21nm, and the average length is 3 mu m.
Example 4
The method is the same as example 1, except that:
(1) adding an additive, ethanol, sodium salicylate, soluble starch and carbamide into water in sequence under the condition of a stirring speed of 1200rpm, and continuously stirring for 8min to prepare a reaction solution; wherein the additive accounts for 0.08 percent of the mass of water, the ethanol accounts for 20 percent of the mass of water, the sodium salicylate accounts for 11 percent of the mass of water, the soluble starch accounts for 12 percent of the mass of water, and the carbamide accounts for 7.2 percent of the mass of water; the additive is a mixture of sodium glutamate and allyl polyoxyethylene ether, wherein the sodium glutamate accounts for 28% of the total mass of the additive;
(2) dropwise adding a zinc citrate solution into the reaction solution under the condition of a stirring speed of 1800rpm, and finishing dropwise adding in 6 min; the concentration of the zinc citrate solution is 0.5M, and the adding amount of the zinc citrate solution is 6 according to the molar ratio of the carbonic amide to the zinc citrate in the reaction solution; the concentration of the ferrous acetate solution is 0.8M;
(3) ultrasonic dispersion for 18 min; heating to 500 deg.C with microwave, and heating at a speed of 19 deg.C/min;
(4) the average particle size of the needle-shaped nano zinc ferrite powder is 30nm, and the average length is 4 mu m.
Claims (7)
1. A preparation method of needle-shaped nano zinc ferrite powder is characterized by comprising the following steps:
(1) adding an additive, ethanol, sodium salicylate, soluble starch and carbamide into water in sequence under the condition of stirring, and continuously stirring uniformly to prepare a reaction solution; wherein the additive accounts for 0.03-0.08% of the mass of water, the ethanol accounts for 5-20% of the mass of water, the sodium salicylate accounts for 3-11% of the mass of water, the soluble starch accounts for 4-12% of the mass of water, and the carbamide accounts for 3-16% of the mass of water;
(2) dropwise adding a zinc citrate solution into the reaction solution under the stirring condition, after dropwise adding is finished for 2-6 min, continuously dropwise adding a ferrous acetate solution under the stirring condition, and obtaining a precursor suspension after dropwise adding is finished;
(3) ultrasonically dispersing the precursor suspension for 5-18 min under the standing condition, and then filtering and separating out a solid phase; washing the solid phase with water until the washing solution is neutral, and then heating to 400-500 ℃ to obtain needle-shaped nano zinc ferrite powder; wherein the heating speed is controlled to be 15-19 ℃/min during heating.
2. The method for preparing the needle-shaped nano zinc ferrite powder according to claim 1, wherein in the step (1), the additive is a mixture of sodium glutamate and allyl polyoxyethylene ether, wherein the sodium glutamate accounts for 19-34% of the total mass of the additive.
3. The method for preparing acicular nano zinc ferrite powder according to claim 1, characterized in that in the step (1), the stirring speed is 900-1200 rpm, and the time for continuing stirring is 2-8 min.
4. The method for preparing the acicular nano zinc ferrite powder according to claim 1, wherein in the step (2), the concentration of the zinc citrate solution is 0.2-0.6M, and the adding amount of the zinc citrate solution is that the molar ratio of the carbonic amide to the zinc citrate in the reaction solution is 3-6; the concentration of the ferrous acetate solution is 0.2-0.8M, and the addition amount of the ferrous acetate is 0.5 according to the molar ratio of the zinc citrate to the ferrous acetate in all the materials.
5. The method for preparing acicular nano zinc ferrite powder according to claim 1, characterized in that in the step (2), the stirring speed is 1200-1800 rpm.
6. The method for preparing acicular nano zinc ferrite powder according to claim 1, characterized in that in the step (3), the heating is microwave heating.
7. The method for preparing acicular nano zinc ferrite powder according to claim 1, characterized in that the average particle size of the acicular nano zinc ferrite powder is 12-30 nm, and the average length is 1-4 μm.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102208637A (en) * | 2010-11-09 | 2011-10-05 | 广州市香港科大霍英东研究院 | ZnFe2O4/C composite cathode material with hollow sphere structure and one-step preparation method thereof |
| WO2013029200A1 (en) * | 2011-08-29 | 2013-03-07 | 山西省电力公司 | Method for preparing hollow ni-zn ferrite microsphere |
| CN103094558A (en) * | 2012-12-18 | 2013-05-08 | 深圳市贝特瑞新能源材料股份有限公司 | Zinc-ferrite-based nanometer composite as well as preparation method and application thereof |
| CN104393244A (en) * | 2014-11-28 | 2015-03-04 | 东北林业大学 | Preparation method of hollow ZnFe2O4 nanometer anode material of lithium ion battery |
| CN110902726A (en) * | 2019-11-15 | 2020-03-24 | 安徽建筑大学 | Micro-nano structure zinc ferrite hollow sphere and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102208637A (en) * | 2010-11-09 | 2011-10-05 | 广州市香港科大霍英东研究院 | ZnFe2O4/C composite cathode material with hollow sphere structure and one-step preparation method thereof |
| WO2013029200A1 (en) * | 2011-08-29 | 2013-03-07 | 山西省电力公司 | Method for preparing hollow ni-zn ferrite microsphere |
| CN103094558A (en) * | 2012-12-18 | 2013-05-08 | 深圳市贝特瑞新能源材料股份有限公司 | Zinc-ferrite-based nanometer composite as well as preparation method and application thereof |
| CN104393244A (en) * | 2014-11-28 | 2015-03-04 | 东北林业大学 | Preparation method of hollow ZnFe2O4 nanometer anode material of lithium ion battery |
| CN110902726A (en) * | 2019-11-15 | 2020-03-24 | 安徽建筑大学 | Micro-nano structure zinc ferrite hollow sphere and preparation method thereof |
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