Preparation method of magnetic metal composite nanomaterial
By loading palladium-iron nanomaterials onto iron oxide using a simple preparation method, the problem of requiring additional additives and special processes in existing methods is solved, and palladium-iron nanomaterials with uniform particle size can be prepared at low cost and with high efficiency.
Patent Information
- Application Number
- CN202610224175.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-02-25
- Publication Date
- 2026-05-05
AI Technical Summary
Existing methods for synthesizing palladium-iron nanomaterials require additional additives and special processes, which are costly and complex.
A simple preparation method was adopted, in which iron tetroxide was ultrasonically stirred in a solvent, iron pentacarbonyl and palladium compound were added, stirred at 80°C for 2 h, cooled, centrifuged, washed and vacuum dried to obtain palladium iron tetroxide-loaded composite material.
This method enables the low-cost and efficient preparation of palladium-iron nanomaterials with uniform particle size, avoiding additional additives and complex processes. It is cost-effective and has good loading performance.
Smart Images
Figure CN121972675A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of magnetic metal composite material preparation technology, and more specifically, to a method for preparing palladium-iron nanomaterials supported on iron tetroxide. Background Technology
[0002] Nanomaterials are materials that have at least one nanometer-sized dimension (0.1–100 nm) in three-dimensional space or are composed of nanometer-sized units, roughly equivalent to 10–100 atoms packed tightly together. The size of these structural units is between 0.1 and 100 nm. Because their size is close to the coherence length of electrons, their properties change significantly due to self-organization resulting from strong coherence. Furthermore, their scale is close to the wavelength of light, and coupled with their large surface area, the properties exhibited by nanomaterials, such as melting point, magnetism, optics, thermal conductivity, and electrical conductivity, often differ from those exhibited by the material in its bulk state. Metallic nanomaterials are an important branch of nanomaterials. Metallic nanoparticles exhibit many superior properties not found in bulk materials and can be applied in many fields. Palladium is a member of the platinum group elements in Group VIII of the fifth period, a silvery-white transition metal. Palladium is relatively soft, with good ductility and plasticity, and can be forged, rolled, and drawn into wires. It is an indispensable key material in high-tech fields such as aerospace and the automotive industry. In the chemical field, palladium is an important catalyst. In addition, palladium is also a raw material in some dental materials, watches, and surgical instruments. Based on the properties of platinum-iron nanoparticles and the similarity of palladium to its platinum family, palladium-iron nanoparticles may have the desired effects and properties.
[0003] Current methods for synthesizing this material include one-pot aqueous phase synthesis (Fu, W.; Zhang, Z.; Zhuang, P.; Shen, J.; Ye, M.). J. Colloid Interface Sci. 2017, 497, 83.), coprecipitation method (Hasan, K.; Shehadi, IA; Joseph, RG; Patole, SP; Elgamouz, A.). ACS Omega 2023, 8, 23901.), polymer coating (Guo, H.; Zheng, R.; Jiang, H.; Xu, Z.; Xia, A.). BMC Chem. 2019, 13, 130.), surface functionalization modification (Sayahi, MH; Serajian, A.; Bahadorikhalili, S.; Mahdavi, M.). Sci. Rep.2024, 14, 26325.), Biosynthetic methods (Xie, W.; Qi, Y.; Qian, H.; Wu, C.). Mod. Chem. Ind. 2020, 40, 77.), Impregnation reduction method (Beheshti, S.; Motavalizadehkakhky, A.; Zhiani, R.; Nouri, SMM; Zahedi, E.). Sci. Rep. 2024, 14, 11969.), Core-shell structure design (Watt, J.; Kotula, PG; Huber, DL) Chempluschem 2017, 82, 347.), supramolecular assembly (Kuchkina, NV; Haskell, AK; Sorokina, SA; Torozova, AS; Nikoshvili, LZ; Sulman, EM; Stein, BD; Morgan, DG; Bronstein, LM; Shifrina, ZB) ACS Appl. Mater. Interfaces 2020, 12, 22170.), Magnetic composite carriers (Dong, Y.; Yang, J.; Zhang, J.; Wei, Q.; Lv, C.; Jiang, Y.; Shi, X.; Zhou, Z.; Jia, X.; Hu, Z.; Zhang, W.; Li, X.). Int. J. Biol. Macromol. (e.g., 2024, 279, 135386.), but these methods require additional ligands, linkers, reducing agents, precursors, or special process techniques. Summary of the Invention
[0004] This invention requires no additional additives or special processes, and is a simple, low-cost, and effective method for preparing magnetic metal composite materials.
[0005] The technical solution of the present invention is achieved through the following technical measures: a novel method for preparing magnetic metal composite material, characterized by comprising the following steps: (1) stirring iron(III) oxide in a solvent under ultrasonic conditions for half an hour; (2) adding iron pentacarbonyl and palladium compounds to the above reaction solution; (3) sealing the above reaction system and stirring at 80°C for 2 hours; (4) opening the above sealed reaction system, cooling to room temperature, and stirring for 2 hours; (5) centrifuging the above reaction solution to obtain a black metallic solid, washing and vacuum drying to obtain a black metallic powder, which is the magnetic palladium-iron composite material loaded on iron(III) oxide.
[0006] Preferably, the solvent in step (1) includes, but is not limited to, water, ethanol, acetonitrile, toluene, etc., and the iron(III) oxide is not limited to spherical nanomaterials. The palladium compound in step (2) includes, but is not limited to, palladium chloride, palladium nitrate, palladium sulfate, palladium acetate, bis(dibenzylacetone)palladium, bis(acetonitrile)palladium dichloride, etc., with a concentration of iron pentacarbonyl of 1~10 mmol / L and a concentration of palladium compound of 0.1~1 mmol / L. The molar ratio of Pd to all Fe elements in steps (1) and (2) is (0.01~0.1). In step (5), the material is washed 3~4 times with anhydrous ethanol, and the vacuum drying temperature is 80℃~100℃. Additional ligands, linkers, reducing agents, precursors, or special process technologies are required. Attached Figure Description
[0007] The invention will be further illustrated with reference to the accompanying drawings, but the embodiments in the drawings do not constitute any limitation on the invention.
[0008] Figure 1 This is a TEM image of the product obtained in Example 1 of the present invention.
[0009] Figure 2 The results are EDS characterization results of the product obtained in Example 1 of this invention.
[0010] The invention will be further illustrated with reference to the accompanying drawings, but the embodiments in the drawings do not constitute any limitation on the invention. Specific Implementation Cases
[0011] To make the present invention easier to understand, specific embodiments of the present invention will be further described below.
[0012] Implementation Case 1. 100 mL of toluene was added as solvent to a round-bottom flask, followed by 100 mg of spherical iron(III) oxide powder. After ultrasonic dispersion for half an hour, 0.17 mmol of iron pentacarbonyl and 0.027 mmol of palladium acetate were added. The flask was sealed and heated to 80 °C for 2 hours. The flask was then opened, and the reaction was allowed to continue for another 2 hours. Centrifugation yielded a black powder, which was washed 3-4 times with anhydrous ethanol and then vacuum dried at 80 °C for 24 hours to obtain a black metallic-luster powder, which is the palladium-iron nanomaterial supported on iron(III) oxide. The obtained product was characterized by TEM and EDS, and the results are as follows: Figure 1 and 2 As shown, the synthesized nanomaterials exhibit good dispersibility, uniform particle size, and are mostly distributed in the range of 2-3 nm.
[0013] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.
Claims
1. A method for preparing magnetic metal composite nanomaterials, characterized in that, Includes the following steps: (1) Stir the iron(III) oxide in a solvent under ultrasonication for half an hour; (2) Add pentacarbonyl iron and palladium compounds to the above reaction solution; (3) Seal the above reaction system and stir at 80°C for 2 hours; (4) Open the above closed reaction system, cool it to room temperature, and stir for 2 hours; (5) Centrifuge the above reaction solution to obtain a black metallic solid, wash and vacuum dry to obtain a black metallic powder.
2. The method for preparing a novel magnetic metal composite material according to claim 1, characterized in that, The solvents used in step (1) include, but are not limited to, water, ethanol, acetonitrile, toluene, etc.
3. The method for preparing a novel magnetic metal composite material according to claim 1, characterized in that, In step (1), iron(III) oxide is a spherical nanomaterial.
4. The method for preparing a novel magnetic metal composite material according to claim 1, characterized in that, The palladium compounds in step (2) include, but are not limited to, palladium chloride, palladium nitrate, palladium sulfate, palladium acetate, bis(dibenzylideneacetone)palladium, bis(acetonitrile)palladium dichloride, etc.
5. The method for preparing a novel magnetic metal composite material according to claim 1, characterized in that, In step (2), the concentration of iron pentacarbonyl is 1~10 mmol / L and the concentration of palladium compound is 0.1~1 mmol / L.
6. The method for preparing a novel magnetic metal composite material according to claim 1, characterized in that, The molar ratio of Pd to all Fe elements in steps (1) and (2) is (0.01~0.1).
7. The method for preparing a novel magnetic metal composite material according to claim 1, characterized in that, In step (5), wash with anhydrous ethanol 3 to 4 times.
8. The method for preparing a novel magnetic metal composite material according to claim 1, characterized in that, In step (5), the vacuum drying temperature is 80℃~100℃.