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CN-121972675-A - Preparation method of magnetic metal composite nano material

CN121972675ACN 121972675 ACN121972675 ACN 121972675ACN-121972675-A

Abstract

A preparation method of a magnetic metal composite nano material. The invention relates to a preparation method of a metal palladium iron nano material. Adding solvent (water, ethanol, acetonitrile, toluene and the like) into spherical nano ferroferric oxide powder, carrying out ultrasonic reaction for half an hour, adding pentacarbonyl iron (1-10 mmol/L) and palladium compound (0.1-1 mmol/L), palladium chloride, palladium nitrate, palladium sulfate, palladium acetate, bis (dibenzylideneacetone) palladium, bis (acetonitrile) palladium dichloride and the like, wherein the ratio of the palladium element to the substances of all iron elements is 0.01-0.1, sealing the reaction vessel, reacting for 2 hours at 80 ℃, opening the reaction vessel, cooling to room temperature, continuing to react for 2 hours, centrifuging the obtained reaction solution to obtain brown solid, washing and vacuum drying the obtained black solid to obtain black powder, namely the palladium-iron composite nanomaterial loaded on the spherical ferroferric oxide. The composite material obtained by the method has good dispersibility, uniform particle size and concentrated size distribution of 2-3 nm.

Inventors

  • ZHU ZHUANGLI
  • SU QIUSHI

Assignees

  • 天津师范大学
  • 朱壮丽

Dates

Publication Date
20260505
Application Date
20260225

Claims (8)

  1. 1. The preparation method of the magnetic metal composite nano material is characterized by comprising the following steps of: (1) Stirring ferroferric oxide in solvent in ultrasonic for half an hour; (2) Adding pentacarbonyl iron and palladium compound into the reaction liquid; (3) Sealing the reaction system, stirring for 2h at 80 ℃; (4) Opening the closed reaction system, cooling to room temperature, and stirring for 2h; (5) And centrifuging the reaction liquid to obtain a black metal luster solid, washing and vacuum drying to obtain black metal luster powder.
  2. 2. The method of claim 1, wherein the solvent in step (1) includes, but is not limited to, water, ethanol, acetonitrile, toluene, etc.
  3. 3. The method for preparing a novel magnetic metal composite material according to claim 1, wherein the ferroferric oxide in the step (1) is a spherical nanomaterial.
  4. 4. The method of claim 1, wherein the palladium compound in step (2) includes, but is not limited to, palladium chloride, palladium nitrate, palladium sulfate, palladium acetate, bis (dibenzylideneacetone) palladium, bis (acetonitrile) palladium dichloride, and the like.
  5. 5. The method for preparing a novel magnetic metal composite material according to claim 1, wherein the concentration of iron pentacarbonyl in the step (2) is 1-10 mmol/L, and the concentration of palladium compound is 0.1-1 mmol/L.
  6. 6. The method for preparing a novel magnetic metal composite material according to claim 1, wherein the mass ratio of Pd element to all Fe elements in the steps (1) and (2) is (0.01 to 0.1).
  7. 7. The method for preparing a novel magnetic metal composite material according to claim 1, wherein the step (5) is performed by washing 3-4 times with absolute ethyl alcohol.
  8. 8. The method for preparing a novel magnetic metal composite material according to claim 1, wherein the vacuum drying temperature in the step (5) is 80-100 ℃.

Description

Preparation method of magnetic metal composite nano material Technical Field The invention relates to the technical field of preparation of magnetic metal composite materials, in particular to a preparation method of a metal palladium iron nano material loaded on ferroferric oxide. Background The nanomaterial is a material having at least one dimension in a three-dimensional space in a nano-size (0.1 to 100 nm) or composed of them as a basic unit, which corresponds to a size of about 10 to 100 atoms closely arranged together. The size of the structural unit of the material is 0.1-100 nm, and the property of the structural unit of the material is greatly changed due to self-organization brought by strong coherence because the size of the structural unit is close to the coherence length of electrons. In addition, the dimensions are close to the wavelength of the light, plus the special effect that it has a large surface, so that the characteristics exhibited by nanomaterials, such as melting point, magnetism, optics, thermal conductivity, electrical conductivity, etc., tend to differ from the properties exhibited by the substance in its bulk state. Metal nanomaterials are an important branch of nanomaterials, and metal nanoparticles exhibit superior properties that many bulk materials do not possess, and are applicable in many fields. Palladium is a member of the group VIII platinum group elements, silver-white transition metals. The alloy is softer, has good ductility and plasticity, can be forged, rolled and drawn, is an indispensable key material in the high-tech fields such as aerospace and the like and the automobile manufacturing industry, is an important catalyst in the chemical field, and is also palladium in some dental materials, raw materials of watches, surgical instruments and the like. Palladium iron nanoparticles may have desirable effects and characteristics based on their performance characteristics, as well as the relatively close nature of palladium and platinum families. Current methods of synthesizing such materials include one pot aqueous phase synthesis (Fu, w.; zhang, z.; zhuang, p.; shan, j.; ye, m.j. Colloid Interface sci.2017, 497, 83.), coprecipitation (Hasan, k.; shehadi, i.a.; joseph, r.g.; patole, s.p.; elgamouz, a. ACS Omega 2023, 8, 23901.), polymer coating (Guo, h.; zheng, r.; jiang, h.; xu, z.; xia, a.bmc chem.2019, 13, 130.; magnetic support structures are required for the assembly of the support, but the methods require additional magnetic support structures for the support, the magnetic support, etc. (Sayahi, m.h.; serajian, a.; bahadorikhalili, s.; mahdavi, m.sci.rep.2024, 14, 26325.; biosynthesis (Xie, w.; qi.; y.; qian, h.; wu, c.chem, chem, industrial support, 77, d.; core, 37, d.; magnetic support, d.; 35, 37, 35, 37. 35, 35.g.; magnetic support, 35). Disclosure of Invention The invention does not need extra additives or special process, and is a simple and feasible technical method for preparing the magnetic metal composite material with low cost and good loading effect. The technical scheme of the invention is realized by the following technical measures that the preparation method of the novel magnetic metal composite material is characterized by comprising the following steps of (1) stirring ferroferric oxide in a solvent for half an hour in an ultrasonic manner, (2) adding pentacarbonyl iron and a palladium compound into the reaction liquid, (3) sealing the reaction system, stirring for 2 hours at 80 ℃, 4) opening the sealed reaction system, cooling to room temperature, stirring for 2 hours, 5) centrifuging the reaction liquid to obtain a black metal luster solid, and washing and then vacuum-drying to obtain black metal luster powder, namely the magnetic palladium iron composite material loaded on the ferroferric oxide. Preferably, the solvent in step (1) includes, but is not limited to, water, ethanol, acetonitrile, toluene, etc., and the ferroferric oxide is not limited to spherical nanomaterial. The palladium compound in the step (2) includes, but is not limited to, palladium chloride, palladium nitrate, palladium sulfate, palladium acetate, bis (dibenzylideneacetone) palladium, bis (acetonitrile) palladium dichloride and the like, wherein the concentration of iron pentacarbonyl is 1-10 mmol/L, and the concentration of the palladium compound is 0.1-1 mmol/L. In the step (1) and (2), the mass ratio of Pd element to all Fe elements is (0.01-0.1). And (5) washing 3-4 times by adopting absolute ethyl alcohol, wherein the vacuum drying temperature is 80-100 ℃. Additional ligands, linkers, reducing agents, precursors or special flow processes are required. Drawings The invention is further illustrated by means of the accompanying drawings, the embodiments in which do not constitute any limitation of the invention. FIG. 1 is a TEM image of the product obtained in example 1 of the present invention. FIG. 2 is a graph showing the EDS characterization of the product ob