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Gamma-Fe2O3/SiO2 nano-grade composite material preparation method, and nano-grade composite material particles

A nano-composite material and nano-particle technology is applied in the field of metal oxide composite materials to achieve the effect of strong magnetic reaction effect

Inactive Publication Date: 2013-09-25
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, there is no preparation of γ-Fe with a spherical shell structure 2 o 3 / SiO 2 Reports on nanocomposites

Method used

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  • Gamma-Fe2O3/SiO2 nano-grade composite material preparation method, and nano-grade composite material particles
  • Gamma-Fe2O3/SiO2 nano-grade composite material preparation method, and nano-grade composite material particles
  • Gamma-Fe2O3/SiO2 nano-grade composite material preparation method, and nano-grade composite material particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] γ-Fe 2 o 3 / SiO 2 The preparation method of the nanocomposite specifically includes the following three steps.

[0038] The first step is to synthesize γ-Fe by high temperature liquid phase method 2 o 3 Nanoparticles;

[0039] A mixture of 1.44mL octadecenoic acid (pure solution) and 10mL octyl ether (pure solution) was heated at 100°C for 30min under argon protection; then 0.2mL Fe(CO) 5 Octyl ether solution (wherein Fe(CO) 5 Concentration of 0.34g / ml) was quickly added to the above mixture, reacted at 295°C for 60min; finally cooled to 200°C, passed air into the system for 2h, cooled to room temperature, washed three times with ethanol and cyclohexane respectively, and then The synthesized γ-Fe 2 o 3 Nanoparticles were dispersed into 5mL of cyclohexane, ready to use. γ-Fe taken by transmission electron microscope 2 o 3 Photos of nanoparticles such as figure 1 shown.

[0040] In the second step, the γ-Fe 2 o 3 Nanoparticles are transferred from the oil p...

Embodiment 2

[0046] Heat the mixture of 1mL octadecenoic acid (pure solution) and 10mL octyl ether (pure solution) at 100°C for 30min under the protection of argon; then add 0.5mL Fe(CO) 5 Octyl ether solution (wherein Fe(CO) 5 Concentration of 0.34g / ml) was quickly added to the above mixture, reacted at 290°C for 70min; finally cooled to 200°C, passed air into the system for 2h, cooled to room temperature, washed three times with ethanol and cyclohexane respectively, and then The synthesized γ-Fe 2 o 3 Nanoparticles were dispersed into 5mL of cyclohexane, ready to use.

[0047] 78 mg sodium lauryl sulfate, 10 mL deionized water, 280 μL dispersed with γ-Fe 2 o 3 Nanoparticles of cyclohexane, mixed with 620 μL cyclohexane, ultrasonically assisted for 8 minutes, then kept at 70°C for 4 hours, and finally cleaned by centrifugation. The cleaning solvent was deionized water. After three times of cleaning, γ-Fe 2 o 3 clusters and disperse them in 1 mL of deionized water for later use.

[...

Embodiment 3

[0050] Heat the mixture of 1mL octadecenoic acid (pure solution) and 12mL octyl ether (pure solution) at 100°C for 30min under the protection of argon; then add 0.1mL Fe(CO) 5 Octyl ether solution (wherein Fe(CO) 5 Concentration of 0.34g / ml) was quickly added to the above mixture, reacted at 295°C for 60min; finally cooled to 200°C, passed air into the system for 2h, cooled to room temperature, washed three times with ethanol and cyclohexane respectively, and then The synthesized γ-Fe 2 o 3 Nanoparticles were dispersed into 5mL of cyclohexane, ready to use.

[0051] 50 mg sodium lauryl sulfate, 10 mL deionized water, 350 μL dispersed with γ-Fe 2 o 3 Nanoparticles of cyclohexane, mixed with 600 μL cyclohexane, ultrasonically assisted for 8 minutes, then kept at 70°C for 4 hours, and finally cleaned by centrifugation. The cleaning solvent was deionized water. After three times of cleaning, γ-Fe 2 o 3 clusters and disperse them in 1 mL of deionized water for later use.

[...

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Abstract

The invention discloses a gamma-Fe2O3 / SiO2 nano-grade composite material preparation method, and nano-grade composite material particles. The method comprises the steps that: a mixed liquid of octadecenoic acid and octyl ether with a volume ratio of 1:6-15 is heated; a Fe(CO)5 octyl ether solution is added, wherein a molar ratio of Fe(CO)5 to octadecenoic acid is 0.03-0.3:1; the mixture is heated, and a reaction is carried out, such that Fe2O3 nano-grade particles are obtained; the particles are dispersed in cyclohexane; gamma-Fe2O3 nano-grade particles dispersed in cyclohexane are mixed with a sodium dodecyl sulfate water solution and cyclohexane; an ultrasonic treatment is carried out, such that gamma-Fe2O3 clusters are assembled; the clusters are dispersed in a water phase; the dispersed gamma-Fe2O3 clusters are dissolved in a mixed solution of deionized water, ammonia water, and anhydrous ethanol; and tetraethyl orthosilicate is added, such that the gamma-Fe2O3 / SiO2 nano-grade composite material is obtained. A molar ratio of tetraethyl orthosilicate to Fe(CO)5 is 3-10:1. The gamma-Fe2O3 / SiO2 nano-grade composite material particles provided by the invention have kiwi shapes, and have strong magnetism response and fast solid-liquid separation effect. Therefore, a magnetic separation material can be provided in fields such as water treatment, catalytic oxidation, and the like.

Description

technical field [0001] The invention belongs to the field of metal oxide composite materials, in particular to a gamma-Fe 2 o 3 / SiO 2 Preparation method of nanocomposite material and nanocomposite material particle. Background technique [0002] In the past few decades, micro-nano structures with nanometer size, such as nanotubes, nanofibers, nanorods, dendritic structures, hollow sphere structures, core-shell structures, flower structures, bridge structures, tower structures, etc. The special physical and chemical properties produced by the structural effect and nano-size effect have attracted extensive attention from researchers at home and abroad, and it is also a hot spot and focus in the field of preparation of inorganic micro-nano materials. Relevant reports at home and abroad pointed out that ZnO, MgO, TiO have been successfully prepared 2 , CuO, Fe 2 o 3 and Fe 3 o 4 Some important and common metal oxide micro-nano structures were characterized, and their co...

Claims

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Application Information

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IPC IPC(8): B01J13/02C01G49/06H01F1/11
Inventor 叶苗苗张土乔张仪萍刘小为邵煜
Owner ZHEJIANG UNIV
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