Preparation method of double-layer Fe3O4@SiO2 magnetic composite nanoparticle

A magnetic composite nanometer and ferroferric oxide technology, which is applied in the direction of iron oxide/hydroxide, silicon dioxide, silicon oxide, etc., can solve the problems of difficult disposal of waste liquid, high processing cost, and easy pollution of the environment. The effect of dense silicon oxide structure, uniform particle size and good dispersion

Inactive Publication Date: 2019-11-15
TIANJIN UNIV
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Problems solved by technology

For example, the patent CN201310631784.3 uses the inverse microemulsion method to prepare ferric oxide@silicon dioxide composite nanoparticles, but because the waste liquid is not easy to handle, it is easy to pollute the environment, and the treatment cost is high; in the patent CN201710875704. The mass ratio of tetraethyl orthosilicate is (1.5-4): 1, react at 100-150°C for 5-15h to obtain ferric oxide@silicon dioxide composite nanoparticles, but there are poor dispersion and particles Disadvantages of unevenness

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  • Preparation method of double-layer Fe3O4@SiO2 magnetic composite nanoparticle
  • Preparation method of double-layer Fe3O4@SiO2 magnetic composite nanoparticle
  • Preparation method of double-layer Fe3O4@SiO2 magnetic composite nanoparticle

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[0028] The preparation method of the double-layer ferroferric oxide@silicon dioxide magnetic composite nano-particles of the present invention obtains double-layer ferric oxide@silicon dioxide magnetic composite nanoparticles with a dense structure and good monodispersity through a large number of experimental investigations , including the following steps:

[0029] Step 1: Disperse iron ferric oxide nanoparticles in trisodium citrate, heat treatment in a water bath at 80°C for 1 hour, then alternately wash with acetone and deionized water, and dry in vacuum at 30°C for 24 hours to obtain treated ferric iron tetroxide particles .

[0030] Wherein, the particle diameter of ferric oxide nanoparticles is 20nm. The concentration of the trisodium citrate is 0.1mol / L, the volume is 200ml, and the ratio of acetone and deionized water is 1:3. The volume fraction of acetone is 99.5%.

[0031] Step 2: Weigh the iron ferric oxide particles obtained in step 1, ultrasonically disperse t...

Embodiment 1

[0036] Step 1: Disperse 0.5g of 20nm spherical ferric ferric oxide in 200ml of 0.1mol / l trisodium citrate, bathe in water at 80°C for 1 hour, wash alternately with acetone and deionized water, the ratio of acetone to deionized water is 1:3, and dried in a vacuum oven at 30°C for 24 hours to obtain the treated ferric oxide particles.

[0037] Step 2: Weigh 0.5 g of ferric oxide particles treated in Step 1, disperse them in 200 ml of ethanol, and ultrasonicate for 15 min. Then add 100ml of water and 0.2ml of ammonia water, under the stirring condition of 1200r / min at 20°C, add 25ml of ethanol solution dissolved in 0.3ml of tetraethyl orthosilicate to the above solution at a speed of 1ml / min, and react for 4h to obtain a single layer The SiO2-coated Fe3O4@SiO2 composite was washed alternately with deionized water and ethanol several times, and the ratio of deionized water to ethanol was 2:1.

[0038] Step 3: Ultrasonic disperse the Fe3O4@Silicon Dioxide composite material treate...

Embodiment 2

[0040] Step 1: Disperse 0.5g of 20nm spherical ferric ferric oxide in 200ml of 0.1mol / l trisodium citrate, bathe in water at 80°C for 1h, wash alternately with acetone and deionized water, the ratio of acetone to water is 1: 3. Drying in a vacuum oven at 30° C. for 24 hours to obtain treated ferric oxide particles.

[0041]Step 2: Weigh 0.5 g of ferric oxide particles treated in Step 1, disperse them in 200 ml of ethanol, and ultrasonicate for 15 min. Then add 100ml of water and 0.3ml of ammonia water, under the stirring condition of 1200r / min at 60°C, add 25ml of ethanol solution dissolved in 0.5ml of tetraethyl orthosilicate to the above solution at a speed of 1ml / min, and react for 4h to obtain a single layer The SiO2-coated Fe3O4@SiO2 composite was washed alternately with deionized water and ethanol several times, with the ratio of deionized water to ethanol being 2:1, until the solution was neutral and clear.

[0042] Step 3: Ultrasonic disperse the Fe3O4@Silicon Dioxide...

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Abstract

The invention discloses a preparation method of double-layer Fe3O4@SiO2 magnetic composite nanoparticle. The ferrosoferric oxide nanoparticle is dispersed in trisodium citrate, treated in water bath,washed alternately with acetone and deionized water, and dried in vacuum to obtain ferric oxide particles; Fe3O4 particles are weighed and dispersed in ethanol solution, ethyl orthosilicate, ammonia water and water are added and react in a homogeneous reactor for 4 h to obtain a single-layer coated Fe3O4@SiO2 composite; the Fe3O4@SiO2 composite material is dispersed in ethyl alcohol, hexadecyl trimethyl ammonium bromide, ethyl orthosilicate, ammonia water and water are added and the raw materials react for 6 h in a homogeneous reactor, so as to obtain the double-layer coated Fe3O4@SiO2 magnetic composite nanoparticle. The invention adopts an improved Stober method to prepare double-layer Fe3O4@SiO2 magnetic composite nanoparticles, which have compact particle structure and good monodispersity.

Description

technical field [0001] The invention belongs to the field of environmental materials, and more specifically relates to a method for preparing a double-layer ferric oxide@silicon dioxide magnetic composite nanoparticle. Background technique [0002] In recent years, nanoparticles have played an important role in the progress of people's industry, agriculture, medicine and the environment. Ferroferric oxide nanoparticles have superparamagnetism and can be quickly separated from liquids under the action of an external electric field. Silica can shield the dipole interaction between particles and prevent particle aggregation, and it has good biocompatibility and affinity. Waterborne and good stability. Because the molecular force between the ferroferric oxide particles will make the particles reunite, trisodium citrate can be grafted on the surface of ferric oxide, so that the particles have good dispersion; the porous structure of the outer silica layer and the larger The spe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08C01B33/18B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B33/18C01G49/08C01P2004/84
Inventor 赵亚君赵鹏王紫璇
Owner TIANJIN UNIV
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