Preparation method of superparamagnetic Fe3O4 microspheres

A superparamagnetic, microsphere technology, applied in ferrous oxides, nanotechnology for materials and surface science, nanotechnology, etc., can solve the problems of unfavorable large-scale industrial production, high pressure, and high requirements for reaction equipment. problem, to achieve the effect of short reaction time, simple steps and good repeatability

Inactive Publication Date: 2013-09-04
SANMING UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The publication number is CN101353181A, and the title of the invention is "Synthetic method of hydrophilic monodisperse shuttle-based superparamagnetic microspheres". It is reacted in a high-pressure reactor, ethylene glycol is used as a solvent, and urea is added in the reaction, and urea is heated and decomposed to produce Ammonia, as an alkaline hydrolyzing agent, has too much pressure in the reaction process of this method and requires high reaction equipment, which is not conducive to large-scale industrial production

Method used

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  • Preparation method of superparamagnetic Fe3O4 microspheres
  • Preparation method of superparamagnetic Fe3O4 microspheres
  • Preparation method of superparamagnetic Fe3O4 microspheres

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Experimental program
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Effect test

Embodiment 1

[0025] Use 3-aminopropanol and ethylene glycol as a solvent in a ratio of 1 mL:14 mL, add 0.16 g of anhydrous ferric chloride and 0.14 g of polyacrylic acid with an average molecular weight of 1800, dissolve to form a clear solution, and transfer to high pressure In the reaction kettle, keep the temperature at 200 °C for 6 h, cool with the furnace, add 15 mL of absolute ethanol, precipitate for 10 min, pour off the supernatant, the fixed product has good magnetic response, wash with water 3 times, and dry at 60 °C Superparamagnetic Fe 3 o 4 Microspheres. Electron microscope photos such as figure 1 As shown, the average particle size of the microspheres is 362 nm, the average particle size of the particles composing the microspheres is 3.7 nm, and the saturation magnetization curve at room temperature is shown as Figure 5 Middle curve 1.

Embodiment 2

[0027] Method is changed into 5mL:10 mL with the ratio of embodiment 1,3-aminopropanol and ethylene glycol, and the electron micrograph of gained product is as follows figure 2 As shown, the average particle size of the microspheres is 240 nm, and the average particle size of the particles composing the microspheres is 6.3 nm.

Embodiment 3

[0029] Method is changed into 10mL:5 mL with the ratio of embodiment 1,3-aminopropanol and ethylene glycol, and the electron micrograph of gained product is as follows image 3 As shown, the average particle size of the microspheres is 153 nm, and the average particle size of the particles composing the microspheres is 11.7 nm.

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Abstract

The invention brings forward a controllable technology for preparing superparamagnetic Fe3O4 microspheres by an amino-terminated alcohol and glycol combined double-solvent method. According to the technology, proportions of the two solvents can be changed to adjust the dimension of the microsphres and particle size of particles which form the microspheres. The diameter of the microspheres can be observed through a transmission electron microscope; the particle size of the microspheres can be measured by x-ray diffraction; the microspheres which undergo different surface modifications are prepared by changing a protective agent; surface components can be measured through infrared, zeta potential, thermogravimetry and the like; and magnetic property is measured by a sample vibration magnetometer.

Description

technical field [0001] The present invention relates to superparamagnetic Fe 3 o 4 The invention relates to a controllable preparation technology of microspheres, which belongs to the field of chemical synthesis. Background technique [0002] Magnetic nanomaterials have unique physical and chemical properties and are widely used in environmental governance, separation detection, biomedicine and other fields. Superparamagnetic microspheres are an important class of magnetic nanomaterials. As magnetic carriers, they can be used in the fields of reversible magnetic separation, quantitative immunoassay, and magnetically targeted drug delivery. The particle size, magnetic substance content, and surface functional modification of the microspheres have an important impact on the separation speed and magnetic signal intensity of the magnetic microspheres in the medium. Therefore, the controllable preparation technology of the magnetic microspheres is developed, and the diameter an...

Claims

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Application Information

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IPC IPC(8): C01G49/08B82Y30/00
Inventor 肖旺钏王仁章张启卫王叶敏
Owner SANMING UNIV
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