Preparation method of mesopore-controllable magnetic microsphere

A magnetic microsphere and mesoporous technology, applied in the direction of ferric oxide, iron oxide/iron hydroxide, etc., can solve the problems of low magnetic response, low crystallinity, small particle size, etc., and achieve high magnetic Responsiveness, good dispersion, and narrow particle size distribution

Inactive Publication Date: 2010-10-20
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of co-precipitation is that magnetic nanoparticles can be prepared in large quantities, but the obtained nanoparticles are often polydisperse, have low crystallinity, small particle size, and low magnetic responsiveness, which is unfavorable for subsequent applications.

Method used

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  • Preparation method of mesopore-controllable magnetic microsphere
  • Preparation method of mesopore-controllable magnetic microsphere
  • Preparation method of mesopore-controllable magnetic microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 16mmol of ferric chloride, 50mmol of ammonium acetate, and 0.5g of polyglutamic acid with a molecular weight of 1000kDa and add it to a 50ml hydrothermal kettle, add 40ml of ethylene glycol solution to the kettle, dissolve it, and heat it at 200°C After 8 hours, the obtained black precipitate was washed with deionized water and dried between 40°C and 80°C to obtain mesoporous ferroferric oxide magnetic microspheres. Figure 1-3 It is the result of characterizing by powder X-ray diffraction, transmission electron microscope and nitrogen adsorption-desorption isotherm curve. The particle size of the microsphere is 436nm, and the specific surface area is 182m 2 / g, the pore volume is 0.65cm 3 / g, the average pore size can be controlled at 5.8nm.

Embodiment 2

[0025] Take 2mmol of ferric chloride, 50mmol of ammonium acetate, and 0.5g of polyglutamic acid with a molecular weight of 1000kDa and add them to a 50ml hydrothermal kettle, add 40ml of ethylene glycol solution to the kettle, dissolve and heat at 250°C After 8 hours, the obtained black precipitate was washed with deionized water and dried between 40°C and 80°C to obtain mesoporous ferroferric oxide magnetic microspheres. The particle size of the microsphere is 49nm, and the specific surface area is 270m 2 / g, the pore volume is 1.35cm 3 / g, the average pore size can be controlled at 2.5nm.

Embodiment 3

[0027] Get 16mmol of ferric nitrate, 50mmol of ammonium acetate, 0.5g of polyglutamic acid with a molecular weight of 1000kDa and add them to a 50ml hydrothermal kettle, add 40ml of ethylene glycol solution to the kettle, after dissolving, heat at 300°C for 8 hours, the obtained black precipitate was washed with deionized water and dried at 40-80° C. to obtain mesoporous ferroferric oxide magnetic microspheres. The particle size of the microsphere is 407nm, and the specific surface area is 210m 2 / g, the pore volume is 0.75cm 3 / g, the average pore size can be controlled at 5.1nm.

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Abstract

The invention belongs to the technical field of inorganic material preparation, relating to a preparation method of a mesopore-controllable magnetic microsphere. The preparation method comprises the following concrete steps: respectively adding soluble ferric ion salts, ammonium acetate and poly glutamic acid into ethylene glycol solution to obtain mixed solution; controlling clarification solution with the concentration of the ferric ion salts of 0.05-0.40mol / L, the concentration of the ammonium acetate of 0.50-4.00mol / L and the concentration of the poly (glutamic acid)of 2.50-50.00g / L in the mixed solution; placing the solution into a closed heating vessel, carrying out a solvent thermal reaction at 200-300DEG C and heating for 8-72 hours; and washing the obtained product with deionized water and drying at 40-80DEG C. The invention provides a novel simple and feasible preparation method capable of batch production. Meanwhile, the invention has the advantages of high magnetic response and specific area, easily-accessible raw materials, favorable repeatability in the preparation process and controllable grain size, specific surface area, pore volume and average pore size of the obtained microspheres.

Description

technical field [0001] The invention belongs to the technical field of inorganic material preparation technology, and in particular relates to a preparation method of mesopore-controllable magnetic microspheres. Background technique [0002] Due to their unique magnetic physical properties, such as the special properties of long-range response to an external magnetic field, the ability to move under the control of an external magnetic field, and the magneto-thermal physical effect under the condition of an external alternating magnetic field, magnetic nanomaterials are widely used in daily life. It has been widely used, such as preparing high-density magnetic storage devices, catalysts, pigments, magnetic fluids, and biodiagnostic related applications. [0003] At present, the method for preparing magnetic nanoparticles is mainly co-precipitation method. The co-precipitation method is to prepare a solution of ferric salt and ferrous salt in a certain ratio, and add lye to c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08
Inventor 汪长春罗彬
Owner FUDAN UNIV
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