Synthetic method of hydrophilic monodisperse carboxyl superparamagnetic microsphere

A synthesis method and monodisperse technology, which is applied in the field of synthesis of hydrophilic monodisperse carboxyl superparamagnetic microspheres, can solve the problems that are not conducive to biomedical applications, the surface has not been functionalized, and the dispersion stability is not good. The effect of expanding application, stable product quality and low equipment requirements

Inactive Publication Date: 2009-01-28
SHANGHAI JIAO TONG UNIV
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Problems solved by technology

In the Chinese patent application with the application number 200410009788.9 and the title of the invention "a method for synthesizing a series of monodisperse ferrite nano-magnetic beads", it is proposed to use ferric chloride hydrate as the iron source and ethylene glycol as the solvent to conduct a closed reaction The method of preparing superparamagnetic microspheres by high-temperature solvothermal method in a container is easy to operate, but due to the weak alkalinity in the reaction system and the slow hydrolysis of iron salt, the preparation time of microspheres is long, and it takes 8 to 72 hours to react. Finish
Moreover, the surface of the obtained microspheres is adsorbed by ethylene glycol, the dispersion stability in the water phase is not good, the surface has not been functionalized, and it is not conducive to downstream biomedical applications.

Method used

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  • Synthetic method of hydrophilic monodisperse carboxyl superparamagnetic microsphere

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: take ferric chloride as iron source, citric acid is carboxylation reagent, prepares hydrophilic monodisperse carboxylation nanometer Fe 3 o 4 superparamagnetic microspheres

[0018] 5mmol of anhydrous ferric chloride, 3mmol of citric acid, 500 microliters of water and 20mmol of urea were dissolved in 20ml of ethylene glycol solvent, and the mixed solution was placed in a 30ml hydrothermal kettle, heated at 200°C for 6 hours, and the obtained black precipitate was washed with ethanol Washed with deionized water for 3 times, and dried at 45°C to obtain nano-Fe with a particle size of about 200nm and surface small molecule carboxylic acid modification 3 o 4 Superparamagnetic microspheres.

Embodiment 2

[0019] Embodiment 2: take ferric sulfate as iron source, sodium citrate is carboxylation reagent, prepares monodisperse carboxylation nanometer Fe in ethylene glycol 3 o 4 superparamagnetic microspheres

[0020] 1mmol ferric sulfate dodecahydrate, 1mmol sodium tartrate, 100 microliters of water and 8mmol urea were dissolved in 20ml of ethylene glycol solvent, the mixed solution was placed in a 30ml hydrothermal kettle, and heated at 200°C for 8 hours, and the obtained black precipitate was washed with ethanol Washed with deionized water for 3 times, and dried at 40°C to obtain hydrophilic monodisperse carboxylated nano-Fe with a particle size of about 50nm 3 o 4 Superparamagnetic microspheres.

Embodiment 3

[0021] Embodiment 3: With iron acetate as iron source, succinic acid is carboxylation reagent, prepares hydrophilic monodisperse carboxylation nanometer Fe 3 o 4 superparamagnetic microspheres

[0022] 2mmol iron acetate, 1mmol succinic acid, 60 microliters of water and 20mmol of urea were dissolved in 20ml of ethylene glycol solvent, and the mixed solution was placed in a 30ml hydrothermal kettle and heated at 160°C for 10 hours. Washed with ion water for 3 times, and dried at 40°C to obtain nano-Fe with a particle size of about 300nm and surface small molecule carboxylic acid modification. 3 o 4 Superparamagnetic microspheres.

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Abstract

A method for synthesizing a hydrophilic monodisperse carboxyl super paramagnetic microsphere belongs to the inorganic chemistry field. In the invention, soluble iron ion salt, urea, water and carboxylic acid or carboxylate are taken as raw materials, dissolved in ethylene glycol and made into nano-ferroferric oxide super paramagnetic microsphere with carboxylated surface by reduction reaction with polyol at the temperature of 160-250 DEG C, and a series of magnetic microspheres with different diameters and densities of surface carboxyl groups are obtained by controlling reaction parameters. The surface carboxylated microsphere obtained by the method is characterized by uniform size, dispersion stability with a great pH range, high specific saturation magnetization and the like; the raw materials are nontoxic, environmental friendly, cheap; and the method has simple operation, low equipment requirements, high yield, and is applicable to large-scale industrialized production. The application of the bead to the biomedical field can be further expanded by inorganic or polymer surface coating of the super paramagnetic microsphere, on the basis of the bead.

Description

technical field [0001] The invention relates to a synthesis method in the field of inorganic chemistry, in particular to a synthesis method of hydrophilic monodisperse carboxyl superparamagnetic microspheres. technical background [0002] Nano-superparamagnetic materials are widely used in industrial fields such as magnetic recording materials and electromagnetic induction devices due to their superior properties. Due to the advantages of non-toxic, metabolizable in vivo, and good manipulation performance under magnetic field, nano-superparamagnetic ferrite materials have been widely used in the field of biomedicine in recent years, such as biological separation and purification, tumor magnetic hyperthermia, Targeted drug loading and magnetic resonance imaging and other fields. Generally speaking, nano-superparamagnetic materials suitable for the biomedical field must have the characteristics of surface hydrophilicity, stable dispersion in the aqueous phase, good biocompati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08
Inventor 古宏晨程昌明文颖慧
Owner SHANGHAI JIAO TONG UNIV
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