Preparation method of magnetic iron oxide nanoparticle capable of stably dispersing in water

A magnetic iron oxide and nanoparticle technology, applied in the fields of biomaterials, nanoscience, and material chemistry, can solve the problems of low particle stability and incomplete replacement, and achieve a simple and controllable reaction process

Inactive Publication Date: 2012-06-27
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to prepare biocompatible nanoparticles that are stably dispersed in neutral water, it is necessary to replace organic solvents such as pyrrolidone adsorbed on the surface of iron oxide nanoparticles by replacement reaction, and the replacement is incomplete.
Jiaqi Wan and Wei Cai et al. (Chemical communications, 2007, 5004-5006), and Dipak Maity (Journal of magnetism and magnetic materials, 2009, 321, 3093-3098) et al. used triglycerides, a small organic molecule with good water solubility. Preparation of water-soluble nano-Fe by pyrolysis of iron acetylacetonate in alcohol (TREG) 3 o 4 particles, but the prepared nano-Fe 3 o 4 Particles are not very stable in water
Ricardo H.Goncalves (Journal of Materials Chemistry, 2010, 20, 1167~1172) et al decomposed iron acetylacetonate in PEG with different molecular weights, and prepared water-soluble nano-Fe 3 o 4 particles, but the synthetic nano-Fe 3 o 4 Particles are easy to combine with each other and quickly form precipitates in water

Method used

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  • Preparation method of magnetic iron oxide nanoparticle capable of stably dispersing in water
  • Preparation method of magnetic iron oxide nanoparticle capable of stably dispersing in water
  • Preparation method of magnetic iron oxide nanoparticle capable of stably dispersing in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 15.1 g of PEG (molecular weight: 1000), and add 0.11 g of PEI (molecular weight: 1800). Put the above raw materials into a three-necked flask, place it on a temperature-controlled magnetic stirrer and heat it to 80°C, then add 0.72 g of analytically pure iron acetylacetonate, stir with a magnetic stirrer for 10 minutes, and protect it with flowing argon during the heating process. Then the temperature was raised to 260° C. and heated for 60 minutes, the solution changed from red to black. After stopping the heating, wait for the solution to cool below 60°C, add 60ml of analytically pure toluene, separate the black precipitate by magnetic adsorption, wash twice with analytically pure acetone to remove excess organic matter, and dissolve the precipitate in water. The electrophoretic particle size of the nanoparticles is 28nm. The morphology of the nanoparticles was observed with a transmission electron microscope (TEM). figure 1 It is a transmission electron micro...

Embodiment 2

[0020] 15.3 g of PEG (molecular weight: 1000) was weighed, and 0.31 g of PEI (molecular weight: 1800) was added. Put the above raw materials into a three-necked flask, place it on a temperature-controlled magnetic stirrer and heat it to 80°C, then add 0.72 g of analytically pure iron acetylacetonate, stir with a magnetic stirrer for 10 minutes, and protect it with flowing argon during the heating process. Then the temperature was raised to 260° C. and heated for 60 minutes, the solution changed from red to black. After stopping the heating, wait for the solution to cool below 60°C, add 60ml of analytically pure toluene, separate the black precipitate by magnetic adsorption, wash twice with analytically pure acetone to remove excess organic matter, and dissolve the precipitate in water. The average electrophoretic particle size of the nanoparticles is 27nm. The morphology of the nanoparticles was observed with a transmission electron microscope (TEM). figure 2It is a transmi...

Embodiment 3

[0022] 15.2 g of PEG (molecular weight: 1000) was weighed, and 0.51 g of PEI (molecular weight: 1800) was added. Put the above raw materials into a three-necked flask, place it on a temperature-controlled magnetic stirrer and heat it to 80°C, then add 0.73 g of analytically pure iron acetylacetonate, stir with a magnetic stirrer for 10 minutes, and protect it with flowing argon during the heating process. Then the temperature was raised to 260° C. and heated for 60 minutes, the solution changed from red to black. After stopping the heating, wait for the solution to cool below 60°C, add 60ml of analytically pure toluene, separate the black precipitate by magnetic adsorption, wash twice with analytically pure acetone to remove excess organic matter, and dissolve the precipitate in water. The average electrophoretic particle size of the nanoparticles is 30nm. The morphology of the nanoparticles was observed with a transmission electron microscope (TEM). image 3 It is a transmi...

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Abstract

The invention discloses a preparation method of a magnetic iron oxide nanoparticle capable of stably dispersing in water. The preparation method provided by the invention comprises the following steps of weighing 10 to 30g of triethylene glycol or polyethylene glycol having molecular weight of 600 to 20000 or polyethylene glycol monomethyl ether having molecular weight of 600 to 20000, adding 0.15 to 3g of an additive into the 10 to 30g of triethylene glycol or polyethylene glycol having molecular weight of 600 to 20000 or polyethylene glycol monomethyl ether having molecular weight of 600 to 20000, putting the mixture into a three-neck flask, putting the three-neck flask with the mixture on a temperature-control magnetic stirrer, heating the mixture to a temperature of 70 to 90 DEG C, adding 0.1 to 3g of analytically pure iron acetylacetonate into the mixture, stirring for 5 to 15 minutes by a magnetic stir bar, wherein in heating, flowing argon is fed into the three-neck flask for protection, heating to a temperature of 150 to 320 DEG C, keeping the temperature for 20 to 600 minutes by heating, cooling to a temperature below 60 DEG C, adding 50 to 70ml of analytically pure toluene or acetone into the three-neck flask, carrying out magnet adsorption, washing by analytically pure acetone twice, and dissolving precipitates obtained by the previous step in water to obtain the magnetic iron oxide nanoparticles having sizes of 3 to 50nm. The preparation method provided by the invention has simple processes and is conducive to production. The magnetic iron oxide nanoparticle obtained by the preparation method can be utilized for the fields of biotechnology, medicine, catalysis and mechanical lubrication.

Description

technical field [0001] The technical field of the invention belongs to material chemistry, nanometer science, and biomaterial field, and particularly relates to a preparation method of magnetic iron oxide nanoparticles that can be stably dispersed in water. Background technique [0002] γ-Fe with spinel structure 2 o 3 or Fe in the inverse spinel structure 3 o 4 With paramagnetism, it is subdivided into small-particle iron oxide nanoparticles (SPIO: hydrodynamic particle size approximately 40-180nm) and ultra-small particle iron oxide nanoparticles (USPIO: hydrodynamic particle size) according to the grain size. less than 40nm). USPIO can exhibit superparamagnetism at room temperature, that is, it is magnetized under an external magnetic field, and its remanence is zero or extremely small when the external magnetic field strength is zero. The extremely low remanence of superparamagnetic particles prevents them from aggregating and can be dispersed in solvents. Superpar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08B82Y40/00
Inventor 张宝林赵方圆涂志江冯凌云
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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