Method of manufacturing superparamagnetic nanocomposite and superparamagnetic nanocomposite manufactured using the same

Patent metadata

Field	Value
Publication number	US-10658097-B2
Application number	US-201715562303-A
Country	US
Kind code	B2
Filing date	Aug 11, 2017
Priority date	Aug 19, 2016
Publication date	May 19, 2020
Grant date	May 19, 2020

Abstract

The present invention relates to a method of manufacturing a superparamagnetic nanocomposite and a superparamagnetic nanocomposite manufactured using the same, and more particularly to a method of manufacturing a superparamagnetic nanocomposite suitable for use in magnetic separation for the detection of a target biomaterial and a superparamagnetic nanocomposite manufactured using the same. The method of manufacturing the superparamagnetic nanocomposite according to the present invention has a higher yield and a high rate without complicated processing than a conventional method of manufacturing a magnetic nanoparticle for magnetic separation and is capable of mass production of the superparamagnetic nanocomposite having excellent properties with uniform size and particle size distribution, high aqueous solution dispersibility and high magnetization and being capable of maintaining superparamagnetism.

First claim

The invention claimed is:

1. A method of manufacturing a superparamagnetic nanocomposite, comprising:
mixing an iron precursor, a solvent, a stabilizing agent and a reducing agent;
subjecting a mixed solution in the mixing step to hydrothermal synthesis at a temperature of 150 to 300° C. and a pressure of 1.5 to 10 bar to synthesize a superparamagnetic nanocomposite in a nanocluster form; and
separating the synthesized superparamagnetic nanocomposite,
wherein the stabilizing agent is a compound having a carboxyl group,
wherein the superparamagnetic nanocomposite comprises a magnetic nanocrystal having a diameter of from more than 0 to 10 nm, wherein a surface of the magnetic nanocrystal is stabilized by carboxylate (COO − ) group, and wherein the superparamagnetic nanocomposite has a plurality of magnetic nanocrystals clustered therein, has a nanoclustered shape having a diameter of 100 nm to 450 nm and has hydrophilicity so as to be dispersed in an aqueous solution.

2. The method of claim 1 , further comprising washing the separated superparamagnetic nanocomposite with a polar solvent.

3. The method of claim 1 , wherein the superparamagnetic nanocomposite in the nanocluster form is synthesized by subjecting the mixed solution to hydrothermal synthesis at a temperature of 200 to 240° C. and a pressure of 1.5 to 6 bar.

4. The method of claim 1 , wherein the iron precursor is selected from the group consisting of ferric chloride hexahydrate (FeCl 3 .6H 2 O), ferrous chloride, ferrous chloride tetrahydrate, ferric chloride, and ferric nitrate nonahydrate (Fe(NO 3 ) 3 .9H 2 O).

5. The method of claim 1 , wherein the solvent is selected from the group consisting of ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, dipropylene glycol, and glycerol.

6. The method of claim 1 , wherein the stabilizing agent is selected from the group consisting of trisodium citrate dihydrate (HOC(COONa)(CH 2 COONa) 2 .2H 2 O; C 6 H 5 Na 3 O 7 ) and dicarboxyl poly(ethylene glycol) having a molecular weight of 500 to 50,000.

7. The method of claim 1 , wherein the reducing agent is selected from the group consisting of sodium acetate, sodium acrylate, urea, sodium formate, and ammonium acetate.

8. The method of claim 1 , wherein the iron precursor and the solvent are mixed at a molar ratio of 1:10 to 1:300.

9. The method of claim 1 , wherein the iron precursor and the stabilizing agent are mixed at a molar ratio of 1:0.0000013 to 1:1.

10. The method of claim 1 , wherein the iron precursor and the reducing agent are mixed at a molar ratio of 1:1 to 1:20.

11. The method of claim 2 , wherein the polar solvent is selected from the group consisting of ethanol, water, methanol, acetone, liquid ammonia, ethyl acetate, ether, tetrahydrofuran, potassium hydroxide, sodium hydroxide, and dichloromethane.

12. The method of claim 2 , wherein the washing the separated superparamagnetic nanocomposite with the polar solvent comprises washing the separated superparamagnetic nanocomposite with an ethanol solvent and washing the superparamagnetic nanocomposite, washed with the ethanol solvent, with a water solvent.

13. The method of claim 1 , wherein dispersibility of the superparamagnetic nanocomposite in an aqueous solution is adjusted using a carboxylate (COO − ) group of the stabilizing agent.

Assignees

• Amolifescience Co Ltd
• Nat Univ Pusan Ind Univ Coop Found

Inventors

• Kim Sung-Il
• Choi Min-Young
• Lee Myoung-Yeol
• Lee Jae-Beom
• Tran Van Tan
• Kim Jeong-Hyo
• Oh Sang-Jin

Classifications

• H01F1/20

  in the form of particles, e.g. powder (H01F1/147 takes precedence) · CPC title

• H01F41/0246 Primary

  Manufacturing of magnetic circuits by moulding or by pressing powder (magnetic cores made by moulding or by pressing powder H01F27/255; soft magnetic particles H01F1/20, H01F1/36) · CPC title

• B82B1/008

  Nanostructures not provided for in groups B82B1/001 - B82B1/007 · CPC title

• H01F1/0054

  Coated nanoparticles, e.g. nanoparticles coated with organic surfactant · CPC title

• C01P2006/22

  Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability · CPC title