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Method for preparing Fe2O3 nano particle with core-shell structure

A nanoparticle and shell structure technology, applied in the field of nanoparticle preparation, can solve problems such as inapplicability, no mention of initiator and detailed reaction process, etc., and achieve the effects of short preparation period, mild reaction conditions, and simple and easy method.

Active Publication Date: 2010-06-09
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the detailed process of the initiator used and the reaction is not mentioned in the above-mentioned patent documents
[0006] Although it has been disclosed in the prior art that the initiator for atom transfer radical polymerization can be a halide, the scope of the halide is very wide, so for those skilled in the art, it is necessary to select a suitable initiator to realize the above reaction creative labor required
Yuan Jinying and others disclosed the method of using ethyl bromoacetate, ethyl α-bromobutyrate, and ethyl α-bromoisobutyrate to initiate atom transfer radical polymerization of styrene in the Journal of Functional Polymer Science 2001 No. 1 However, the above three initiators are not suitable for the atom transfer radical polymerization of N,N-dimethylaminoethyl methacrylate

Method used

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  • Method for preparing Fe2O3 nano particle with core-shell structure
  • Method for preparing Fe2O3 nano particle with core-shell structure
  • Method for preparing Fe2O3 nano particle with core-shell structure

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preparation example Construction

[0040] According to the present invention, for the Fe coated with oleic acid 2 o 3 The preparation method of nanoparticles is not particularly limited, and preparation methods well known to those skilled in the art can be adopted. The present invention preferably uses the method disclosed in Chinese patent document CN101186342, and the preparation process includes steps:

[0041] a1) dissolving iron stearate and oleic acid in toluene at 80°C to 100°C;

[0042] a2) Add the toluene solution of step a1) to the aqueous solution of tert-butylamine and then heat it to 150°C-200°C to react to form Fe wrapped with oleic acid 2 o 3 Nanoparticles.

[0043] The dissolution process of step a1) is preferably carried out under normal pressure, and the molar ratio of stearic acid:oleic acid is 0.1-1:1-10, more preferably 0.2-0.8:2-8, more preferably 0.4-0.7 : 3-7; said oleic acid: toluene is preferably 1-10: 5-50 according to the volume ratio, more preferably 2-8: 5-50, more preferably 2...

Embodiment 1

[0049] Preparation of oleic acid-coated Fe 2 o 3 Nanoparticles:

[0050] Under the condition of 85°C, dissolve 0.2mmol iron stearate and 1mmol oleic acid in 10ml toluene to obtain a red transparent solution; after cooling to room temperature, add the red transparent solution to 10ml tert-butylamine aqueous solution with a volume concentration of 0.25%, and then heat up To 180°C, react under the condition of 0.5MPa pressure for 10 hours to obtain a crude solution, precipitate the crude solution with methanol, centrifuge, and vacuum dry at 80°C to obtain 32mg of oleic acid-coated Fe 2 o 3 Nanoparticles, scanning electron microscope photographs such as figure 1 shown.

Embodiment 2

[0052] Preparation of 2-bromo-2-methylpropionic acid-coated Fe 2 o 3 nano-encapsulated Fe 2 o 3 Nanoparticles;

[0053] Take 32mg of the oleic acid-encapsulated Fe 2 o 3 Nanoparticles were dissolved in 10 g of n-hexane solution, then 30 g of n-hexane solution containing 300 mg of 2-bromo-2-methylpropionic acid was added, and at room temperature, stirred under nitrogen protection in the dark for 72 hours, centrifuged to obtain the crude product, Wash the crude product repeatedly with n-hexane to remove excess 2-bromo-2-methylpropionic acid, and dry it under vacuum at 80°C to obtain 50 mg of 2-bromo-2-methylpropionic acid-coated Fe 2 o 3 Nanoparticles.

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Abstract

The invention discloses a method for preparing Fe2O3 nano particle with a core-shell structure, which is characterized in comprising the steps of: mixing copper salt and ligand, wherein the ligand is tetramethylenediamine, pentamethyl dien, hexamethyl trine, 3 [2-(dimethylkyanamid) ethyl] amine, 3[(2-pyridyl) methyl] amine, 2,2-bipyridyl or 4, 4-dinonyl-2, 2-bipyridyl; adding organic solution of initiator-packed Fe2O3 nano particle into mixture of the copper salt and the ligand, wherein the initiator is 2-bromine-2-methylpropionate; adding methacrylic acid N,N-dimethyl amino ethyl ester (DMAEMA) to obtain reaction raw material liquid; deoxidizing the reaction raw material liquid; and performing a grafting reaction at 20-100 DEG C to obtain Fe2O3 @ PDMAEMA nano particle with the core-shell structure. The experiment results show that the 2-bromine-2-methylpropionate is taken as the initiator so that the PDMAEMA can be successfully grown on the surface of the Fe2O3 nano particle to obtain the Fe2O3 @ PDMAEMA nano particle.

Description

technical field [0001] The invention relates to a method for preparing nanoparticles, in particular to a core-shell structured Fe 2 o 3 Methods for the preparation of nanoparticles. Background technique [0002] Magnetic nanoparticles have been widely used in bio-related fields due to their mesoscopic magnetic properties, such as magnetic resonance imaging, drug release, and rapid bioseparation. In magnetic nanoparticles, Fe 2 o 3 Nanoparticles are the most widely used. [0003] After the surface of nanoparticles is modified with organic ligands to form nanoparticles with core-shell structure, the nanoparticles can be endowed with better surface properties, especially after the formation of polymer ligands on the surface of nanoparticles, the nanoparticles can have good properties. Excellent colloidal stability, processability, biocompatibility and environmental (temperature, pH) responsiveness. At present, the synthesis of nanoparticles stabilized by polymer ligands i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K49/12A61K47/32
Inventor 赵娜娜毛骏聂伟范燕迪李海东刘庆辉姬相玲
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES