Superparamagnetic Fe3O4 nanometer particle with synthetic polymer modification from one-step method

A technology for synthesizing polymers and nanoparticles, which is applied in the treatment of dyed polymer organic compounds and fibrous fillers, etc. It can solve the problems of difficult control of particle size, high viscosity of polymer sol, and non-coating of magnetic nanoparticles to achieve reaction The effects of different kinds of substances are easy to obtain, the method is simple and direct, and there are few kinds of reactants

Inactive Publication Date: 2007-02-07
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the process of coating the polymer, it is necessary to elute or replace the strong surfactant on the surface of the magnetic nanoparticles, which will easily cause the aggregation of the magnetic nanoparticles or the surfactant cannot be completely replaced, which will affect the bond between the polymer and the magnetic nanoparticles. Affect the stability and uniformity of the final product, and this process is very cumbersome and time-consuming
Moreover, the organic phase thermal decomposition technology has strict requirements on the reaction conditions, the temperature is relatively high, and a large amount of flammable organic solvents and expensive organic reagents are used.
[0005] The background technology close to the present invention is scheme 2., mainly in the system that polymer exists as in the polyelectrolyte system by Fe 2+ and Fe 3+ Co-precipitation or thermal decomposition and other methods have the advantage that the magnetic nanoparticles can be coated by the polymer immediately after the generation, and there is no need to elute or replace the surfactant, but the particle size obtained is difficult to control, especially the co- The precipitation method is generally synthesized under high pH conditions. A large number of cations will compete with the magnetic nanoparticles for the active groups of the polymer, resulting in that the magnetic nanoparticles cannot be completely covered by the polymer. At the same time, the high molecular weight polymer sol has a high viscosity. Its long chains are easily entangled together, resulting in another sense of "agglomeration" of magnetic nanoparticles, which affects further applications

Method used

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  • Superparamagnetic Fe3O4 nanometer particle with synthetic polymer modification from one-step method
  • Superparamagnetic Fe3O4 nanometer particle with synthetic polymer modification from one-step method
  • Superparamagnetic Fe3O4 nanometer particle with synthetic polymer modification from one-step method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 2.5 g of acrylic acid and 1.38 g of ferrous chloride tetrahydrate into a reaction vessel filled with 50 ml of anaerobic distilled water, and slowly stir for 30 minutes under nitrogen protection. Then under the protection of nitrogen in the range of 85°C, stir vigorously at a constant temperature, and add 200 ml of a mixed solution containing 0.338 g of potassium peroxodisulfate and 1.8 g of sodium hydroxide dropwise to the reaction vessel within 4 hours. Then continue to react for 30 minutes while stopping heating and naturally cooling to room temperature. Centrifuge, wash with water, and centrifuge again to obtain a black precipitate, a light black powder dried in vacuum at room temperature, and redisperse the black precipitate in a mixed solution of ethanol and water to obtain a stable sol, which can be stored for a long time.

[0025] Some structures and properties of the prepared polymer-coated magnetic nanoparticles were characterized. TEM characterization of ...

Embodiment 2

[0027] Add 2.5 g of acrylic acid and 0.3452 g of ferrous chloride tetrahydrate into a reaction vessel filled with 50 ml of anaerobic distilled water, and slowly stir for 30 minutes under nitrogen protection. Then under the protection of nitrogen in the range of 85°C, stir vigorously at a constant temperature, and add 200 ml of a mixed solution containing 0.1688 g of potassium peroxodisulfate and 1.8 g of sodium hydroxide dropwise to the reaction vessel within 3 hours. Then continue to react for 30 minutes while stopping heating and naturally cooling to room temperature. Centrifuge, wash with water, and centrifuge again to obtain a black precipitate, a light black powder dried in vacuum at room temperature, and redisperse the black precipitate in a mixed solution of ethanol and water to obtain a stable sol, which can be stored for a long time, and the particle size ratio can be implemented The one prepared in Example 1 is smaller.

Embodiment 3

[0029] Add 5.0 g of acrylic acid and 0.6903 g of ferrous chloride tetrahydrate into a reaction vessel filled with 50 ml of anaerobic distilled water, and slowly stir for 30 minutes under nitrogen protection. Then, under the protection of nitrogen in the range of 85°C, stir vigorously at a constant temperature, and add 200 ml of a mixed solution containing 0.253 g of potassium peroxodisulfate and 2.63 g of sodium hydroxide dropwise to the reaction vessel within 4 hours. Then continue to react for 30 minutes while stopping heating and naturally cooling to room temperature. Centrifuge, wash with water, and centrifuge again to obtain a black precipitate, a light black powder dried in vacuum at room temperature, and redisperse the black precipitate in a mixed solution of ethanol and water to obtain a stable sol, which can be stored for a long time.

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Abstract

A superparamagnetic Fe3O4 nanometer particle with polymer modification from one-step synthesis is prepared by adding polymer monomer and ferrous salt with mol ratio 1-20:1 into anaerobic distilled water, stirring under nitrogen protection at 75-100DEG, dripping into mixed solution of disulfide acid salt and base, reacting for 30-60mins, and obtaining magnetic nanometer particle sol coated by black polymer with polymer concentration 0.05-0.3M and ferrous salt concentration 0.005-0.05M. Its advantages include stable dispersion, simple process, short time and high productivity.

Description

technical field [0001] The invention belongs to the field of preparation of magnetic nanomaterials, in particular to a preparation method of a polymer-inorganic nanocomposite material, in particular to a superparamagnetic Fe modified by a soluble polymer with uniform particle size distribution 3 o 4 Methods for the preparation of nanoparticles. Background technique [0002] Due to the significant difference in physical properties from the corresponding bulk materials, magnetic nanomaterials have become a hot spot in current scientific research due to their scientific importance and wide application value in technology, especially in the application and development of biological related fields. Rapid, including magnetic resonance imaging (MRI), drug delivery, biological rapid separation technology and clinical diagnosis and treatment, especially the diagnosis and treatment of cancer. In the above-mentioned bio-related fields, magnetic nanoparticles are required to have a su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09C3/10C09C1/24C08F2/44C08F20/00
Inventor 陈接胜李新昊李国栋
Owner JILIN UNIV
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