Preparation process of magnetic partical/polymer/silicon dioxide structure magnetic microball

A technology of silicon dioxide and magnetic microspheres, applied in the direction of magnetism of organic materials/organic magnetic materials, etc., can solve the problems of complicated operation, unfavorable biological application, poor biocompatibility of magnetic microspheres, etc., and achieve a simple and good growth process. The effect of biocompatibility and chemical stability, simple preparation method

Inactive Publication Date: 2007-07-18
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of the background technology has cumbersome steps and complex operation, and a large amount of surfactant is introduced in the process of growing silica, and the magnetic microspheres stabilized by surfactant have poor biocompatibility and the surfactant is in SiO 2 The surface is not easy to remove, which is not conducive to further biological applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: Preparation of hydrophobic magnetic nanoparticles (1)

[0016] Add 0.046mol of Fe to 100ml of water that has been passed through nitrogen and deoxygenated 3+ and 0.023mol of Fe 2+ A mixed solution was obtained. Take 400ml of water and pass nitrogen to remove oxygen in a 1L reaction flask, add 20ml of concentrated ammonia water with a mass percentage concentration of 25% and 1.33g of 10-undecylenic acid in turn, and quickly pour the above-mentioned iron salt into it under vigorous stirring The solution was mixed and reacted at 50°C for 1h. After the reaction is completed, adjust the reaction solution to acidity with hydrochloric acid, separate the black solid from the reaction solution with a 0.1T permanent magnet, and wash the obtained solid with high-purity water for 3 to 5 times to obtain the hydrophobic Fe 3 o 4 Nanoparticles.

[0017] Will Fe 3+ and Fe 2+ respectively replaced by Co 3+ and Co 2+ , the hydrophobic Co can be obtained 3 o 4 Nan...

Embodiment 2

[0018] Embodiment 2: Preparation of hydrophobic magnetic nanoparticles (2)

[0019] Add 0.046mol of Fe to 100ml of water that has been passed through nitrogen and deoxygenated 3+ and 0.023mol of Fe 2+ A mixed solution was obtained. Take 400ml of water in a 1L round-bottomed flask, pass through nitrogen to remove oxygen, add 20ml of concentrated ammonia water with a mass percentage concentration of 25-28% and 5.52g of myristic acid in turn, and quickly pour the above-mentioned iron salt into it under vigorous stirring. solution, and reacted at 80°C for 1h. Oxygen was then introduced into the reaction solution for 2 h. After the reaction is completed, adjust the reaction solution to acidity with hydrochloric acid, separate the red solid from the reaction solution with a 0.1T permanent magnet, and wash the obtained solid with high-purity water for 3 to 5 times to obtain hydrophobic γ-Fe 2 o 3 Nanoparticles

Embodiment 3

[0020] Embodiment 3: Preparation of hydrophobic magnetic nanoparticles (3)

[0021] Add 0.046mol of Fe to 100ml of water that has been passed through nitrogen and deoxygenated 3+ and 0.023mol Co 2+to obtain a mixed solution. Take 400ml of water in a 1L reaction flask to pass through nitrogen to remove oxygen, add 20ml of concentrated ammonia water with a mass percentage concentration of 25% and 10.8g of oleic acid in turn, and quickly pour the above mixed solution into it under vigorous stirring, and heat it at 90°C. Under reaction 1h. After the reaction is completed, adjust the reaction solution to acidity with hydrochloric acid, separate the black solid from the reaction solution with a 0.1T permanent magnet, and wash the obtained solid with high-purity water for 3 to 5 times to obtain CoFe 2 o 4 Hydrophobic nanoparticles.

[0022] Will Co 2+ replace with Mn 2+ , the hydrophobic MnFe can be obtained 2 o 4 Nanoparticles.

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Abstract

The present invention is preparation process of magnetic particle / polymer / silica magnetic microsphere and belongs to the field of magnetic material technology. The technological process includes the following steps: 1. dispersing nanometer hydrophobic magnetic particle in solvent comprising silane reagent and olefin monomer to form oil phase, dissolving surfactant in water to form water phase, mixing to form oil-in-water suspension, adding initiator to initiate polymerization to obtain magnetic microsphere with polymer in the surface; and 2. dispersing the magnetic microsphere with polymer in mixed solvent comprising alcohol, water and ammonia water and hydrolyzing condensation of ethyl silicate to grow silica layer. The present invention has simple silica layer growth process and excellent controllability, and the prepared magnetic composition particle has excellent biocompatibility and high chemical stability and may be further functionated.

Description

technical field [0001] The invention belongs to the field of magnetic materials, in particular to a method for preparing magnetic particle / polymer / silicon dioxide structured magnetic microspheres. Background technique: [0002] Superparamagnetic microspheres have a wide range of applications in the fields of biotechnology and biomedicine, such as the separation and purification of cells, proteins, DNA and RNA, magnetic resonance imaging, and the directional delivery of drugs. These applications require magnetic microspheres to have strong magnetism, good chemical stability, good biocompatibility and relatively uniform particle size distribution. In order to meet the above requirements, magnetic microspheres are generally prepared by coating the surface of magnetic particles with a protective layer. The methods for preparing magnetic microspheres in the prior art mainly include biomolecule embedding, polymer coating and silica coating. The magnetic microspheres prepared by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/44C08F2/16C08K3/36H01F1/42
Inventor 杨文胜颜峰王刚陆子阳李军韩延东王明辉
Owner JILIN UNIV
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