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A kind of monodisperse superparamagnetic carboxyl silicon magnetic bead and preparation method thereof

A technology of superparamagnetic and carboxyl silicon, which is applied in the fields of magnetism of organic materials/organic magnetic materials, manufacturing of inductors/transformers/magnets, and electrical components, etc. Problems such as poor dispersion of carboxyl magnetic bead emulsion, to achieve the effect of high specific binding rate, good dispersion and small particle size

Active Publication Date: 2021-09-21
YANSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Currently reported functional nano-magnetic bead materials are coated with silica and have functional groups on the surface, but they cannot achieve superparamagnetism, stable dispersion in the medium and specific adsorption of proteins at the same time, so their application is greatly restricted. limit
In the preparation of existing carboxylated magnetic beads, polyethylene glycol (molecular weight from 1000 to 20000) is basically selected as the dispersant, and the spherical shape of ferric oxide prepared by solvothermal is irregular, so as to further disperse the carboxylated magnetic bead emulsion Poor sex

Method used

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  • A kind of monodisperse superparamagnetic carboxyl silicon magnetic bead and preparation method thereof
  • A kind of monodisperse superparamagnetic carboxyl silicon magnetic bead and preparation method thereof
  • A kind of monodisperse superparamagnetic carboxyl silicon magnetic bead and preparation method thereof

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Embodiment 1

[0028] The present embodiment provides a kind of monodisperse superparamagnetic carboxy silicon magnetic bead, and its preparation method comprises:

[0029] (1) Fe 3 o 4 Preparation of nanoclusters: weigh 1.08g FeCl 3 ·6H 2 0 to a three-necked flask, add 40ml of ethylene glycol to fully dissolve, and when heated to 60°C, add 0.108g of polyacrylic acid (PAA) and 9g of NaAc simultaneously at a stirring rate of 500r / min, and stir to completely dissolve the solid. The reaction solution was transferred to a reaction kettle, and reacted at 200° C. for 12 hours. After the reaction is completed, use a magnetic stand for auxiliary magnetic separation, alternately wash with deionized water and ethanol several times, remove the residual components and by-products of the reaction, dry in a drying oven, and collect monodisperse superparamagnetic Fe 3 o 4 Nanoclusters, whose transmission electron microscope pictures are shown in figure 1 shown.

[0030] (2) Fe 3 o 4 @SiO 2 Prepar...

Embodiment 2

[0034] The present embodiment provides a kind of monodisperse superparamagnetic carboxy silicon magnetic bead, and its preparation method comprises:

[0035] (1) Fe 3 o 4 Preparation of nanoclusters: weigh 1.08g FeCl 3 ·6H 2 O to a three-necked flask, add 40ml of diethylene glycol to fully dissolve, and when heated to 60°C, add 0.108g of PAA and 9g of NaAc simultaneously at a stirring rate of 500r / min, and stir to completely dissolve the solid. The reaction solution was transferred to a reaction kettle, and reacted at 250° C. for 12 hours. After the reaction is completed, use a magnetic stand for auxiliary magnetic separation, alternately wash with deionized water and ethanol several times, remove the residual components and by-products of the reaction, dry in a drying oven, and collect monodisperse superparamagnetic Fe 3 o 4 nanoclusters.

[0036] (2) Fe 3 o 4 @SiO 2 Preparation: Weigh 0.1g of Fe obtained in step (1) 3 o 4 Nanoclusters, 60ml ethanol and 20ml deioni...

Embodiment 3

[0039] The present embodiment provides a kind of monodisperse superparamagnetic carboxy silicon magnetic bead, and its preparation method comprises:

[0040] (1) Fe 3 o 4 Preparation of nanoclusters: weigh 1.08g FeCl 3 ·6H 2 O to a three-necked flask, add 40ml of ethylene glycol to fully dissolve, and when heated to 60°C, add 0.108g of PAA and 9g of NaAc simultaneously at a stirring rate of 500r / min, and stir to completely dissolve the solid. The reaction solution was transferred to a reaction kettle, and reacted at 200° C. for 12 hours. After the reaction is completed, use a magnetic stand for auxiliary magnetic separation, alternately wash with deionized water and ethanol several times, remove the residual components and by-products of the reaction, dry in a drying oven, and collect monodisperse superparamagnetic Fe 3 o 4 nanoclusters.

[0041] (2) Fe 3 o 4 @SiO 2 Preparation: Weigh 0.1g of Fe obtained in step (1) 3 o 4 Nanoclusters, 60ml ethanol and 20ml deionize...

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Abstract

The invention provides a monodisperse superparamagnetic carboxyl silicon magnetic bead and a preparation method thereof, belonging to the technical field of magnetic material preparation. The preparation method comprises: Fe 3 o 4 The nanoclusters are dispersed in the alcohol solution, then ammonia water and TEOS are added, and stirred for 4-6 hours to obtain Fe with a diameter of 100-240nm 3 o 4 @SiO 2 complex; then Fe 3 o 4 @SiO 2 The compound is dispersed in alcohol solution, acrylic compound and acrylamide are added, then mixed with initiator and crosslinking agent under the protection of nitrogen, and reacted at 65-80°C for 8-12 hours to obtain Fe 3 o 4 @SiO 2 ‑COOH composite particles. The preparation method is simple and controllable, and the prepared magnetic beads have uniform particle size, good dispersibility, superparamagnetism, and can specifically bind to proteins, and can be further used for the separation of biological macromolecules such as proteins.

Description

technical field [0001] The invention relates to the technical field of magnetic material preparation, in particular to a monodisperse superparamagnetic carboxyl silicon magnetic bead and a preparation method thereof. Background technique [0002] Magnetic beads refer to superparamagnetic microspheres with fine particle size. Functionalized nano-magnetic beads firstly have super-strong paramagnetism, can quickly gather in a magnetic field, and can be uniformly dispersed after leaving the magnetic field. Secondly, it has a suitable and uniform particle size, which ensures strong enough magnetic response and good dispersion. Third, it has abundant surface active groups, so that it can be coupled with biochemical substances, and can be separated from the sample to be tested under the action of an external magnetic field. Generally, the application of functionalized nano-magnetic beads in the fields of biology, medicine and food needs to meet several conditions: ① high magnetic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F220/06C08F220/56C08F222/38H01F1/42H01F41/02
CPCC08F292/00H01F1/42H01F41/02C08F220/06C08F220/56C08F222/385
Inventor 李秋荣裴家蓉栗坤刘志伟肖海燕石明李健
Owner YANSHAN UNIV
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