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Magnetic silicon dioxide microspheres with nuclear shell and surface anisotropic double functional groups and preparation method thereof

A silica and anisotropic technology, applied in the field of magnetic silica microspheres and their preparation, to achieve the effects of good repeatability, strong versatility and regular shape

Active Publication Date: 2011-08-24
SUZHOU WIN BIO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some existing physical or chemical methods only achieve surface anisotropic modification on micron-sized microspheres without magnetic cores, or obtain the oxidation of bifunctional groups on the surface by step-by-step modification of two silane coupling agents. silicon particles

Method used

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  • Magnetic silicon dioxide microspheres with nuclear shell and surface anisotropic double functional groups and preparation method thereof
  • Magnetic silicon dioxide microspheres with nuclear shell and surface anisotropic double functional groups and preparation method thereof
  • Magnetic silicon dioxide microspheres with nuclear shell and surface anisotropic double functional groups and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Example 1. 0.81 g FeCl 3 ·6H 2 O and 2.16 g of sodium citrate were dissolved in 30 ml of ethylene glycol respectively, and after mixing, they were moved into a stainless steel reaction kettle with a tetrafluoroethylene liner, tightened the reaction kettle, heated to 200 ° C, and reacted for 8 hours to obtain the average particle size. The 350 nm inorganic magnetic microspheres were washed with ethanol and water three times under magnetic separation. Obtain magnetic separation products of magnetic microspheres; use strong acid to activate inorganic magnetic microspheres, disperse inorganic magnetic microspheres in deionized water, use magnetic field to separate and wash, and then disperse in 1 M hydrochloric acid solution, ultrasonication for 10-40 Minutes, then use a magnet to separate the magnetic microspheres treated with strong acid, and wash with deionized water 3-5 times. Add the dispersion of magnetic microspheres activated by strong acid into the alcohol / wat...

Embodiment 2

[0039] Example 2. 0.81 g FeCl 3 ·6H 2 O and 2.16 g of sodium citrate were dissolved in 30ml of ethylene glycol respectively. After mixing, they were moved into a stainless steel reaction kettle with a tetrafluoroethylene liner, tightened the reaction kettle, heated to 200°C, and reacted for 16 hours to obtain the average particle size. The 400 nm inorganic magnetic microspheres were washed 3 times with ethanol and water respectively under magnetic separation. Obtain magnetic separation products of magnetic microspheres; use strong acid to activate inorganic magnetic microspheres, disperse inorganic magnetic microspheres in deionized water, use magnetic field to separate and wash, and then disperse in 1 M hydrochloric acid solution, ultrasonication for 10-40 Minutes, then use a magnet to separate the magnetic microspheres treated with strong acid, and wash with deionized water 3-5 times. Add the dispersion of magnetic microspheres activated by strong acid into the alcohol / w...

Embodiment 3

[0043] Example 3. 0.81 gFeCl 3 ·6H 2O and 2.16 g of sodium citrate were dissolved in 30ml of ethylene glycol respectively. After mixing, they were moved into a stainless steel reaction kettle with a tetrafluoroethylene liner, tightened the reaction kettle, heated to 200°C, and reacted for 24 hours to obtain the average particle size. Inorganic magnetic microspheres of 520 nm were washed with ethanol and water three times under magnetic separation. Obtain magnetic separation products of magnetic microspheres; use strong acid to activate inorganic magnetic microspheres, disperse inorganic magnetic microspheres in deionized water, use magnetic field to separate and wash, and then disperse in 1 M hydrochloric acid solution, ultrasonication for 10-40 Minutes, then use a magnet to separate the magnetic microspheres treated with strong acid, and wash with deionized water 3-5 times. Add the dispersion of magnetic microspheres activated by strong acid into the alcohol / water mixture...

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Abstract

The invention relates to magnetic silicon dioxide microspheres with a nuclear shell and surface anisotropic double functional groups and a preparation method thereof. The preparation method comprises the following steps of: preparing superparamagetic microspheres by a solvothermal process; preparing magnetic microspheres which are coated by silicon dioxide by a sol-gel process; preparing the magnetic silicon dioxide microspheres of which the surface has amino group by taking the magnetic silicon dioxide microspheres as seeds and by the copolycondensation of alkyl ester orthosilicate and a silane coupling agent, and drying the magnetic silicon dioxide microspheres to obtain samples; and by a PICKERING emulsion technology, stabilizing a paraffin / aqueous emulsion system with a micrometer scale by using the aminated magnetic microspheres to form single-layer close packing of the magnetic microspheres on the surface of paraffin spheres, then reacting the amino group on the surface of the magnetic microspheres which is exposed in a liquid phase with succinic anhydride to introduce carboxyl into the partial surface of the microspheres, so that the surfaces of the magnetic microspheres have the anisotropic double functional groups. The obtained magnetic microspheres with the double functional groups have the advantages that: magnetic responsiveness is high; grain size can be controlled between 200 and 800 namometers; and the density of the surface functional groups can be adjusted.

Description

field of invention [0001] The invention belongs to the technical field of controllable surface modification of inorganic magnetic composite materials, and specifically relates to a magnetic silica microsphere with a core-shell structure and surface anisotropic dual functional groups and a preparation method thereof. Background technique [0002] Since Ugelstad et al. disclosed the preparation of monodisperse (CV<3%) micron-scale magnetic composite microspheres in US Patent PCT / NO83 / 00014, nano-superparamagnetic materials have been widely used in biomolecules due to their excellent characteristics. There are many biomedical fields such as separation and purification, immunodiagnosis, targeted drug delivery and therapy, and biosensors. From the perspective of the application of magnetic microspheres, in order to improve the colloidal stability of microspheres, regulate their surface affinity, hydrophobicity and binding ability with specific biomolecules, it is necessary to ...

Claims

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Application Information

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IPC IPC(8): B01J13/02H01F1/11
Inventor 王祎龙张兵波郭方方时东陆
Owner SUZHOU WIN BIO TECH CO LTD
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