Magnetic inorganic nano-particle/ordered meso-porous silica core-shell microspheres and preparation thereof

A technology of mesoporous silica and amorphous silica, applied in the direction of fibrous fillers, etc., can solve the problems of poor magnetic response effect of composite materials, uneven shape and disorder of composite materials, etc.

Inactive Publication Date: 2008-06-25

FUDAN UNIV

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AI-Extracted Technical Summary

Problems solved by technology

But so far, there are few reports on the synthesis of core-shell composite nanospheres with magnetic oxide particles as the core and ordered mesoporous materials as the shell.

In the existing reports, the synthesized composite materials have disadvantages such as poor ...

Abstract

The invention belongs to the nano-composite material technology field, in particular to a magnetic inorganic nano-particle/ordered mesoporous silica core-shell microsphere and a preparation method thereof. The invention first utilizes sol-gel chemical synthesis method, coats a layer of amorphous silica on the surface of a plurality of magnetic inorganic nano-particles, then utilizes self-assembly of an organic surfactant as structure-directing agent and inorganic species in the solution, coats a layer of ordered meso-structured silica/surfactant composite material on the surface of the magnetic inorganic nano-particle/ silica composite microsphere, removes the surfactant through solvent extraction, and obtains the ordered mesoporous magnetic inorganic nano-particle/silica core-shell structure composite microsphere material. The composite microsphere has high specific surface area, strong magnetic responsiveness, and wide application prospect in bioseparation and bioabsorption. The invention is simple in method, easy in obtaining raw materials, and suitable for large scale production.

Application Domain

Pigmenting treatment

Technology Topic

Chemical synthesisSol-gel +12

Examples

Experimental program(4)

Example Embodiment

[0015] Example 1:

[0016] (1) Disperse 0.1g magnetic ferroferric oxide particles with a size of about 300nm in 80ml ethanol, 20ml deionized water and 1ml concentrated ammonia (28wt%), add 0.3g ethyl orthosilicate (TEOS), room temperature After stirring for 6 hours, a magnetic composite microsphere with a layer of silica deposited on the surface was obtained. The product was separated with a magnet and washed with a mixed solution of ethanol and water. After washing, the product was dried at room temperature and then ready for use.

[0017] (2) The magnetic ferroferric oxide composite microspheres with a layer of silica deposited on the surface were ultrasonically dispersed in 60ml ethanol, 80ml deionized water, 1.00g concentrated ammonia and 0.30g cetyltrimethylammonium bromide (CTAB) mixed solution, after stirring for 0.5h to make the solution uniform, add 0.40g of ethyl orthosilicate (TEOS) dropwise, and continue to stir for 6h after the addition is complete, to obtain a magnetic ferroferric oxide/surfactant-containing Silica composite microspheres, magnets collect the product, and wash with a mixed solution of ethanol and water.

[0018] (3) The composite microspheres obtained above were extracted three times in 60 ml of acetone at 80° C. for 48 hours to remove the surfactant, washed with deionized water, and dried. The magnetic saturation intensity of the obtained product is 40.8emu/g, the particle size is 410nm, and the mesopore diameter is 2.1nm.

Example Embodiment

[0019] Example 2:

[0020] (1) Disperse 0.1g magnetic ferroferric oxide particles with a size of about 500nm in 100ml ethanol, 10ml deionized water and 1ml concentrated ammonia (28wt%), add 0.25g ethyl orthosilicate (TEOS), room temperature After stirring for 7 hours, a magnetic composite microsphere with a layer of silica deposited on the surface was obtained. The product was separated with a magnet and washed with a mixed solution of ethanol and water. After washing, the product was dried at room temperature and then ready for use.

[0021] (2) The magnetic ferroferric oxide composite microspheres with a layer of silica deposited on the surface were ultrasonically dispersed in 90ml ethanol, 60ml deionized water, 1.00g concentrated ammonia and 0.30g cetyltrimethylammonium bromide (CTAB) mixed solution, after stirring for 0.8h to make the solution uniform, add 0.40g ethyl orthosilicate (TEOS) dropwise, and continue to stir for 5h after the addition is complete, to obtain a magnetic ferroferric oxide/surfactant-containing Silica composite microspheres, magnets collect the product, and wash with a mixed solution of ethanol and water.

[0022] (3) The composite microspheres obtained above were extracted three times in 60 ml of acetone at 80° C. for 48 hours to remove the surfactant, washed with deionized water, and dried. The resulting product has a magnetic saturation intensity of 38.0emu/g, a particle size of 620nm, and a mesopore diameter of 2.4nm.

Example Embodiment

[0023] Example 3:

[0024] (1) Combine 0.1g magnetic NiFe with a size of about 300nm 2 O 4The particles are uniformly dispersed in 90ml of ethanol, 10ml of deionized water and 1ml of concentrated ammonia (28wt%), add 0.5g of ethyl orthosilicate (TEOS), stir at room temperature for 10h to obtain a magnetic composite with a layer of silica deposited on the surface For microspheres, the product is separated with a magnet and washed with a mixed solution of ethanol and water. After washing, the product is dried at room temperature and ready for use.

[0025] (2) Magnetic NiFe after depositing a layer of silicon dioxide on the surface 2 O 4 The composite microspheres were ultrasonically dispersed in 30ml ethanol, 110ml deionized water, 1.00g hydrochloric acid aqueous solution (1.0M) and 0.30g Brij 56(C 16 H 33 EO 10 ), after stirring for 0.4h to make the solution uniform, add 0.40g of methyl orthosilicate (TEOS) dropwise, and continue to stir for 8h after the addition is complete to obtain magnetic NiFe 2 O 4 /Silica composite microspheres containing surfactants, magnets collect the product, and wash with a mixed solution of ethanol and water.

[0026] (3) The composite microspheres obtained above were extracted three times in 60 ml of acetone at 80° C. for 36 hours to remove the surfactant, washed with deionized water, and dried. The obtained product has a magnetic saturation intensity of 52.7emu/g, a particle size of 440nm, and a mesopore diameter of 2.0nm.

PUM

Property	Measurement	Unit
Magnetic saturation	40.8	emu/g
Particle size	410.0	nm
Mesopore diameter	2.1	nm

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