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Preparation method of periodic mesoporous organosilica (PMO) magnetic ball Fe3O4@PMO material

A technology of mesoporous organosilicon and organosilicon source is applied in the preparation of microspheres, the magnetic properties of inorganic materials, and the preparation of microcapsules. Effect

Inactive Publication Date: 2013-09-11
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, to the best of our knowledge reported ordered mesoporous organosilicon Fe 3 o 4 PMO magnetic ball materials are relatively less and the morphology is relatively poor (L. Zhang., et al., Adv. Mater. 2008, 20:805-809.)

Method used

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  • Preparation method of periodic mesoporous organosilica (PMO) magnetic ball Fe3O4@PMO material
  • Preparation method of periodic mesoporous organosilica (PMO) magnetic ball Fe3O4@PMO material
  • Preparation method of periodic mesoporous organosilica (PMO) magnetic ball Fe3O4@PMO material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Weigh 0.2g Fe 3 o 4 100nm nanoparticles were put into a 1000mL three-neck flask, and 600mL of 0.1M hydrochloric acid (HCl) solution was added to sonicate for 30min. Magnet recovery, repeated washing 3 times to remove residual hydrochloric acid. Add 0.5g cetyltrimethylammonium bromide (CTAB), 7mL 0.5M sodium hydroxide (NaOH) and 240mL water (H 2 O), stirring manually every 5min, ultrasonic 30min.

[0025] (2) Move the three-necked flask in step (1) to an 80°C oil bath, and mechanically stir at 480r / min for 10min to make the temperature of the solution in the three-necked flask reach 80°C.

[0026] (3) Increase the mechanical stirring speed to 600r / min, slowly add 2.16mL of 1,4-bis(triethoxysilyl)benzene (BTEB) dropwise into the three-necked flask, and continue the mechanical stirring for 2h.

[0027] (4) Pour the product obtained in step (3) into a 500mL beaker, attach a magnet to the beaker, let it stand for 5min, and pour off the reaction solution. Repeat 6 w...

Embodiment 2

[0032] Weigh 1.2g Fe 3 o 4 0.2g Fe in alternative embodiment one step (1) 3 o 4 , reduce the stirring speed, and keep other conditions unchanged.

[0033] image 3 For the Fe prepared by Example 2 of the present invention 3 o 4 Scanning electron microscope (SEM) picture of PMO magnetic ball material, by figure 1 It can be seen that the prepared Fe 3 o 4 The agglomeration of PMO magnetic ball materials is relatively severe, and the diameters are different, the small one is about 300nm, and the large one is about 700nm.

[0034] figure 2 For the Fe prepared by Example 2 of the present invention 3 o 4 Transmission electron microscopy (TEM) of PMO magnetic ball material. Depend on figure 2 It can be seen that the prepared Fe 3 o 4 The agglomeration of iron tetroxide wrapped by PMO magnetic ball material is relatively strong, and the wrapping of phenyl silicon source is also irregular.

Embodiment 3

[0036] Use 2.16mL 1,2-bis(triethoxysilyl)ethane (BTE) 1,4-bis(triethoxysilyl)benzene (BTEB) in step (3) of Example 1, other Conditions remain the same

[0037] Figure 5 Fe prepared for Example 3 of the present invention 3 o 4 Scanning electron microscope (SEM) picture of PMO magnetic ball material, by image 3 It can be seen that the prepared Fe 3 o4 The dispersion of PMO magnetic ball material is relatively uniform, and the diameter is about 450nm.

[0038] Figure 6 Fe prepared for Example 3 of the present invention 3 o 4 Transmission electron microscopy (TEM) of PMO magnetic ball material. Depend on figure 2 It can be seen that the prepared Fe 3 o 4 The PMO magnetic ball material is evenly wrapped, and the wall thickness is about 50nm.

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Abstract

The invention discloses a preparation method of periodic mesoporous organosilica (PMO) magnetic ball Fe3O4@PMO material. The synthesis route of the material comprises the following steps of: uniformly dispersing magnetic ferroferric oxide particles into an aqueous solution containing a template agent and alkali, then heating to 80 DEG C, then dropping an organic silicon source, hydrolyzing the silicon source in the presence of the alkali, wrapping the hydrolyzed silicon source on the surface of the magnetic ferroferric oxide in the presence of the template agent so as to form magnetic balls, removing the template agent by using an organic solvent for refluxing, and finally forming the target product Fe3O4@PMO in a mesoporous core-shell structure. The preparation method has the advantages that (1) as a large quantity of silicon hydroxyls are adsorbed on the surface of the material, functional groups can be further modified, so that the material can be widely applied to the fields of catalysis and sewage treatment; (2) the material synthesized through the preparation method can be conveniently and rapidly recycled only by additionally arranging a magnet; and (3) the magnetic material acquired through the preparation method is more uniformly dispersed than conventional magnetic materials, and the synthesis route of the material is simple and convenient.

Description

technical field [0001] The invention relates to material preparation technology, in particular to an ordered mesoporous organic silicon magnetic ball Fe 3 o 4 Preparation method of PMO material. Background technique [0002] Magnetic materials are widely used in production, life and scientific research due to their special properties. With the development of nanotechnology, the combination of magnetism and nanotechnology has aroused great interest of a large number of scientific researchers. Because magnetic nanomaterials can be attracted by external magnetic fields, magnetic nanoparticles are widely used in magnetic fluids, catalysis, biomedical technology, nuclear magnetic resonance imaging technology, data storage, and environmental improvement (A.H.Lu., et al. .,Angew.Chem.Int.Ed.2007,46:1222-1244;S.Shylesh.,et al.,Angew.Chem.Int.Ed.2010,49:3284-3459;L.Liu.,et al ., Small. 2011, 7:425-443.). [0003] Since the first discovery of ordered nano-mesoporous materials in 1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02H01F1/01
Inventor 刘国华高小双徐向明金荣华程探宇
Owner SHANGHAI NORMAL UNIVERSITY
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