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Preparation method of meso-porous nanometer magnetic material

A technology of nano-magnetic materials and mesoporous materials, applied in the field of inorganic nano-material preparation technology, can solve the problems of no response, slow response to external magnetic field, weak magnetic properties of mesoporous nano-magnetic materials, etc. simple craftsmanship

Inactive Publication Date: 2012-10-10
CHINA JILIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few research reports on mesoporous silica nano-magnetic materials at home and abroad, and they mainly focus on γ-Fe 2 o 3 , Fe 3 o 4 、Co 3 o 4 Doped / filled mesoporous nanomagnetic materials [E.Kockrick, et al.Adv.Mater., 19(2007) 3021; ​​J.-S.Jung, et al.J.Magn.Magn.Mater., 272- 276(2004)e 1157; T.Tajiri, et al.J.Phys.Soc.Jpn., 75(2006)113704; S.V.Kolotilov, et al.J.Solid State Chem., 179(2006)2426], but Related reports show that the magnetism of mesoporous nano-magnetic materials is not strong, and even superparamagnetism appears [E.Delahaye, et al.J.Phys.Chem.B, 110(2006) 26001]
This type of material responds slowly or has no response to external magnetic fields, and is not suitable as a carrier for targeted drugs

Method used

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  • Preparation method of meso-porous nanometer magnetic material
  • Preparation method of meso-porous nanometer magnetic material
  • Preparation method of meso-porous nanometer magnetic material

Examples

Experimental program
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Effect test

Embodiment 1

[0023] 2g block polymer (P123(EO) 20 (PO) 70 (EO) 20 ) dissolved in 50ml 2M HCl and 10ml H 2 In O, stir at a constant temperature of 39°C for 3 hours; then add 2.5ml of tetraethyl orthosilicate (TEOS) dropwise, stir for about 30 minutes, a colloidal suspension will appear, and adjust the pH value between 7 and 8 with ammonia water; add Appropriate amount of iron nitrate (Fe(NO) 3 9H 2 (0) an aqueous solution, so that the ratio of the number of molecules of iron to silicon is 15: 100, and continue stirring at 39°C for 24h; the solution is transferred to a polytetrafluoroethylene stainless steel hydrothermal kettle, and heated at 100°C for 72h; After the reaction is completed, dry at 60°C and then calcinate at 750°C for 6 hours to remove the template. After fully grinding, dry at 150°C for several days to obtain SBA-15 mesoporous molecular sieve with iron-containing skeleton.

[0024] Get 1g of the above-mentioned obtained SBA-15 mesoporous molecular sieve and dissolve it ...

Embodiment 2

[0026] Dissolve 2.5g of CTAB in 60g of water, add 20ml of concentrated ammonia water, stir at room temperature for a while, add 14ml of TEOS dropwise, and add an appropriate amount of ferric nitrate (Fe(NO) 3 9H 2 O) an aqueous solution, so that the ratio of the number of molecules of iron to silicon is 3:100, the solution is continuously stirred for 2-3 hours, and then heated at 100° C. for 3 days. The product is filtered, washed, dried, and calcined at 550°C to remove the template agent.

[0027] Take 1g of the above-mentioned obtained MCM-41 mesoporous molecular sieve and dissolve it in about 20ml absolute ethanol, 2.5mmol cobalt nitrate (Co(NO) 2 ·6H 2 O) and 5mmol iron nitrate (Fe(NO) 3 9H 2 O) Slowly evaporate the solvent at 50°C, wash the residue three times, dry at 80°C for 24 hours, and finally calcinate at 550°C for 6 hours to obtain CoFe 2 o 4 / Fe 2 o 3 - MCM-41 nano magnetic material.

Embodiment 3

[0029] 4. Dissolve 11g CTAB in 21g water, add 0.38g NaOH, stir at room temperature for a while, add 5ml TEOS dropwise, continue stirring the solution for 2-3h, add an appropriate amount of cobalt nitrate (Co(NO) 2 ·6H 2 O) an aqueous solution, so that the ratio of the number of molecules of iron to silicon is 10:100, and after stirring evenly, heat at 100° C. for 3 days. The product is filtered, washed, dried, and calcined at 550°C to remove the template agent.

[0030] Take 1g of the above-mentioned obtained MCM-48 mesoporous molecular sieve and dissolve it in about 20ml anhydrous water, 0.1mmol barium nitrate (Ba(NO) 2 ) and 1.2mmol iron nitrate (Fe(NO) 3 9H 2 O) Slowly evaporate the solvent at 40°C, wash the residue three times, dry at 80°C for 24 hours, and finally calcinate at 550°C for 6 hours to obtain BaFe 12 o 19 / Co 3 o 4 - MCM-48 nano magnetic material.

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Abstract

The invention relates to a preparation method of a meso-porous nanometer magnetic material. The preparation method is characterized by comprising the following steps: (1) adopting a sol-gel compounding hydrothermal method to directly compound a meso-porous material containing a nanometer magnetic material in a framework; dissolving a certain amount of block copolymer or surface active agent to an acidic / alkaline aqueous solution; uniformly stirring at a constant temperature; then dripping a certain amount of ethyl orthosilicate and adding a certain amount of various dissoluble salts of iron, cobalt, nickel, and the like; continuing to stir at the temperature for 10-30 hours; adjusting a pH value before hydrothermal treatment at 100 DEG C for 1-3 days; filtering products; washing ethanol twice; drying at 60-80 DEG C; and calcining at 550-750 DEG C in air for 6-10 hours to obtain the meso-porous nanometer magnetic material containing the nanometer magnetic material in the framework. The over-long one-dimensional nanometer material synthesized by the method has a favorable microstructure and can promote the application of the one-dimensional nanometer material to the aspects of integrated circuits and functional element devices, such as nanometer electronic and photoelectronic devices, and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation technology of inorganic nanometer materials, and in particular relates to a preparation method of mesoporous nanometer magnetic materials with a new structure. Background technique [0002] At present, nano-magnetic materials have potential application prospects in the fields of non-destructive magnetic sealing, ultra-high magnetic recording, biomedicine, and broadband microwave absorption. In the field of biomedicine, nanomagnetic materials have shown great advantages in the fields of biomagnetic separation, targeted drug carriers, and tumor magnetic hyperthermia prevention and treatment. As a drug carrier, nano-magnetic materials can directly make the drug reach the diseased organ through the action of an external magnetic field or by injection, and accumulate and release the drug in the organ under the action of an external magnetic field to achieve the purpose of curing the disease. Compa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01F1/01B22F9/06B22F9/24A61K47/02
Inventor 王新庆金红晓金顶峰葛洪良
Owner CHINA JILIANG UNIV