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Superparamagnetism material carrying CuO and preparation method thereof

A technology of superparamagnetic and superparamagnetic particles, which is applied in the preparation of microspheres, magnetism of inorganic materials, microcapsule preparations, etc., to achieve the effects of good chemical stability, simple operation, and wide and easy access to raw materials

Inactive Publication Date: 2008-01-16
SOUTH CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, it solves the problem of stability and agglomeration of superparamagnetic particles during use; functional material is separated from the reactor)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 Fe 3 o 4 Synthesis of / MCM-41 / CuO

[0029] (1) With superparamagnetic nano-Fe 3 o 4 Synthesis

[0030] Under nitrogen protection, 1.1263g (NH 4 ) 2 C 2 o 4 , 9.0016gFeSO 4 ·7H 2 O and 12.9054gFe 2 (SO 4 ) 3 Dissolve in 150mL of 80°C water, add concentrated ammonia water to pH = 9, react for 1.5h, wash, and magnetically separate to obtain Fe 3 o 4 precipitation.

[0031] (2) Fe 3 o 4 / Synthesis of MCM-41

[0032] At room temperature, the above Fe 3 o 4 Precipitate on N 2 Stir and disperse in 23mL deionized water under protection, add 3.6mL NH 3 ·H 2 O (25%, mass percent). Dissolve 0.2220g TBAB (tetrabutyl ammonium bromide, tetrabutylammonium bromide) in 10mL deionized water, and 1.0026g CTAB (cetyl trimethyl ammonium bromide, cetyltrimethylammonium bromide) in 10mL deionized water. Add TBAB and CTAB solutions sequentially to the 3 o 4 To the precipitated dispersion system, 4.05mLTEOS (tetraethyl orthosilicate) was added dropwise with s...

Embodiment 2

[0035] The synthesis of embodiment 2 Fe / MCM-48 / CuO

[0036] (1) Superparamagnetic nano Fe 3 o 4 Synthesis

[0037] Under nitrogen protection, 1.1260g (NH 4 ) 2 C 2 o 4 , 9.0057gFeSO 4 ·7H 2 O and 12.9042gFe 2 (SO 4 ) 3 Dissolve in 150mL of 80℃ water, adjust pH=8.6 with ammonia water, continue to react for 1.5h, wash, and magnetically separate to obtain Fe 3 o 4 precipitation.

[0038] (2) Synthesis of Fe / MCM-48 / CuO

[0039] Under nitrogen atmosphere, the temperature is 273K to Fe 3 o 4 Add 50mL of deionized water, stir, add 14mL of NH 3 ·H 2 O (32%, mass fraction), add 5 mg copper nitrate solid, add 2.4 g CTAB and 50 mL absolute ethanol (EtOH). After stirring for 0.5 h, 3.66 mL of TEOS (tetraethyl orthosilicate) was added dropwise under rapid stirring. After dropping, react at room temperature for 3h. The molar ratio of the reactants is CTAB:TEOS:NH 3 :H 2 O:EtOH=0.4:1:12.5:174:54. Put into the hydrothermal reactor, keep the constant temperature at 480K ...

Embodiment 3

[0040] Example 3 Fe 3 o 4 Synthesis of / SBA-15 / CuO

[0041] (1) Superparamagnetic nano Fe 3 o 4 Synthesis

[0042] 1.5050g (NH 4 ) 2 C 2 o 4 , 12.0085gFeSO 4 ·7H 2 O and 17.1995gFe 2 (SO 4 ) 3 Dissolve in 200g of 70-80℃ water, add ammonia water, stir for 1.5h, wash to get Fe 3 o 4 After precipitation, separation and washing under magnetic field conditions, disperse it into a mixture of 10mL deionized water and 60mL isopropanol and adjust pH=9.8 with ammonia water, then add TEOS (tetraethyl orthosilicate) drop by drop to pH=9.1 , Reaction 3h. Take it out, separate it with a magnet, and wash it to get SiO 2 Coated Fe 3 o 4 .

[0043] (2) Fe 3 o 4 / Synthesis of SBA-15

[0044] 6.0g P123 (polyoxyethylene ether-epoxypropylene ether-epoxyethylene ether triblock polymer surfactant, average molecular weight is 5800, molecular formula EO 20 PEOs 70 EO 20 ) was dissolved in 135mL distilled water and 616mL (4mol / L) HCl to obtain solution P; transfer P to SiO 2 ...

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Abstract

The invention relates to an ultra-paramagnetic material of load CuO, which is composed of ultra-paramagnetic particles, a mesoporous material layer, and CuO loaded on the internal and the external surfaces of mesoporous material layer; the preparation method includes: produce ultra-paramagnetic particle or its infusible precursor with the common sedimentation method; cover a layer of compact SiO2 or molecular sieve on the surface of the ultra-paramagnetic particle or the infusible precursor chemically with the sol-gel method; increase the temperature and maintain the temperature in gas atmosphere; samples obtained are placed into infusible cupric salt solution for separation, washing, filtering, and drying; burn in gas atmosphere; obtain the material with performances such as ultra-paramagnetism, catalyzing, and decoking. On one hand, the invention solves the problem of stability and conglobation of ultra-paramagnetic particle in the using process, and on the other hand, the invention makes it easier to separate catalyzer and desulfurizer in the using process. Meanwhile, the ultra-paramagnetic material of load CuO is also an infrared radiation material or microwave absorption material with high performance.

Description

technical field [0001] The present invention relates to new materials and their synthesis techniques, specifically including CuO-loaded superparamagnetic materials and their preparation methods Background technique [0002] Superparamagnetic materials refer to a class of nanomaterials that show magnetism in an external magnetic field when the size of the magnetic particles reaches or is smaller than a certain critical size, but their magnetism disappears after the magnetic field is removed. At present, superparamagnetic nanomaterials have been applied in chemical industry, machinery, electronics, printing, medicine and other industries, such as high-density magnetic recording materials, gas sensor devices, magnetic immune cell separation, nuclear magnetic resonance imaging and controlled release of drugs. Because nano-ions are easy to agglomerate, they lose some special properties that only nano-structures have. Agglomeration can be prevented by adding surfactants such as o...

Claims

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Application Information

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IPC IPC(8): H01F1/11B01J13/02C04B35/26C04B35/624C04B35/628B22F1/02
Inventor 铁绍龙曲玲玲
Owner SOUTH CHINA NORMAL UNIVERSITY
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