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
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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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