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Super-hydrophobic hollow Fe3O4/mesoporous silicon dioxide nanocomposite, preparation method and application thereof

A technology of mesoporous silica and nanocomposite materials, applied in chemical instruments and methods, alkali metal compounds, adsorbed water/sewage treatment, etc., can solve the problems of hindering large-scale application of materials, poor circulation effect, increased energy consumption, etc. problems, to achieve the effect of improving oil absorption effect, saving reagents, and improving oil absorption efficiency

Active Publication Date: 2015-12-09
NANJING UNIV OF SCI & TECH
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Problems solved by technology

QanminPan et al. 2 o 3 CNanoparticlesunderMagneticField.[J].ACSAppliedMaterials&Interfaces,2010,2(11):3141-3146.) An organic and inorganic hydrophobic oil-absorbing material was prepared by emulsion polymerization, but due to its low oil absorption rate and poor circulation effect, it hinders Large-scale application of materials
LeiWu et al. (LeiWu, JunpingZhang, BuchengLia, AiqinWanga, Magneticallydrivensuperdurablesuperhydrophobicpolyestermaterialsforoil / waterseparation.[J].PolymerChemistry,2014,5(7):2382-2390) prepared by simply adding hexadecyltriethoxysilane dip coating Highly hydrophobic and super lipophilic polyester materials have been developed, which have a certain adsorption capacity for oil and organic reagents, but because the recovery of oil pollution can only be done through mechanical extrusion, which greatly increases energy consumption, thus limiting industrial use. application
Alireza Javadi et al. (Shaoqin Gong, Alireza Javadi, Qifeng Zheng, Francois Payen, Abdolreza Javadi, Yasin Altin, Zhiyong Cai, Ronald Sabo. PolyvinylAlcohol-CelluloseNanofibrils-GrapheneOxideHybridOrganicAerogels. [J]. ACS AppliedMaterials&Interfaces, 1913, 9) Polyvinyl alcohol for cellulose, 5: 5 Using graphene oxide nanosheets as raw materials, a hydrophobic graphene oxide composite airgel was prepared by freeze-drying. Although its oil absorption multiple is significant, the preparation process is too demanding. In addition, how to recycle the material has also become a major problem.

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  • Super-hydrophobic hollow Fe3O4/mesoporous silicon dioxide nanocomposite, preparation method and application thereof
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  • Super-hydrophobic hollow Fe3O4/mesoporous silicon dioxide nanocomposite, preparation method and application thereof

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preparation example Construction

[0028] A kind of superhydrophobic hollow Fe of the present invention 3 o 4 / The preparation method of mesoporous silica nanocomposite material, specific preparation process such as figure 1 , including the following steps:

[0029] The first step: the hollow Fe 3 o 4 Nanospheres were dissolved in isopropanol solution to form Fe with a mass concentration of 3.3 mg / mL 3 o 4 solution, ultrasonically disperse at 25-35°C for 10-20min to obtain Fe 3 o 4 Precursor solution is transferred to a three-necked flask, wherein the hollow Fe 3 o 4 The particle size of the nano-microspheres is 220-260nm, and the isopropanol solution is composed of deionized water and isopropanol in a volume ratio of 1:(2-4);

[0030] In the second step, take 30-50mLFe 3 o 4 Precursor solution, add 2.6~3mLNH 3 .H 2 O, stir at room temperature for 10-20min, then slowly add 0.9-1.1mLTEOS in batches and continue to stir for reaction, the reaction time is 5-7h;

[0031] The third step is to wash the ...

Embodiment 1

[0034] In the first step, the hollow Fe 3 o 4 Nanospheres were dissolved in isopropanol solution to form Fe with a mass concentration of 3.3 mg / mL 3 o 4 solution, sonicated at 25°C for 10 min to form Fe 3 o 4 Precursor solution is transferred to a three-necked flask, in which the hollow Fe 3 o 4 The particle size of the nanospheres is 220nm, and the isopropanol solution is composed of 10mL water and 20mL isopropanol;

[0035] The second step, to 30mL, the Fe obtained in the first step 3 o 4 Add 2.6mL NH to the precursor solution 3 .H 2 O, stirred at room temperature for 10 min, then slowly added 0.9mLTEOS in portions at room temperature and continued to stir the reaction, the reaction time was 5h;

[0036] In the third step, the product obtained in the second step was washed with absolute ethanol and deionized water several times, redispersed in 80mL of deionized water, then added 0.8g of PVPK15, stirred at 90°C, and the reaction time was 2.5h , adding 0.6g NaOH to ...

Embodiment 2

[0039] In the first step, the hollow Fe 3 o 4 Nanospheres were dissolved in isopropanol solution to form Fe with a mass concentration of 3.3 mg / mL 3 o 4 solution, sonicated at 30°C for 15 min to form Fe 3 o 4 Precursor solution is transferred to a three-necked flask, in which the hollow Fe 3 o 4 The particle size of the nanospheres is 240nm, and the isopropanol solution is composed of 10mL water and 30mL isopropanol;

[0040] The second step, to 40mL, the Fe obtained in the first step 3 o 4 Add 2.8mL NH to the precursor solution 3 .H 2 O, stirred at normal temperature for 15min, then slowly added 1.0mLTEOS in portions at normal temperature and continued to stir the reaction, the reaction time was 6h;

[0041] In the third step, the product obtained in the second step was washed with absolute ethanol and deionized water several times, redispersed in 80mL of deionized water, and then 0.9g of PVPK15 was added, and the temperature of the water bath was raised to 95°C for...

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Abstract

The invention discloses a super-hydrophobic hollow Fe3O4 / mesoporous silicon dioxide nanocomposite which is of a core-shell structure. Hollow Fe3O4 nano microspheres serve as magnetic cores, SiO2 serves as shells, the particle size of the cores ranges from 220 nm to 260 nm, the thickness of the shells ranges from 35 nm to 50 nm, a SiO2 shell layer is of a mesoporous structure, and the surface of the composite is modified with vinyl and methyl. The invention further provides a preparation method of the composite. The method comprises the steps that firstly, the hollow Fe3O4 nano microspheres are ultrasonically dispersed in an isopropyl alcohol solution, then NH3.H2O is added at room temperature, and after the mixture is stirred evenly, tetraethyl orthosilicate is slowly added for several times; secondly, after a reaction is competed, washing is performed, then the mixture is dispersed in deionized water, and under the protection of polyvinylpyrrolidone K15, NaOH is added for surface etching; thirdly, the surface hydrophobicity is modified through vinyl trimethoxy silane, and the super-hydrophobic hollow Fe3O4 / mesoporous silicon dioxide nanocomposite is finally obtained. The composite is light and porous, can effectively absorb oil and lock oil, can be recycled and reused and has a great application prospect in the aspect of oil pollution treatment.

Description

technical field [0001] The present invention specifically relates to a superhydrophobic hollow Fe 3 o 4 The invention relates to a mesoporous silicon dioxide nanocomposite material, a preparation method and an application thereof, belonging to the technical field of environment-friendly oil-absorbing materials. Background technique [0002] In recent years, water pollution incidents caused by oil have occurred frequently. Oil pollution not only affects the natural ecological environment, but also poses a huge threat to human beings. Studies have shown that the toxic and harmful substances in diesel, gasoline, and kerosene are harmful to human systems, and the aromatic hydrocarbons in petroleum, especially polycyclic aromatic hydrocarbons, are relatively toxic and have strong carcinogenic effects. The problem of oil pollution has attracted worldwide attention. To deal with oil spills quickly, efficiently, simply, and in a green and environmentally friendly way can fundame...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28
Inventor 姜炜郁榴华谢覃郝嘎子施金秋尹作柱彭铮陆月张娜李凤生
Owner NANJING UNIV OF SCI & TECH
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