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Preparation method and application of core-shell hollow structured MoO3 @ mSiO2 microspheres

A microsphere, m-6sio2 technology, which is applied in the field of preparation of core-shell hollow nanocomposite materials, can solve the problems of polluted environment, equipment corrosion, and many side reactions, and achieves the effects of less by-products, no corrosion, and less pollution.

Active Publication Date: 2013-12-11
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The industry mainly uses concentrated sulfuric acid as a catalyst to synthesize butyl acetate, which not only pollutes the environment, but also severely corrodes equipment, and has poor selectivity and many side reactions (G.Mitran, et al.Esterification of acetic acid with n-butanol using molybdenum oxides supported onγ- Alumina, Catal. Lett., 2010, 140(1-2), 32-37)

Method used

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  • Preparation method and application of core-shell hollow structured MoO3 @ mSiO2 microspheres
  • Preparation method and application of core-shell hollow structured MoO3 @ mSiO2 microspheres
  • Preparation method and application of core-shell hollow structured MoO3 @ mSiO2 microspheres

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1# core-shell hollow structure MoO 3 mSiO 2 The concrete preparation steps of catalyst are as follows:

[0039] (1) Preparation of cetyltrimethylammonium phosphomolybdate:

[0040] Measure 100mL of absolute ethanol into a beaker, add 0.4g of CTAB, stir until CTAB is completely dissolved, measure 50mL of absolute ethanol into another beaker, add 0.75g of phosphomolybdic acid, and stir with a glass rod until the phosphomolybdenum The acid is all dissolved. While stirring, use a dropper to drop the phosphomolybdic acid solution into the CTAB solution. After the addition is complete, continue to stir for half an hour to make it fully react. After filtering and drying, the product quaternary ammonium phosphomolybdic acid was obtained, which was denoted as M-6.

[0041] (2) M-6SiO2 2 Preparation of microspheres:

[0042] Weigh 80mg of M-6, put it into a round bottom flask, add 15mL of absolute ethanol, disperse in ultrasonic wave for 30min, until the solid is completely...

Embodiment 2

[0046] 2# core-shell hollow structure MoO 3 mSiO 2 The concrete preparation steps of catalyst are as follows:

[0047] (1) Preparation of M-6:

[0048] With the preparation method of M-6 among the embodiment 1.

[0049] (2) M-6SiO2 2 Preparation of microspheres:

[0050] Weigh 80mg of M-6, put it into a round bottom flask, add 15mL of absolute ethanol, disperse in ultrasonic wave for 30min, until the solid is completely dispersed, add 60mL of distilled water dropwise, and keep stirring at 28°C. After stirring for 6h, add 0.14mL ammonia water and 0.10mLTEOS, continue stirring at constant temperature for 16h, filter and dry to obtain M-6SiO 2 Microspheres.

[0051] (3) MoO 3 mSiO 2 Preparation of microspheres:

[0052] Same as the preparation method of step (3) in Example 1.

Embodiment 3

[0054] 3# core-shell hollow structure MoO 3 mSiO 2 The concrete preparation steps of catalyst are as follows:

[0055] (1) Preparation of M-6:

[0056] With the preparation method of M-6 among the embodiment 1.

[0057] (2) M-6SiO2 2 Preparation of microspheres:

[0058] Weigh 80mg of M-6, put it into a round bottom flask, add 15mL of absolute ethanol, disperse in ultrasonic wave for 30min, until the solid is completely dispersed, add 60mL of distilled water dropwise, and keep stirring at 28°C. After stirring for 6h, add 0.14mL ammonia water and 0.05mLTEOS, continue stirring at constant temperature for 16h, filter and dry to obtain M-6SiO 2 Microspheres.

[0059] (3) MoO 3 mSiO 2 Preparation of microspheres:

[0060] Same as the preparation method of step (3) in Example 1.

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Abstract

The invention discloses a preparation method of MoO3 @ mSiO2 microspheres, belonging to the technical field of nano material preparation. The preparation method comprises the following steps: through taking hexadecyl trimethyl ammonium phosphomolybdate as a core, coating the core with a layer of SiO2 by using a sol gel method, and then calcining the obtained product so as to obtain a core-shell hollow structured MoO3 @ mSiO2 microsphere. The MoO3 @ mSiO2 microsphere is good in dispersity, has a particle size of 200-900 nm and is of a hollow core-shell structure, the core is MoO3, and a shell is porous SiO2. The microsphere has a good catalytic effect on an esterification reaction between acetic acid and butanol for synthesizing butyl acetate; and under the reaction conditions that the reaction temperature is 150 DEG C, the molar ratio of acetic acid to butanol is 1:5, the application amount of a catalyst accounts for 36% of the mass of the acetic acid and the reaction time is 3h, the esterification rate of the acetic acid can reach 93.8%.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to the preparation and application of a core-shell hollow nanocomposite material. Background technique [0002] Core-shell particles are nanoscale ordered assembly structures formed by one nanomaterial wrapping another nanomaterial through chemical bonds or other forces. Core-shell nanoparticles show comprehensive properties that are different from both core materials and shell materials (Liu Dexin et al., Advances in Chemical Preparation and Application of Core-Shell Nanomagnetic Composite Particles, Polymer Materials Science and Engineering, 2011 ,27(12),172-175.C.Chen,et al.CuO nanoclusters coated with mesoporous SiO 2 as highly active and stable catalysts for olefin oxidation, J. Mater. Chem., 2011, 21, 5774-5779). The introduction of shell components can not only increase the stability and dispersion performance of the central particle, but also endow the ce...

Claims

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Application Information

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IPC IPC(8): B01J23/28B01J35/02B82Y30/00C07C69/14C07C67/08
Inventor 陈国昌刘猛乔红斌裘小宁蒋伟峰吴胜华
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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