WO3@mSiO2 microballoon sphere with nuclear shell hollow structure as well as preparation method and application thereof

A core-shell structure and microsphere technology, applied in the field of nanomaterials, to achieve the effects of less by-products, high catalytic efficiency 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

(Julien Polleux, et.al., Template-Free Synthesis and Assembly of Single-Crystalline Tungsten Oxide Nanowires and their Gas-Sensing Properties, Angew. Chem. Int. Ed. 2005, 44, 267-271.) The closest to this patent Literature reports include: Zhang et al. (L. Zhang, et.al., Facile synthesis and photocatalytic activity of hierarchical WO 3 core-shell microspheres, Applied Surface Science, 2011, 258, 1719-1724) prepared core-shell WO 3 microspheres, and Liu et al. (J.Liu, et.al., Novel MoO 3 and WO 3 hollow nanospheres assembled with polymeric micelles, Materials Letters, 2012, 66, 25-28) prepared WO 3 Hollow spheres, they are prepared pure WO with different morphological structures 3 , while the hollow core-shell WO 3 mSiO 2 Composite microspheres have not been reported

Method used

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  • WO3@mSiO2 microballoon sphere with nuclear shell hollow structure as well as preparation method and application thereof
  • WO3@mSiO2 microballoon sphere with nuclear shell hollow structure as well as preparation method and application thereof
  • WO3@mSiO2 microballoon sphere with nuclear shell hollow structure as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1# core-shell hollow structure WO 3 mSiO 2 The concrete preparation steps of catalyst are as follows:

[0038] (1) Preparation method of cetyltrimethylammonium phosphotungstate:

[0039] Measure 100mL of absolute ethanol into a beaker, add 0.44g of cetyltrimethylammonium bromide (CTAB), stir until CTAB is completely dissolved, measure 50mL of absolute ethanol into another beaker, add 1.15g For phosphotungstic acid, stir with a glass rod until the phosphotungstic acid is completely dissolved. While stirring, use a dropper to add the phosphotungstic acid solution to the CTAB solution dropwise. After the addition is complete, continue to stir for half an hour to make it fully react. After filtering and drying, the product hexadecyltrimethylphosphotungstic acid quaternary ammonium was obtained, which was designated as W-6.

[0040] (2) W-6SiO2 2 Microsphere preparation method:

[0041] Weigh 200mg of W-6 and 110mg of CTAB into a round bottom flask, add 20mL of absolut...

Embodiment 2

[0045] 2# core-shell hollow structure WO 3 mSiO 2 The concrete preparation steps of catalyst are as follows:

[0046] (1) Preparation method of W-6:

[0047] With the preparation method of W-6 among the embodiment 1.

[0048] (2) W-6SiO2 2 Microsphere preparation method:

[0049] Weigh 200mg of W-6 and 110mg of CTAB into a round bottom flask, add 20mL of absolute ethanol, disperse in ultrasonic wave for 30min, until the solid is completely dispersed, add 50mL of distilled water dropwise, and keep stirring at 28°C. After stirring for 6h, add 0.3mL ammonia water and 0.6mL TEOS, continue stirring at constant temperature for 16 hours, filter and dry to obtain W-6SiO 2 Microspheres. WO prepared in embodiment 2 3 mSiO 2 The SEM pictures of the microspheres are shown in figure 2 .

[0050] (3) WO 3 mSiO 2 Preparation of microspheres

[0051] Same as the preparation method of step (3) in Example 1.

Embodiment 3

[0053] 3# core-shell hollow structure WO 3 mSiO 2 The concrete preparation steps of catalyst are as follows:

[0054] (1) Preparation method of W-6:

[0055] With the preparation method of W-6 among the embodiment 1.

[0056] (2) W-6SiO2 2 Microsphere preparation method:

[0057] Weigh 200mg of W-6 and 110mg of CTAB into a round bottom flask, add 20mL 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 0.3mL ammonia water and 0.6mL TEOS, continue stirring at constant temperature for 16 hours, filter and dry to obtain W-6SiO 2 Microspheres.

[0058] (3) WO 3 mSiO 2 Preparation of microspheres

[0059] Same as the preparation method of step (3) in Example 1.

[0060] WO prepared in embodiment 3 3 mSiO 2 The SEM pictures of the microspheres are shown in figure 1 . Depend on figure 1 It can be seen that the dispersion and unifo...

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Abstract

The invention discloses a prepared WO3@mSiO2 microballoon sphere as well as a preparation method and an application thereof, belonging to the technical field of preparation of nano materials. The preparation method comprises the steps of utilizing hexadecyl trimethyl ammonium phosphotungstate as a nucleus and covering one layer of SiO2 by adopting a sol-gel method; then calcining to obtain the WO3@mSiO2 microballoon sphere with a nuclear shell hollow structure. The WO3@mSiO2 microballoon sphere is good in dispersity, has a grain diameter of 500nm-600nm and has the nuclear shell hollow structure; the nucleus is WO3 and the shell is porous SiO2. The microballoon sphere has a very good catalytic effect on an esterification reaction for synthesizing methyl oleate (biodiesel) by taking oleic acid and methanol as raw materials; the reaction temperature is 90 DEG C and the reaction time is 8 hours; the mass ratio of the oleic acid to the methanol is 1 to 5.2; the esterification rate of the oleic acid can be up to 97.6% under the condition that the use amount of a catalyst is 36% of the mass of the oleic acid.

Description

technical field [0001] The invention relates to the technical field of nanomaterials, in particular to a core-shell hollow nanocomposite material and its preparation method and application. 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 centr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/30B01J35/08C11C3/04C07C69/58C07C67/08
CPCY02E50/13Y02E50/10
Inventor 陈国昌赵晓乔红斌裘小宁蒋伟峰吴胜华
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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