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Small-sized metallic oxide nano-cluster/mesoporous SiO2 nanocomposite and preparation method thereof

A nano-composite material and oxide technology, which is applied in the field of nano-material preparation and heterogeneous catalysis, can solve the problems of long reaction time and complicated process, and achieve the effect of small size, relatively large pore size and large specific surface area.

Active Publication Date: 2016-10-12
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2015, Kuroda et al. prepared mesoporous silica with a particle size of 20 nm and a pore size of 5 nm by hydrocolloid method using methyl orthosilicate as a silicon source and triisopropylbenzene as an additive at 80 °C for 12 h. ~8nm, this preparation method takes a long time to react and the process is relatively complicated (Nanoscale, 2015, 7, 19557)

Method used

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  • Small-sized metallic oxide nano-cluster/mesoporous SiO2 nanocomposite and preparation method thereof
  • Small-sized metallic oxide nano-cluster/mesoporous SiO2 nanocomposite and preparation method thereof
  • Small-sized metallic oxide nano-cluster/mesoporous SiO2 nanocomposite and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0029]Add 0.01mol of cationic surfactant cetyltrimethylammonium chloride into the flask, then add 11mL of cyclohexane, 3mL of n-butanol, and 0.6mL of ammonia water into the flask, stir at 25°C for 3min, and then Add 50 μL ammonium molybdate (0.05 mol / L ammonium molybdate aqueous solution) and continue stirring for 40 min. Measure 0.08 mL of ethyl orthosilicate, add octadecyltrimethoxysilane, make the molar ratio of octadecyltrimethoxysilane: ethyl orthosilicate to be 1:4, and react for 2 hours. After the reaction is finished, isopropanol is added, and then undergoes ultrasonication, centrifugation, washing, roasting, and natural cooling to obtain the target product. The roasting process is as follows: during the whole roasting process, air with a flow rate of 20mL / min is introduced, and the temperature is programmed from room temperature to 250 °C at a rate of 5 °C / min, and then roasted for 30 minutes, and then the temperature is programmed to rise to 300 °C at a rate of 2 °C / ...

Embodiment 2

[0031] 0.01 mol of cationic surfactant cetyltrimethylammonium bromide was added to the flask, and then 17 mL of cyclohexane, 5 mL of n-butanol and 0.8 mL of ammonia water were added to the flask. Stir at 35°C for 3 min, then add 50 μL ammonium molybdate (0.1 mol / L ammonium molybdate aqueous solution) and continue stirring for 40 min. Measure 1.8mL tetraethyl orthosilicate, add octadecyltrimethoxysilane, make C 18 The molar ratio of TMS to TEOS was 1:4, and the reaction was 2h. After the reaction is finished, isopropanol is added, and then undergoes ultrasonication, centrifugation, washing, roasting, and natural cooling to obtain the target product. The roasting process is as follows: during the entire roasting process, air with a flow rate of 30mL / min is introduced, and the temperature is programmed from room temperature to 250 °C at a rate of 10 °C / min, and the temperature is programmed to rise to 500 °C at a rate of 5 °C / min. Calcined for 2 hours to get MoO 3 Nanocluster / ...

Embodiment 3

[0034] Take 0.01mol of cationic surfactant cetyltrimethylammonium chloride and add it into the flask, then add 19mL of cyclohexane, 5.5mL of n-butanol, and 1mL of ammonia water into the flask, stir at 45°C for 3min, and then Add 50 μL ammonium molybdate (0.2 mol / L ammonium molybdate aqueous solution) and continue stirring for 40 min. Measure 6 mL of ethyl orthosilicate, add octadecyltrimethoxysilane to make the molar ratio of octadecyltrimethoxysilane: ethyl orthosilicate is 1:40, and react for 2 hours. After the reaction is finished, isopropanol is added, and then undergoes ultrasonication, centrifugation, washing, roasting, and natural cooling to obtain the target product. The roasting process is as follows: during the whole roasting process, air with a flow rate of 40mL / min is introduced, and the temperature is programmed from room temperature to 250 °C at a rate of 2 °C / min, and then roasted for 50 minutes, and then the temperature is programmed to rise to 380 °C at a rate...

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Abstract

The invention belongs to the field of nanometer material preparation and particularly relates to a small-sized metallic oxide nano-cluster / mesoporous SiO2 nanocomposite and a preparation method thereof. The particle size and the pore diameter of every mesoporous SiO2 nanosphere carrier are 5-30 nm and 2-5 nm respectively; every metallic oxide nano-cluster refers to MoO3 or WO3 and 0.1-2 nm in particle size. A reversed-phase microemulsion method is adopted for synthesis. The preparation method of the small-sized metallic oxide nano-cluster / mesoporous SiO2 nanocomposite is simple in technology, economic and safe; the metallic oxide nano-clusters are highly dispersed on the mesoporous SiO2 carrier, the metallic oxide nano-clusters and the mesoporous SiO2 carrier are controllable in both size and shape, and accordingly the small-sized metallic oxide nano-cluster / mesoporous SiO2 nanocomposite is excellent in catalytic performance.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation and heterogeneous catalysis, and relates to a kind of MoO 3 / Mesoporous SiO 2 and WO 3 / Mesoporous SiO 2 Nanocomposite materials and their synthesis methods, especially related to the preparation of MoO with inverse microemulsion as a reaction system 3 / Mesoporous SiO 2 and WO 3 / Mesoporous SiO 2 nanocomposites. Background technique [0002] Mesoporous silica is a non-toxic material. Due to its high chemical stability and biocompatibility, as well as its huge specific surface area and uniform and adjustable pores, it is a carrier with excellent properties. , separation, adsorption and drug transport play an important role. Therefore, the preparation of mesoporous silica with high specific area and high pore volume has become a research hotspot of scholars, and many preparation methods have been developed so far. [0003] In the 1890s, Exxon Mobil used the principle of liq...

Claims

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Application Information

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IPC IPC(8): B01J23/28B01J23/30B01J35/10B82Y30/00C10G27/00
CPCC10G27/00B82Y30/00B01J23/28B01J23/30B01J35/61B01J35/63B01J35/647
Inventor 王加升武文佩包明
Owner DALIAN UNIV OF TECH
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