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

AI Technical Summary

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 t

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

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0028] Example 1

[0029] Take 0.01mol of the cationic surfactant cetyltrimethylammonium chloride and add it to the flask, and then add 11mL cyclohexane, 3mL n-butanol, 0.6mL ammonia to the flask, stir at 25℃ for 3min, then Add 50 μL of ammonium molybdate (0.05 mol / L ammonium molybdate aqueous solution) and continue stirring for 40 minutes. Measure 0.08 mL of ethyl orthosilicate, add octadecyltrimethoxysilane to make the molar ratio of octadecyltrimethoxysilane: ethyl orthosilicate 1:4, and react for 2h. After the reaction is over, isopropanol is added, and the target product is obtained through ultrasonic, centrifugal, washing, roasting process, and natural cooling. The specific roasting process is as follows: the air with a flow rate of 20mL / min is passed through the whole roasting process, the temperature is programmed from room temperature to 250℃ at a rate of 5℃ / min, and the temperature is roasted for 30 minutes, and then at a rate of 2℃ / min to 300℃ Calcination for 4h to g...

Example Embodiment

[0030] Example 2

[0031] Take 0.01 mol of the cationic surfactant cetyltrimethylammonium bromide and add it to the flask, and then add 17 mL of cyclohexane, 5 mL of n-butanol, and 0.8 mL of ammonia to the flask. Stir at 35°C for 3 min, then add 50 μL of ammonium molybdate (0.1 mol / L ammonium molybdate aqueous solution) and continue stirring for 40 min. Measure 1.8 mL of ethyl orthosilicate and add octadecyl trimethoxysilane to make C 18 The molar ratio of TMS to TEOS was 1:4, and the reaction was conducted for 2 hours. After the reaction is over, isopropanol is added, and the target product is obtained through ultrasonic, centrifugal, washing, roasting process, and natural cooling. The specific roasting process is as follows: the air with a flow rate of 30mL / min is introduced during the whole roasting process, the temperature is programmed from room temperature to 250℃ at a rate of 10℃ / min, and the temperature is roasted for 40 minutes, and then at a rate of 5℃ / min to 500℃. Ca...

Example Embodiment

[0033] Example 3

[0034] Take 0.01mol of the cationic surfactant cetyltrimethylammonium chloride and add it to the flask, then add 19mL cyclohexane, 5.5mL n-butanol, 1mL ammonia to the flask, stir at 45℃ for 3min, then Add 50 μL of ammonium molybdate (0.2mol / L ammonium molybdate aqueous solution) and continue stirring for 40 minutes. Measure 6 mL of ethyl orthosilicate, add octadecyltrimethoxysilane to make the molar ratio of octadecyltrimethoxysilane: ethyl orthosilicate 1:40, and react for 2h. After the reaction is over, isopropanol is added, and the target product is obtained through ultrasonic, centrifugal, washing, roasting process, and natural cooling. The specific roasting process is as follows: the air with a flow rate of 40mL / min is passed through the whole roasting process, the temperature is increased from room temperature to 250°C at a rate of 2°C / min, and then the temperature is increased to 380°C at a rate of 1°C / min. Calcination time 2h to get MoO 3 Nanocluster / ...

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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
CPCB01J23/28B01J23/30B01J35/1004B01J35/1033B01J35/1061B82Y30/00C10G27/00
Inventor 王加升武文佩包明
Owner DALIAN UNIV OF TECH
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