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Preparation method of mesoporous composite taking chelate surfactant as template

A surfactant and composite technology, applied in the fields of nanostructure manufacturing, nanotechnology, nanotechnology, etc., can solve the problems of long period, uneven particle distribution, and complex reaction equipment.

Inactive Publication Date: 2012-03-14
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction device of the traditional method is complicated, the cycle is long, and the operation is difficult, and it often cannot solve the problems of uneven distribution of particles in the pores and difficult control of the blending amount.

Method used

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  • Preparation method of mesoporous composite taking chelate surfactant as template
  • Preparation method of mesoporous composite taking chelate surfactant as template
  • Preparation method of mesoporous composite taking chelate surfactant as template

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] At 42°C, 0.127g (0.435mmol) Ni(NO 3 ) 2 ·6H 2 O was added to 40 mL of 0.027 mol / L sodium N-dodecylethylenediaminetriacetate solution and stirred vigorously for 2 hours to form a uniform and stable blue solution. The pH of the system was adjusted to 6 with 0.1 mol / L hydrochloric acid solution, and the stirring was continued for 2 hours.

[0030] Add 0.523g (2.92mmol) 3-aminopropyltrimethoxysilane to the aqueous chelate system, and when the color of the solution starts to turn white, quickly add 0.90g (4.32mmol) tetraethyl orthosilicate, and stir for 3 minutes.

[0031] The reaction bottle was taken out and aged at room temperature for 48 hours, then the precipitate was filtered and washed with deionized water until the washing liquid was neutral. The precipitate was collected and dried, and the resulting product was calcined in a muffle furnace at 560 °C for 5 hours to obtain NiO / SiO 2 mesoporous complex.

Embodiment 2

[0033] At 45°C, 0.208g (0.872mmol) Co(Cl) 2 ·6H 2 O was added to 40 mL of 0.027 mol / L sodium N-tetradecyl ethylenediamine triacetate solution, and stirred vigorously for 2 hours to form a uniform and stable lavender-red solution. The pH value of the system was adjusted to 6.8 with 0.1 mol / L NaOH solution, and the stirring was continued for 2 hours.

[0034] Add 0.581g (3.24mmol) 3-aminopropyltrimethoxysilane to the chelate solution system, and when the color of the solution starts to turn white, quickly add 1.12g (5.39mmol) tetraethyl orthosilicate, and stir for 3 minutes.

[0035] The reaction bottle was taken out and aged at room temperature for 64 hours, then the precipitate was filtered and washed with deionized water until the washing liquid was neutral. The precipitate was collected and dried, and the resulting product was calcined in a muffle furnace at 580 °C for 6 hours to obtain Co 3 o 4 / SiO 2 mesoporous complex.

Embodiment 3

[0037] At 48°C, 0.063g (0.217mmol) Ni(NO 3 ) 2 ·6H 2 O with 0.052g (0.218mmol) Co(Cl) 2 ·6H 2 O was added to 40 mL of 0.027 mol / L sodium N-hexadecyl ethylenediamine triacetate solution and stirred vigorously for 2 hours to form a uniform and stable dark blue solution. The pH value of the system was adjusted to 6.5 with 0.1 mol / L hydrochloric acid solution, and the stirring was continued for 2 hours.

[0038] Add 0.542g (3.02mmol) 3-aminopropyltrimethoxysilane to the chelate solution system, and when the color of the solution starts to turn white, quickly add 1.01g (4.86mmol) tetraethyl orthosilicate, and stir for 3 minutes.

[0039] The reaction bottle was taken out and aged at room temperature for 72 hours, then the precipitate was filtered and washed with deionized water until the washing liquid was neutral. The precipitate was collected and dried, and the resulting product was calcined in a muffle furnace at 600 °C for 7 hours to obtain NiO-Co 3 o 4 / SiO 2 mesoporou...

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Abstract

The invention discloses a preparation method of a mesoporous composite taking a chelate surfactant as a template, belonging to the technical field of preparation of mesoporous composites. The mesoporous composite with the particle size being between 300 nm and 500 nm, the specific surface being between 450 m<2> / g and 900 m<2> / g, the pore size distribution being between 3 nm and 8 nm and the opening structure being in a long-range order is made by the method comprising the following steps: mixing one of Mn, Fe, Co, Cd, Zn, Pb, Cu, Ni and Hg or a mixed metal salt and N-alkyl ethylenediamine sodium triacetate in a water solution to form a soluble chelate; regulating the pH value of the solution, taking the chelate surfactant containing a metal ion as the template and obtaining a mesoporous composite precipitate by adding a structure directing agent, i.e. 3-aminopropyl trimethoxy silane and tetraethyl orthosilicate and stirring violently; precipitating at a room temperature, aging for 48 to 72 hours, filtering, washing and drying before roasting the obtained powder at 500 to 600 DEG C. Due to directional introduction action of the chelate surfactant, the metal in the composite is eventually distributed uniformly in the mesopore opening in the form of nanometer oxide.

Description

technical field [0001] The invention discloses a method for preparing a mesoporous complex using a chelating surfactant as a template, and belongs to the technical field of mesoporous complex preparation. Background technique [0002] Mesoporous composites refer to materials composed of nanoscale metal or nonmetal (such as organic polymers, noble metals and their oxides, etc.) particles placed in the pores of mesoporous solids by physical or chemical methods. Since mesoporous molecular sieves have the periodicity and topological perfection of channel space or nanocages, introducing inorganic semiconductors, organic polymers and other substances into cages or channels by chemical modification can greatly improve the performance of mesoporous molecular sieves and form excellent Functionalized mesoporous molecular sieve materials. This new type of material has high porosity (pore size 2-50nm) and high specific surface area, and the interaction between pores and particle interf...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B82B3/00
Inventor 陈明清牛奎倪忠斌傅成武刘晓亚
Owner JIANGNAN UNIV
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