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Method for synthesizing MCM-48 mesoporous silica

A mesoporous silica, MCM-48 technology, applied in the direction of silica, silicon oxide, etc., can solve the problems of pollution caused by fluoride ion environment, and achieve the effect of saving surfactant, high degree of order, and uniform pore size

Inactive Publication Date: 2017-08-08
TAISHAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses sodium fluoride (NaF), a crystallization agent, in which a large amount of fluoride ions are likely to pollute the environment

Method used

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  • Method for synthesizing MCM-48 mesoporous silica
  • Method for synthesizing MCM-48 mesoporous silica
  • Method for synthesizing MCM-48 mesoporous silica

Examples

Experimental program
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Effect test

Embodiment 1

[0021] The features of the present invention are further described below through examples, but the present invention is not limited to the following examples.

[0022] The scanning electron micrographs of the materials in the examples were measured by a DSM 962 scanning electron microscope from Zeiss Company, Germany.

[0023] The transmission electron micrographs of the materials in the examples were measured by a Tecnai G2 F20 S-Twin type transmission electron microscope from FEI Company of the United States.

[0024] The scanning electron specific surface area, pore diameter, and pore volume of the materials in the examples were measured using an Autosorb-IQ gas adsorption instrument from Quanta Corporation, USA.

[0025] The XRD of the materials in the examples is measured by a D / max-rB X-ray diffractometer of Rigaku Corporation.

[0026] The thermogravimetric curves of the materials in the examples were measured with a DTG-60AH thermal analyzer from Shimadzu Corporation ...

Embodiment 2

[0030] Take 2.48g of tetradecyltrimethylammonium bromide and 0.13g of 2-hydroxy-3-naphthoic acid dissolved in 60 ml of water at room temperature, stir for 0.5 h to obtain A solution, another 63.11 g of Na 2 SiO 3 9H 2 Dissolve O in 60 ml of water to obtain solution B; quickly mix solution A and solution B, and add 2 mol / L sulfuric acid solution drop by drop to the above mixture under vigorous stirring until the pH is 9-10; Heated at constant temperature in an oven for 48 hours, filtered the obtained solid precipitate, washed with water and dried in air to obtain a composite product; the resulting composite product was placed in a muffle furnace and heated in air at a speed of 1.5°C / min to The product can be obtained by calcination at constant temperature at 600°C for 5 hours.

Embodiment 3

[0032] Take 2.48g tetradecyltrimethylammonium bromide and 0.35g 2-hydroxy-3-naphthoic acid dissolved in 60 ml water at room temperature, stir for 0.5 h to obtain A solution, and take another 63.11 g Na 2 SiO 3 9H 2 Dissolve O in 60 ml of water to obtain solution B; quickly mix solution A and solution B, and add 2 mol / L sulfuric acid solution drop by drop to the above mixture under vigorous stirring until the pH is 9-10; Heating at constant temperature in an oven for 48 hours, filtering the obtained solid precipitate, washing with water and drying in air to obtain a composite product; placing the obtained composite product in a muffle furnace and heating it in air at a speed of 1.5 °C / min to The product can be obtained by calcination at constant temperature at 600°C for 5 hours.

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Abstract

The invention discloses a method for synthesizing MCM-48 mesoporous silica. The method utilizes tetradecyl trimethyl ammonium bromide (C14TAB) and 2-hydroxyl-3-naphthoic acid (NaHN) as template agents and sodium silicate (Na2SiO3.9H2O) as a silicon source. The method comprises the following synthesizing steps: completely dissolving C14TAB into water and then adding NaHN; additionally taking Na2SiO3.9H2O to be completely dissolved into water; then quickly mixing two kinds of solution, stirring for 20 minutes in room temperature and then adding 2mol / L sulfuric acid drop by drop; transferring a mixture into 100 DEG C water in a high-pressure kettle, heating for 48 hours, filtering, washing and putting in air to be dried; then roasting for 6 hours in a 560 DEG C muffle furnace to remove organic matter to obtain a product. Raw material ratio of C14TAB / NaHN / Na2SiO3.9H2O / H2SO4 / H2O is 1 : (0.15 to 0.27) : 30 : 30 : 900. The raw materials of the C14TAB, the NaHN and the Na2SiO3.9H2O utilized by the method disclosed by the invention are easy to obtain, so that production cost is greatly reduced. A fluorine-containing additive is avoided in a production process, so that environmental friendliness is achieved, a product is high in order degree and uniform in pore diameter, and large-scale industrial production is facilitated.

Description

technical field [0001] The invention relates to a preparation method of porous silicon dioxide molecular sieve, in particular to a preparation method of low-cost synthetic silicon-based mesoporous MCM-48. Background technique [0002] MCM-48 mesoporous silica is one of the series of mesoporous silica materials developed by Mobil Corporation. This kind of mesoporous material is different from MCM-41 and MCM-50 series in that it has three three-dimensional intersecting channels with high symmetry. Compared with one-dimensional channels, three-dimensional channels are more conducive to the transmission of reactants and products, and are less likely to be blocked. Therefore, MCM-48 mesoporous materials have better application prospects in the fields of selective catalysis, adsorption, and separation. However, the synthesis conditions of the MCM-48 series are harsh, the reproducibility is poor, and the synthesis cost is high, so there are relatively few research papers and pate...

Claims

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Application Information

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IPC IPC(8): C01B33/12
CPCC01B33/12C01P2002/72C01P2004/03C01P2004/04C01P2006/12C01P2006/16
Inventor 朱延美王仁亮葛海燕
Owner TAISHAN MEDICAL UNIV
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