Method for preparing large-pore mesoporous molecular sieve

A technology of mesoporous molecular sieves and large pore diameters, applied in the direction of crystalline aluminosilicate zeolites, etc., can solve the problems of low reaction activity, low hydrothermal stability, and increased pore wall thickness, and achieve simple synthesis methods and high repeatability , the effect of improving the utilization rate

Inactive Publication Date: 2014-12-10
EAST CHINA NORMAL UNIV
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  • Application Information

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Problems solved by technology

However, the large-scale synthesis of mesoporous materials, low hydrothermal stability, and low reactivity have not been resolved.
The direct high-temperature hydrothermal synthesis strategy can greatly increase the pore size, but the thickness of the pore wall does not increase significantly. Compared with the mesoporous materials synthesized at low temperature, the hydrothermal stability is slightly improved (Eur. J. Inorg. Chem. 2011, 59.)

Method used

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  • Method for preparing large-pore mesoporous molecular sieve
  • Method for preparing large-pore mesoporous molecular sieve

Examples

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Comparison scheme
Effect test

Embodiment 1

[0019] Synthesis of MCM-41 mesoporous material: The pure silicon macroporous MCM-41 mesoporous material was synthesized by the method reported in the literature, which was used as the starting material for the synthesis of macroporous MCM-41 mesoporous material. Take 50 ml of tetramethylammonium bromide solution with a molar concentration of 0.05 M, add 1.50 g of pure silicon MCM-41 mesoporous material containing surfactant, stir for 30 minutes, then transfer the mixture into a stainless steel reaction kettle, 150 °C After 2 days of crystallization, a macroporous MCM-41 mesoporous molecular sieve was obtained. The X-ray diffraction (XRD) and scanning electron microscope (SEM) characterization of the sample is as follows: figure 1 and figure 2 shown.

Embodiment 2

[0021] Synthesis of MCM-48 mesoporous material: The method reported in the literature was used to synthesize pure silicon MCM-48 mesoporous material as the starting material for the synthesis of macroporous MCM-48 mesoporous material. Take 50 ml of tetramethylammonium bromide solution with a molar concentration of 0.05 M, add 1.50 g of pure silicon MCM-48 mesoporous material containing surfactant, mix well, continue to stir for 30 minutes, and then transfer the mixture into a stainless steel reaction kettle Crystallization at 160°C for 2 days to obtain macroporous MCM-48 mesoporous molecular sieves.

Embodiment 3

[0023] Synthesis of SBA-15 mesoporous material: The pure silicon SBA-15 mesoporous material was synthesized by the method reported in the literature, and the block copolymer was removed by calcination at 550°C as the initial material for the synthesis of Al-SBA-15 mesoporous material. Take 50 ml of tetramethylammonium bromide solution with a molar concentration of 0.05 M, add 1.0 g of pure silicon SBA-15 mesoporous material roasted at high temperature, mix well, continue stirring for 30 minutes, and then transfer the mixture into a stainless steel reaction kettle, Crystallize at 170°C for 1 day to obtain a macroporous SBA-15 mesoporous molecular sieve.

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Abstract

The invention discloses a method for preparing a large-pore mesoporous molecular sieve. According to the method, a mesoporous molecular sieve with different topological structures is synthesized by using the methods reported in literature, then a certain amount of mesoporous molecular sieve raw powders or roasting samples are mixed with a solution containing small molecule organic ammonium with a certain concentration, and the large-pore mesoporous molecular sieve is prepared through controlling the crystallization temperature and crystallization time by using hydrothermal synthesis. The synthesis method is simple and has high repeatability, and the mesoporous molecular sieve finally obtained has higher hydrothermal stability; and in addition, the synthesis method does not need additional silicon sources, the synthesis cost is reduced, and the method is an environment-friendly synthesis method.

Description

technical field [0001] The invention relates to a method for preparing mesoporous molecular sieves, in particular to a new method for preparing large-diameter mesoporous materials with high hydrothermal stability by using a hydrothermal post-synthesis strategy. Background technique [0002] After the birth of M41S series mesoporous materials with ordered and adjustable pore size, they have attracted extensive research interest due to their wide application in catalysis, adsorption and separation (Chem. Rev. 2007, 107, 2821). However, the large-scale synthesis of mesoporous materials, low hydrothermal stability, and low reactivity have not been resolved. The most typical mesoporous materials, such as MCM-41 and MCM-48, are usually synthesized at a mild temperature below 130°C, resulting in extremely unstable mesoporous structures with a wall thickness of less than 1 nm, and pure silicon MCM-41 / 48 Mesoporous materials do not have any reactivity (J. Am. Chem. Soc., 1992, 114, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 张坤马晓静蒋金刚徐浪浪袁恩辉杨太群
Owner EAST CHINA NORMAL UNIV
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