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Method for preparing MCM 48 molecular sieve

A technology of MCM-48 and molecular sieve, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of limiting the application of MCM-48 molecular sieve and long cycle.

Inactive Publication Date: 2006-05-24
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the long cycle of preparing MCM-48 molecular sieves, the application of MCM-48 molecular sieves is limited.

Method used

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  • Method for preparing MCM 48 molecular sieve

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preparation example Construction

[0013] The preparation method of said MCM-48 molecular sieve of the present invention comprises the steps:

[0014] (1) First place tetraethyl silicate and water in a container, then add sodium hydroxide and hexadecyltrimethylammonium bromide to the container in turn, stir for 30-40 minutes, and Under the condition of 30°C-40°C, add sodium fluoride into the container and stir for 1 hour to obtain a reaction mixture; among them, tetraethyl silicate, sodium hydroxide, cetyltrimethylammonium bromide , The molar ratio of water and sodium fluoride is 1: 0.25: 0.65: 60: 0.1~0.4;

[0015] (2) Transfer the reaction mixture obtained from step (1) into a polytetrafluoroethylene cup, conduct a hydrothermal crystallization reaction at 120° C. for 10 to 24 hours, then wash the product of the hydrothermal crystallization reaction until neutral, dry and Burn at 450-550°C for 2-6 hours to obtain the target product.

Embodiment 1～7

[0018]

[0019] The preparation of cubic mesoporous MCM-48 according to the above examples not only greatly shortens the reaction time, but also has good repeatability. The synthesized sample is characterized by XRD (X-ray diffraction) technology, and the structure of the product is judged from the strength of the characteristic peaks on the X-ray diffraction spectrum: the weaker the characteristic peak, the worse the pore structure ; The stronger the characteristic peak, the better the channel order. It can be seen from the attached figure that the XRD peak strength of MCM-48 synthesized without fluorine is very weak, indicating that the order of the pore structure is poor; the XRD peak strength of the sample synthesized after adding fluorine is greatly enhanced, and the eight characteristic peaks of MCM-48 All are clearly visible, indicating that the crystal form of the obtained MCM-48 is good, and the pores are long-range ordered.

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Abstract

The invention relates to a MCM-48 molecular sieve preparing method, including the main steps of: firstly in turn placing silicon source, alkali source, template agent and water soluble fluorine salt in a vessel; then making hydrothermal crystallization reaction at 0.1MPa; and finally washing, drying and baking the resultant to obtain the target matter. As compared with existing techniques, its remarkable advantage is shortening the preparing cycle of the MCM-48 molecular sieve.

Description

technical field [0001] The invention relates to a preparation method of a molecular sieve, in particular to a preparation method of a high-regularity silicon-based mesoporous molecular sieve MCM-48. Background technique [0002] In 1992, Mobil successfully developed the M41S series of mesoporous molecular sieves. M41S series mesoporous molecular sieves include MCM-41 with one-dimensional hexagonal structure, MCM-48 with three-dimensional cubic structure and layered unstable MCM-50. The pore size range of this type of molecular sieve is between 2-10 nanometers, and they have the following main excellent characteristics: ①The pores are well formed and the pore size is uniform; ②The pore size can be adjusted within a certain range; ③Have a high specific surface area and thermal stability ; ④ Based on the high degree of order on the micro scale. Therefore, it has good application prospects in catalysis, adsorption separation, host-guest combinatorial chemistry, etc. [0003] ...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 张金龙王灵芝邵耀锋陈锋
Owner EAST CHINA UNIV OF SCI & TECH