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Preparation method of MCM-49/MCM-41 microporous-mesoporous composite molecular sieve

A technology of MCM-49 and MCM-41, which is applied in the field of preparation of microporous-mesoporous composite molecular sieves, can solve the problems of long cycle, environmental pollution, complex synthesis process, etc. less effect

Active Publication Date: 2014-09-24
HEILONGJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention provides a method for preparing a microporous-mesoporous MCM-49 / MCM-41 composite molecular sieve in order to solve the problems of complex synthesis process, long period and environmental pollution existing in the existing method

Method used

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  • Preparation method of MCM-49/MCM-41 microporous-mesoporous composite molecular sieve
  • Preparation method of MCM-49/MCM-41 microporous-mesoporous composite molecular sieve

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specific Embodiment approach 1

[0028] Embodiment 1: The preparation method of a kind of microporous-mesoporous MCM-49 / MCM-41 composite molecular sieve of the present embodiment is carried out according to the following steps:

[0029] 1. Add cetyltrimethylammonium bromide to distilled water, and stir for 8min to 12min at a temperature of 30 to 40°C and a stirring speed of 400r / min to 800r / min to obtain a clear solution; The ratio of the quality of the cetyltrimethylammonium bromide to the volume of distilled water is (0.5~1.5) g: 26mL;

[0030]2. Use ammonia water to adjust the pH value of the clarified solution obtained in step 1 to a pH value of 9 to 12, then add tetraethyl orthosilicate at a rate of 0.5 mL / min to 2 mL / min, and then add it at a temperature of 15 to 35 ° C and Stir at a stirring speed of 400r / min to 800r / min until a white gel is obtained; The mass ratio is (4.3~14.3):1;

[0031] 3. Add MCM-49 microporous molecular sieves to the white gel obtained in step 2, and then stir for 2h to 4h at ...

specific Embodiment approach 2

[0036] Embodiment 2: This embodiment differs from Embodiment 1 in that the ratio of the mass of cetyltrimethylammonium bromide described in step 1 to the volume of distilled water is 1.1 g: 26 mL. Other steps and parameters are the same as those in the first embodiment.

specific Embodiment approach 3

[0037] Embodiment 3: This embodiment is different from Embodiment 1 or 2 in that: in step 1, stir for 10 min at a temperature of 35° C. and a stirring speed of 600 r / min. Other steps and parameters are the same as those in Embodiment 1 or 2.

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Abstract

The invention relates to a preparation method of an MCM-49 / MCM-41 microporous-mesoporous composite molecular sieve, which solves the problems of complicated synthetic process, long cycle and environmental pollution in an existing method. The method comprises the following steps: 1, adding cetyl trimethyl ammonium bromide into distilled water, and stirring for dissolving to obtain a clear solution; 2, adjusting the pH value by using ammonia water, adding ethyl orthosilicate, and stirring to obtain white gel; 3, adding an MCM-49 microporous molecular sieve, and stirring to obtain a mixed gel solution; 4, transferring to a reaction kettle configured with a polytetrafluoroethylene liner tube, and performing crystallization reaction to obtain a white solid-liquid mixture; 5, performing suction filtration, performing drip washing on solid matters by using ethanol, drying, and roasting to finally obtain the MCM-49 / MCM-41 microporous-mesoporous composite molecular sieve. The method is simple in process, short in synthetic cycle, low in environmental pollution and good in repeatability.

Description

technical field [0001] The invention relates to a preparation method of a microporous-mesoporous composite molecular sieve. Background technique [0002] In order to overcome the shortcomings of relatively small pore size of microporous molecular sieves and amorphous pore walls of mesoporous molecular sieves, researchers have developed microporous-mesoporous composite molecular sieves with double acidity and double pore structure. The amorphous pore wall of the mesoporous molecular sieve is crystallized or partially crystallized, so that the synthesized molecular sieve has uniform and adjustable mesopores, and the pore wall is highly crystallized. Larger mesopores can provide channels for macromolecular reactions, and the crystallization or partial crystallization of the pore walls provides the possibility for shape-selective catalysis of small molecules or macromolecular catalysis that requires stronger acid centers. Therefore, microporous-mesoporous composite molecular si...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02
Inventor 魏立国董永利宋微娜程志刚刘晓旭薛丽梅丁慧贤解丽萍宋坤垚
Owner HEILONGJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY