M-MCM-41 mesoporous molecular sieve with high transition metal content and high regularity and preparation method thereof

A M-MCM-41, mesoporous molecular sieve technology, applied in the field of molecular sieves, can solve the problems of low framework metal content and uneven distribution of molecular sieve framework structure, and achieve the effect of expanding the scope of application and large industrial application value

Inactive Publication Date: 2013-09-18
李潇
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  • Abstract
  • Description
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Problems solved by technology

[0007] The present invention aims to provide a method for preparing mesoporous molecular sieve M-MCM-41 with high transition metal content and high regularity to solve the problem of low content of framework metal in heteroatom mesoporous molecular sieves in the prior art and the distribution of metals in the framework structure of molecular sieves. uneven problem

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  • M-MCM-41 mesoporous molecular sieve with high transition metal content and high regularity and preparation method thereof
  • M-MCM-41 mesoporous molecular sieve with high transition metal content and high regularity and preparation method thereof
  • M-MCM-41 mesoporous molecular sieve with high transition metal content and high regularity and preparation method thereof

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preparation example Construction

[0025] In a typical embodiment of the present invention, a preparation method of M-MCM-41 mesoporous molecular sieve with high transition metal content and high regularity is provided, the transition metal M is a group consisting of Ni, Co and Cu Any one of them, the preparation method comprises the following steps: (1), preparing the ionic association formed by the complex of transition metal and cationic surfactant [C 16 h 33 (CH 3 ) 3 N] 2 + [M(EDTA)] 2- As a template for the preparation of M-MCM-41 mesoporous molecular sieves, the complexes of transition metals are complexes of transition metals and EDTA, and the cationic surfactant is composed of cetyltrimethylammonium bromide, cetyltrimethylammonium One or more of the group consisting of methyl ammonium chloride, dodecyltrimethylammonium bromide, tetradecyltrimethylammonium bromide and octadecyltrimethylammonium bromide; ( 2), the silicon source, inorganic base, water and the ionic association of step (1) are mixed...

Embodiment 1

[0036] Take by weighing 2.03g nickel nitrate and be dissolved in 10g deionized water, be that the disodium edetate solution of 5wt%-6wt% is added in the described metal salt solution by concentration, stir 0.5 hour, generate metal complex Ni(EDTA ) 2- . Then weigh 5.63g of cetyltrimethylammonium bromide, associate the metal complex with water-soluble cationic surfactant cetyltrimethylammonium bromide, stir for more than 1 hour, and the generated template agent association [C 16 h 33 (CH 3 ) 3 N] 2 + [Ni(EDTA)] 2- As a template for the synthesis of molecular sieves.

[0037] Add 11.31ml tetraethyl orthosilicate dropwise to the prepared template, continue to stir for 1.5 hours, add sodium hydroxide to adjust the pH to 11, and finally add water to make the total amount of water 120ml. It was carried out in a water bath, and after continuous stirring for 3 hours, the obtained gel was transferred into a polytetrafluoroethylene-lined reaction tank for static crystallization...

Embodiment 2

[0039] Weigh 2.02g of cobalt nitrate and dissolve it in 10g of deionized water, add a disodium edetate solution with a concentration of 5wt%-6wt% into the metal salt solution, stir for 0.5 hour, and generate the metal complex Co(EDTA ) 2- . Then weigh 5.63g of cetyltrimethylammonium bromide, associate the metal complex with water-soluble cationic surfactant cetyltrimethylammonium bromide, stir for more than 1 hour, and the generated template agent association [C 16 h 33 (CH 3 ) 3 N] 2 + [Co(EDTA)] 2- As a template for the synthesis of molecular sieves.

[0040] Add 11.31ml tetraethyl orthosilicate to the prepared template, continue to stir for 1.5 hours, add sodium hydroxide to adjust the pH to 11, and finally add water to make the total amount of water 120ml. The above synthesis process is carried out in a water bath at 50°C To proceed, after 3 hours of continuous stirring the resulting gel was transferred into a Teflon-lined reaction tank for static crystallization ...

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Abstract

The invention provides an M-MCM-41 mesoporous molecular sieve with high transition metal content and high regularity and a preparation method thereof. According to the preparation method, Ni-MCM-41, Co-MCM-41 and Cu-MCM-41 molecular sieves with heteroatom content as high as 12 wt% are successfully designed and synthesized through synthesis of an ion association complex and direct introduction of transition metal ions into the skeleton of an MCM-41 molecular sieve under mild hydro-thermal synthesis conditions. The M-MCM-41 mesoporous molecular sieve provided by the invention has the advantages of a regular structure, a uniform particle size, a great specific surface area, a large pore volume and good thermal stability.

Description

technical field [0001] The invention relates to the field of molecular sieves, in particular to an M-MCM-41 mesoporous molecular sieve with high transition metal content and high regularity and a preparation method thereof. Background technique [0002] With the development of molecular sieves and the improvement of performance requirements for catalytic materials in the field of catalysis, microporous molecular sieves, as important shape-selective catalysts in the modern petroleum industry, have the defect of small pore size. The macromolecules generated by the reaction in the channel cannot escape quickly, which leads to the occurrence of side reactions, thus limiting its application range. In order to overcome the limitations of the pore size of microporous molecular sieves, the preparation of molecular sieves with larger pore size and spatial structure has become a research hotspot. The appearance of mesoporous materials is a great leap forward in the development histor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/00
Inventor 李潇
Owner 李潇
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