Method for preparing mesoporous molecular sieve Fe-MCM-41 with high iron content

A fe-mcm-41, 1fe-mcm-41 technology is applied in the field of preparation of heteroatom mesoporous molecular sieve Fe-MCM-41, which can solve the problems of uneven surface of molecular sieve and uneven distribution of metal ions, and achieve strong application Value, enhanced selectivity and activity, good dispersion effect

Inactive Publication Date: 2011-09-28
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In terms of the synthesis of heteroatom molecular sieves, the domestic patent CN 96117259 adopts the Zr metal element molecular sieve prepared by the ion exchange method, the Na type molecular sieve is ion exchanged into the H type molecular sieve, and then impregnated with a soluble salt solution containing Zr, and the metal Zr is loaded on the On the molecular sieve, the molecular sieve obtained by this method has defects such as uneven surface
CN 101205073 describes the heteroatom molecular sieve Mo-MCM-41 obtained by direct synthesis, US 5108725, US5102643, and US5057296 describe the synthesis process, reaction reagents, composition, physical and structural properties of heteroatom MCM-41, and CN 1613765 describes the nano The preparation of titanium dioxide and MCM-41 composite material, CN 1552624 has introduced a kind of method that the molecular sieve MCM-41 is modified by aftertreatment, but the molecular sieve metal content that the direct method prepares is generally below 5%, and metal ion distribution is uneven uniform

Method used

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  • Method for preparing mesoporous molecular sieve Fe-MCM-41 with high iron content
  • Method for preparing mesoporous molecular sieve Fe-MCM-41 with high iron content
  • Method for preparing mesoporous molecular sieve Fe-MCM-41 with high iron content

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Experimental program
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Effect test

Embodiment 1

[0028] Add 5.63g CTAB to 100ml deionized water, stir for 15min, add 1.7g Fe(NO3)3.9H2O, stir for 30min, add a certain amount of nitric acid, adjust the solution pH=1, continue stirring for 30min, add 10 times to the solution A total of 13.83ml TEOS was added to the solution; after 2 hours, a certain amount of NaOH was added to adjust the pH to 9. After 3 hours of reaction, the solution was transferred to a polytetrafluoro-lined autoclave, and the crystal state was crystallized under autogenous pressure of 403K for 3 days. Then the sample was suction filtered, washed with deionized water until neutral, and dried at 373K for 6h. Program the temperature up to 550°C at a rate of 1°C min-1, keep it warm for 5 hours, and remove the template agent.

Embodiment 2

[0030] Add 3.82g SDS to 100ml deionized water, stir for 15min, then add 1.2g Fe2(SO4)3.7H2O, stir for 30min, add a certain amount of sulfuric acid, adjust the solution pH=1, continue stirring for 30min, add 10 times to the solution A total of 13.83ml TEOS was added to the solution; after 2 hours, a certain amount of NaOH was added to adjust the pH to 9. After 3 hours of reaction, the solution was transferred to a polytetrafluoro-lined autoclave, and the crystal state was crystallized under autogenous pressure of 403K for 3 days. Then the sample was suction filtered, washed with deionized water until neutral, and dried at 373K for 6h. Program the temperature up to 550°C at a rate of 1°C min-1, keep it warm for 5 hours, and remove the template agent.

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Abstract

The invention relates to a method for preparing a mesoporous molecular sieve Fe-MCM-41 with high iron content. In the method, the problem that iron is easily aggregated to generate a precipitate in the process of synthesizing the molecular sieve is solved by controlling the pH value in the synthesis process, an iron atom is directly introduced into a framework of the MCM-41 molecular sieve under the mild hydrothermal synthesis condition, and the Fe-MCM-41 molecular sieve with the iron content of 10 percent is successfully synthesized. The mesoporous molecular sieve material with the high iron content has a regular structure, a uniform pore size, large specific surface area and pore volume and high heat stability.

Description

[0001] manual 1. Technical field [0002] The invention relates to a preparation method of heteroatom mesoporous molecular sieve Fe-MCM-41, in particular to a preparation method of Fe-MCM-41 mesoporous molecular sieve with high iron content. 2. Background technology [0003] As an important class of catalysts, zeolite molecular sieves are widely used in various catalytic processes, but the traditional zeolite molecular sieves have small pores (usually less than 1), limited by the size of the pores, and can only be used for catalytic reactions of small molecules. Therefore, the synthesis has Molecular sieve materials with larger pore sizes have been the object of research. In 1992, Mobil Company discovered a new series of mesoporous materials M41S. As one of the members, MCM-41 is a kind of mesoporous molecular sieve material with a hexagonal ordered pore structure, high specific surface area and high adsorption performance, and The pore size distribution is uniform and can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/76C01B39/04C01B39/48
Inventor 李保山徐俊青
Owner BEIJING UNIV OF CHEM TECH
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