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Multistage pore structure nano molecular sieve catalyst and preparation method thereof

A nano-molecular sieve and catalyst technology, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of easy generation of carbon deposits, large grains, short service life, etc., achieve high conversion rate, simplify Synthesis steps, effect of increasing specific surface area

Inactive Publication Date: 2011-04-06
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the small pore size of microporous molecular sieves, the catalytic reaction of macromolecules is limited, and it is increasingly unable to meet the needs of fine chemical reactions in recent years. Therefore, the industrial application of microporous molecular sieves is largely limited.
[0003] At present, most of the ZSM-5 catalysts used in industry are large-grained zeolites with a size of a few microns. Due to the limitation of large crystal grains and narrow and long channels, it is easy to generate carbon deposits and has a short service life. The diffusion resistance of macromolecules in the crystal is relatively low. Large, and small grain molecular sieves just make up for this deficiency

Method used

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  • Multistage pore structure nano molecular sieve catalyst and preparation method thereof
  • Multistage pore structure nano molecular sieve catalyst and preparation method thereof
  • Multistage pore structure nano molecular sieve catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 13.5ml (0.06mol, equivalent to SiO 2 0.06mol), aluminum isopropoxide 0.41g (0.002mol, equivalent to Al 2 o 3 0.001mol), n-butylamine 0.88g (0.012mol) and water 30ml (1.67mol) were mixed evenly into a three-necked flask to form the original molecular sieve solution; and 0.39g 3-aminopropyltrimethoxysilane (0.002mol) was directly Add it to the original molecular sieve solution, condense and reflux at 70°C and stir for 18 hours to form a uniform gel;

[0031] The reaction mixture was added to the synthesis reaction kettle, and crystallized at 150°C for 48 hours to make it crystallize under static conditions;

[0032] After the crystallization is complete, the product is centrifuged, and the precipitate is taken and washed with deionized water until the pH is 9-10, dried at 110°C, and calcined at 500°C for 3 hours to remove n-butylamine and organosilane, thereby obtaining SiO 2 / Al 2 o 3 The ZSM-5 nanometer molecular sieve catalyst with a molar ratio of 30, numbere...

Embodiment 2

[0035] Mix 22.5ml (0.1mol) of ethyl orthosilicate, 0.41g (0.002mol) of aluminum isopropoxide, 0.72g (0.012mol) of ethylenediamine and 30ml (1.67mol) of water into a three-necked flask to form the original molecular sieve solution; and 0.50g N-aminoethyl-γ-aminopropyltrimethoxysilane (0.002mol) was directly added to the original solution of molecular sieves, condensed and refluxed at 80°C and stirred for 20h to form a uniform gel;

[0036] Add the above reaction mixture into the synthesis reactor, crystallize at 160°C for 60 hours, and make it crystallize under static condition;

[0037] After the crystallization is complete, the product is centrifuged, and the precipitate is taken and washed with deionized water until the pH is 9-10, dried at 110°C, and roasted at 600°C for 4 hours to remove ethylenediamine and organosilane, thereby obtaining SiO 2 / Al 2 o 3 The ZSM-5 nanometer molecular sieve catalyst with a molar ratio of 50, numbered B.

[0038] Molecular sieve catalyst pa...

Embodiment 3

[0040] Mix 22.5ml (0.1mol) of tetraethylorthosilicate (0.1mol), 0.41g (0.002mol) of aluminum isopropoxide, 2.66g (0.01mol) of tetrapropylammonium bromide and 30ml (1.67mol) of water into a three-necked flask, Form the original molecular sieve solution; add 0.47g N,N-diethylaminopropyltrimethoxysilane (0.002mol) directly to the original molecular sieve solution, reflux and stir at 90°C for 24 hours to form a uniform gel;

[0041] Add the above reaction mixture into the synthesis reaction kettle, crystallize at 170°C for 72 hours, and make it crystallize under static condition;

[0042] After the crystallization is complete, the product is centrifuged, and the precipitate is taken and washed with deionized water until the pH is 9-10, dried at 110°C, and roasted at 700°C for 5 hours to remove tetrapropylammonium bromide and organosilane, thereby obtaining SiO 2 / Al 2 o 3 A ZSM-5 nanometer molecular sieve catalyst with a molar ratio of 70.

[0043] Molecular sieve catalyst part...

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Abstract

The invention discloses a multistage pore structure nano molecular sieve catalyst, belonging to the field of materials and catalysts. A preparation method of the catalyst comprises the following steps of: mixing tetraethoxysilane, aluminum isopropoxide and an organic template agent to obtain a molecular sieve original solution; directly adding organosilane into the molecular sieve original solution, and grafting organosilane to a ZSM-5 molecular sieve under condensation and flux conditions; and roasting to remove the organosilane and the organic template agent. The multistage pore structure nano molecular sieve catalyst with micropores and mesopores can be obtained by using the method, contains nano particles with proper nano particle size, has high stability and is applied to macromolecule reactions.

Description

technical field [0001] The invention relates to the field of materials and catalysts, in particular to a nano molecular sieve catalyst with a hierarchical porous structure and a preparation method thereof, in particular to a nano ZSM-5 molecular sieve catalyst with a hierarchical porous structure containing micropores and mesopores and a preparation method thereof. Background technique [0002] ZSM-5 is a type of high-silica zeolite developed by Mobil in the 1970s. It has good shape selectivity and is not easy to deposit carbon during the catalytic process. It is the most widely used zeolite after Y-type zeolite. Microporous zeolite molecular sieves such as ZSM-5 have been used as solid acid catalysts in petrochemical and other fields. Mainly because of its regular channels, adjustable acidity and shape selectivity. Therefore, molecular sieves with different pore sizes have different shape-selective effects. However, due to the small pore size of microporous molecular siev...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J35/10C07C15/073C07C2/66
Inventor 郭亚军郭亚平王海瑾郭丽华褚联峰
Owner SHANGHAI NORMAL UNIVERSITY
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