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Nanometer ZSM-5 molecular sieve catalyst with high silica-alumina ratio and preparation method thereof

A ZSM-5 technology with a high silicon-aluminum ratio is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc. It can solve the problem that the acidity and alkalinity of the synthetic liquid are not easy to control, and achieve good catalytic activity and wide application prospects. The effect of improving catalytic activity

Inactive Publication Date: 2012-09-19
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This synthesis method needs to add seed crystals, and the pH of the synthesis solution is not easy to control

Method used

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  • Nanometer ZSM-5 molecular sieve catalyst with high silica-alumina ratio and preparation method thereof
  • Nanometer ZSM-5 molecular sieve catalyst with high silica-alumina ratio and preparation method thereof
  • Nanometer ZSM-5 molecular sieve catalyst with high silica-alumina ratio and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 13.5ml (0.06mol) of ethyl orthosilicate, 0.49g of aluminum isopropoxide (2.4×10 -3 mol), 10ml (0.01mol) of 25% tetrapropylammonium hydroxide and 30ml (1.67mol) of water were mixed evenly and added to the three-necked flask, refluxed and stirred at 60°C for 20h, and 0.48g (0.002mol) N,N- Diethylaminopropyltrimethoxysilane was added to the original molecular sieve solution, then condensed and refluxed and stirred for 6 hours to form a uniform gel;

[0033] Add the above reaction mixture into the synthesis reaction kettle, crystallize at 150°C for 48h, and make it crystallize under static conditions; after the crystallization is complete, the product is centrifuged and washed with deionized water until the pH is 9-10. °C, and roasted at 500 °C for 3h to remove tetrapropylammonium hydroxide and organosilane, so as to obtain an average grain size of 300nm, SiO 2 / Al 2 o 3 ZSM-5 molecular sieve A of 50, and has micropores of 0.8~1.7nm.

[0034] Organosilane N,N-diethylami...

Embodiment 2

[0036] 22.5ml (0.10mol) of ethyl orthosilicate, 0.41g of aluminum isopropoxide (2.0×10 -3 mol), 10ml (0.01mol) of 25% tetrapropylammonium hydroxide and 30ml (1.67mol) of water were mixed evenly into the three-necked flask, refluxed and stirred at 80°C for 20h, and 0.48g (0.002mol) of 3-ammonium Propyltrimethoxysilane was added to the original molecular sieve solution, then condensed and refluxed and stirred for 6 hours to form a uniform gel;

[0037] Add the above reaction mixture into the synthesis reaction kettle, crystallize at 160°C for 60 hours, and make it crystallize under static conditions; after the crystallization is complete, the product is centrifuged and washed with deionized water to pH 9-10, °C, and roasted at 550 °C for 4h to remove tetrapropylammonium hydroxide and organosilane, so as to obtain an average grain size of 200nm, SiO 2 / Al 2 o 3 It is ZSM-5 molecular sieve B of 100, and has micropores of 0.8-1.5nm.

Embodiment 3

[0039] 31.5ml (0.14mol) of ethyl orthosilicate, 0.29g of aluminum isopropoxide (1.4×10 -3 mol), 2.66g (0.01mol) of tetrapropylammonium bromide and 30ml (1.67mol) of water were mixed evenly and added to the three-necked flask, refluxed and stirred at 90°C for 20h, and 0.96g (0.004mol) of 3-aminopropyl Trimethoxysilane was added to the original molecular sieve solution, then condensed and refluxed and stirred for 6 hours to form a uniform gel;

[0040] Put the reaction mixture into the synthesis reaction kettle, crystallize at 170°C for 72h, and make it crystallize under static conditions; after the crystallization is complete, the product is centrifuged, washed with deionized water until the pH is 9-10, and dried at 110°C , and roasted at 700°C for 5h to remove tetrapropylammonium bromide and organosilane, so as to obtain an average grain size of 200nm, SiO 2 / Al 2 o 3 The ZSM-5 molecular sieve is 200, and has micropores of 1.1-1.7nm.

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Abstract

The invention relates to the field of materials and catalysts, and provides a nanometer ZSM-5 molecular sieve catalyst with a high silica-alumina ratio. The nanometer ZSM-5 molecular sieve catalyst has an appropriate nano particle size and a high silica-alumina ratio, wherein the nano particle size is in the range of 0.1nm to 500nm; the molar ratio of SiO2 to Al2O3 is not less than 30; and micropores 0.5-2nm in diameter are arranged in a molecular sieve. An organic template method is adopted; organosilane is directly added into an original solution of the molecular sieve and silane is grafted onto a ZSM-5 molecular sieve seed crystal under the conditions of condensation and backflow; and a product is roasted to remove an organic template and the organosilane. By adopting the invention, synthetic steps are simplified, the synthetic method is simple, the cost is low and the application prospect is wide.

Description

technical field [0001] The invention belongs to the field of materials and catalysts, and relates to a nano molecular sieve catalyst with a high silicon-aluminum ratio and a preparation method thereof, in particular to a preparation method of a nano ZSM-5 molecular sieve with a high silicon ratio. technical background [0002] ZSM-5 is a type of high-silica zeolite developed by Mobil in the 1970s. It has two-dimensional ten-membered ring channels (ten-membered ring straight channels with a pore size of 0.54nm×0.56nm and ten-membered ring sinusoidal channels with a pore size of 0.51 nm × 0.54nm), has the functions of shape-selective catalysis, ion exchange, molecular sieving, etc., and is the most widely used catalytic material so far. Due to the high thermal stability and hydrothermal stability of the desodium hydrogen microporous zeolite molecular sieve ZSM-5 (H-ZSM-5), the silicon-aluminum ratio of the skeleton can be adjusted within a wide range, and it has strong surface...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40C07C15/073C07C2/66
Inventor 郭亚军郭亚平郭丽华王海瑾褚联峰
Owner SHANGHAI NORMAL UNIVERSITY
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