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Synthetic method of novel ordered macroporous-mesoporous-microporous hierarchical porous silicon-aluminium molecular sieve

A silica-alumina molecular sieve and microporous molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve problems such as limitations, improve catalytic activity, improve molecular flow and diffusion performance, shorten material The effect of the transmission path

Active Publication Date: 2014-08-13
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the controllable synthesis of hierarchical pore order of hierarchical zeolite molecular sieves is limited to the order of mesopores or macropores, and there is no hierarchical zeolite molecular sieve with ordered macropores and ordered mesopores. to report

Method used

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  • Synthetic method of novel ordered macroporous-mesoporous-microporous hierarchical porous silicon-aluminium molecular sieve
  • Synthetic method of novel ordered macroporous-mesoporous-microporous hierarchical porous silicon-aluminium molecular sieve
  • Synthetic method of novel ordered macroporous-mesoporous-microporous hierarchical porous silicon-aluminium molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Add 20g of 500nm polystyrene microspheres with uniform particle size, 3g of 20nm silica nanospheres, and 3g of sucrose to 400g of ultrapure water for 1h to make them uniformly dispersed, evaporate and self-assemble at 60°C for 12h, then add 0.3 After the initial carbonization at 100°C for 6h and the secondary carbonization at 160°C for 6h after g concentrated sulfuric acid, a precursor material mixed with polystyrene microspheres / silica nanospheres / carbon was obtained. The above-mentioned precursor material is added to the aqueous solution of sodium metaaluminate and tetrapropyl ammonium hydroxide (0.082g sodium metaaluminate+30ml1M tetrapropyl ammonium hydroxide aqueous solution+30ml DI H 2 O) After fully stirring at 20°C for 2h, vacuum rotary evaporation at a speed of 1r / s at a temperature of 60°C for 2h to remove water molecules in the mixed system, so that aluminum ions and structure-directing agent molecules can be uniformly infiltrated into the precursor system. T...

Embodiment 2

[0042] Add 28g of 100nm polymethyl methacrylate microspheres with uniform particle size, 4g of 5nm silica nanospheres, and 3.2g of glucose into 550g of ultrapure water for 2h to make them uniformly dispersed, and evaporate and self-assemble at 40°C for 48h Finally, after adding 0.32g of concentrated sulfuric acid, primary carbonization at 110°C for 5h and secondary carbonization at 150°C for 8h, the precursor material of polymethyl methacrylate microsphere / silica nanosphere / carbon mixture was obtained. The above-mentioned precursor material is added to the aqueous solution of aluminum isopropoxide and tetrapropyl ammonium hydroxide (0.08g aluminum isopropoxide+40ml1M tetrapropyl ammonium hydroxide aqueous solution+80ml DI H 2 O) After fully stirring at 30°C for 1h, vacuum rotary evaporation at a speed of 2r / s at a temperature of 70°C for 1.5h to remove water molecules in the mixed system, so that aluminum ions and structure-directing agent molecules can be uniformly infiltrated...

Embodiment 3

[0044] Add 8g of 300nm carbon microspheres with uniform particle size, 1g of 20nm silica nanospheres, and 1.2g of fructose to 80g of ultrapure water for 0.5h to make them uniformly dispersed, evaporate and self-assemble at 50°C for 12h, then add 0.12 After g concentrated sulfuric acid, initial carbonization at 80°C for 8h and secondary carbonization at 180°C for 4h to obtain a carbon microsphere / silica nanosphere / carbon mixed precursor material. The above precursor material was added to an aqueous solution of aluminum sulfate and tetrapropylammonium bromide (0.06g aluminum isopropoxide+2.66g tetrapropylammonium bromide+15ml DI H 2 O) After fully stirring at 15°C for 2h, vacuum rotary evaporation at a speed of 2r / s at a temperature of 50°C for 1h to remove water molecules in the mixed system, so that aluminum ions and structure-directing agent molecules can be evenly infiltrated into the precursor system. The above mixture was transferred to a 15mL autoclave, and crystallized a...

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Abstract

The invention provides a synthetic method of a novel ordered macroporous-mesoporous-microporous hierarchical porous silicon-aluminium molecular sieve. The method organically combines a template method with a crystal transformation process of a molecular sieve. Through a controllable selection of a macroporous template and a mesoporours template, a three-dimension ordered macroporous-mesoporous hierarchical porous structure having different pore sizes and interpenetrating pores is prepared. A micropore molecular sieve structure guiding agent is used for preparing an ordered micropore structure of the silicon-aluminium molecular sieve, thereby achieving regulation and control of pore sizes of macroporous structures, mesoporous structures and microporous structures. The method is simple, is feasible and is short in synthetic period. Operation conditions of the method are easy to control. Application of the molecular sieve is expected to be expanded into the technical field of organic macromolecule catalysis in which a conventional molecular sieve is not available.

Description

technical field [0001] The invention relates to the technical field of molecular sieve synthesis, in particular to a method for synthesizing an ordered macroporous-mesoporous-microporous multi-level silica-alumina molecular sieve. Background technique [0002] About 90% of the chemical products provided by the modern petrochemical and synthetic chemical industries are produced by means of catalytic processes. Catalyst is the core of catalytic technology and plays a decisive role in the development of catalytic technology. In recent years, as an environment-friendly solid acid catalyst, zeolite molecular sieves have been widely used in important fields such as petrochemical industry, petroleum cracking, and organic macromolecular synthesis, and are gradually replacing sulfuric acid, hydrofluoric acid, and aluminum trichloride, which are commonly used in industry. Strongly corrosive liquid acid catalyst. However, the size of the micropores of zeolite molecular sieves greatly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02B01J29/06
Inventor 陈丽华孙明慧李昱邓兆苏宝连
Owner WUHAN UNIV OF TECH
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