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Preparation method of mesoporous-microporous hierarchical porous MFI type molecular sieve

A multi-level porous, molecular sieve technology, applied in the direction of polymorphic crystalline silicon, silicon dioxide, silicon compounds and other characteristics of molecular sieves, can solve the problems of small nanoparticles agglomeration, difficult to overcome, etc., to shorten the transmission path and improve the flow and diffusion. sexual effect

Active Publication Date: 2017-10-13
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to realize the nanonization of molecular sieves, the problem of agglomeration of small nanoparticles often occurs in crystal synthesis, and it is difficult to overcome. Therefore, the synthesis of molecular sieves with multi-level channels is often the subject that researchers try to overcome at this stage.

Method used

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  • Preparation method of mesoporous-microporous hierarchical porous MFI type molecular sieve
  • Preparation method of mesoporous-microporous hierarchical porous MFI type molecular sieve
  • Preparation method of mesoporous-microporous hierarchical porous MFI type molecular sieve

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Embodiment 1

[0035] A preparation method of mesoporous-microporous multi-level porous MFI type molecular sieve, its preparation method comprises the following steps:

[0036] 1)SiO2 2 Synthesis of @meso-C material: add 2g mesoporous pore former F127, 2g organic carbon source glucose, 3.1g silica sol (40wt%, Sigema, AS, uniform size, particle size 20nm) into 200mL water, ultrasonic 1h, stirring for 24h, to make it fully mixed and dissolved; put the obtained solution into a centrifuge tube for centrifugation, the centrifugation rate is 10000r / min, and the centrifugation time is 10min; the obtained solid is dried in an oven at 60°C for 10h to obtain a dry powder, and then placed in a tube carbonization in a type furnace, the carbonization atmosphere is Ar gas, the carbonization temperature is 800°C, and the carbonization time is 3h to obtain SiO 2 @meso - C material;

[0037] 2) Aging and crystallization process: 0.7mL TPAOH (1M, 20wt%) was added to 0.15g of the above SiO 2 In the @meso-C ...

Embodiment 2

[0041] A preparation method of mesoporous-microporous multi-level porous MFI type molecular sieve, its preparation method comprises the following steps:

[0042] 1)SiO2 2 Synthesis of @meso-C material: add 2g mesoporous pore former P123, 2g organic carbon source dopamine, 3g silica sol (40wt%, Sigema, HS, uniform size, particle size is 12nm) into 200mL water, ultrasonic for 1h , stirred for 24 hours to make it fully mix and dissolve; put the obtained solution into a centrifuge tube for centrifugation at a centrifugal rate of 8000r / min and a centrifugation time of 20min; dry the obtained solid in a 60°C oven for 10 hours to obtain a dry powder, and then place it in a tube Carbonization in the furnace, the carbonization atmosphere is Ar gas, the carbonization temperature is 900°C, and the carbonization time is 3h to obtain SiO 2 @meso - C material;

[0043] 2) Aging and crystallization process: 0.75mL TPAOH (1M, 20wt%) was added to 0.15g of the above SiO 2 In the @meso-C core...

Embodiment 3

[0046] A preparation method of mesoporous-microporous multi-level porous MFI type molecular sieve, its preparation method comprises the following steps:

[0047] 1)SiO2 2 Synthesis of @meso-C material: add 2g mesoporous pore former P123, 2g organic carbon source fructose, 3g silica sol (40wt%, Sigema, HS, uniform size, particle size is 12nm) into 200mL water, ultrasonic for 1h , stirred for 24 hours to fully mix and dissolve; put the obtained solution into a centrifuge tube for centrifugation at a centrifugal rate of 10,000r / min and a centrifugation time of 10min; dry the obtained solid in an oven at 60°C for 10 hours to obtain a dry powder, and then place it in a tube Carbonization in the furnace, the carbonization atmosphere is Ar gas, the carbonization temperature is 800°C, and the carbonization time is 5h to obtain SiO 2 @meso - C material;

[0048] 2) Aging and crystallization process: 0.3mL TPAOH (2M, 40wt%) was added to 0.16g of the above SiO 2 @meso-C core-shell str...

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Abstract

The invention discloses a preparation method of a novel hierarchical porous mesoporous-microporous MFI type molecular sieve. The method organically combines a hard template method and a molecular sieve in-situ crystallization process in molecular sieve synthesis and successfully realizes perfect combination of nanometer effects and hierarchical pore advantages to prepare the hierarchical porous mesoporous-microporous MFI type molecular sieve with a great quantity of intracrystalline mesoporous. The method disclosed by the invention is simple and feasible and easy to operate; the conditions are easy to control; moreover, the synthesis time is short in period; the introduced mesoporous system is expected to expand application of traditional microporous molecular sieve to catalytic reaction involving macromolecules or generation of macromolecules.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve synthesis, and in particular relates to a method for synthesizing mesoporous-microporous multi-level porous MFI molecular sieves. Background technique [0002] Molecular sieve is a kind of crystallized porous material with a large number of uniform micropores (usually 0.25~1.5nm). Because of its large specific surface area, uniform pore size and pores, high adsorption capacity, thermal stability and mechanical Stability, widely used in many industrial reactions, such as: petrochemical, fine chemistry, and related hydrocarbon conversion reactions; at the same time, it is also widely used in adsorption separation and ion exchange. However, as more and more reactions require faster diffusion rates of reactants, and more macromolecules participate in catalytic reactions as reactants, the original micropores of molecular sieves cannot satisfy the freedom of macromolecules inside the molecular s...

Claims

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Application Information

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IPC IPC(8): C01B37/02C01B39/04
CPCC01B37/02C01B39/04C01P2002/72C01P2002/86C01P2004/03C01P2006/12C01P2006/14C01P2006/17
Inventor 陈丽华彭钊孙明慧肖珊珊苏宝连
Owner WUHAN UNIV OF TECH