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Preparation method of MFI micro-mesoporous lamellar molecular sieve with different interlayer spacings

A medium-micro double-porous, interlayer-spacing technology, applied in the direction of crystalline aluminosilicate zeolite, can solve the problems of framework destruction crystallinity, few types of template agents, uneven mesopores, etc., and achieves low cost, simple process and wide range of The effect of the application foreground

Inactive Publication Date: 2013-12-18
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above technology can be used for the preparation of hierarchically porous molecular sieves, the mesopores introduced by desilication and dealumination methods are mostly inhomogeneous, and easily lead to the destruction of the skeleton and the reduction of crystallinity; the hierarchical porous molecular sieves prepared by the soft template method Most of the pore wall structures are still amorphous in nature; and there are very few templates for micro-double-porous molecular sieves in the synthetic sheets

Method used

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  • Preparation method of MFI micro-mesoporous lamellar molecular sieve with different interlayer spacings
  • Preparation method of MFI micro-mesoporous lamellar molecular sieve with different interlayer spacings
  • Preparation method of MFI micro-mesoporous lamellar molecular sieve with different interlayer spacings

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Mix 0.18g sodium hydroxide, 0.031g sodium metaaluminate, 0.889g four-head rigid Bola surfactant (C 6-6-6 Br 4 ) and 13.5mL of water were stirred to obtain a milky white solution, and the stirring was continued at 60°C for 1 hour;

[0036] (2) Slowly add 3.986g tetraethyl orthosilicate (98%, J￡K) dropwise to the milky white solution prepared in step (1) under magnetic stirring at 60°C to obtain a silica-alumina gel, and after aging at room temperature for 10 minutes, Keep the silica-alumina gel at 60°C and continue to stir for 6h;

[0037] (3) Put the product of step (2) into a sealed stainless steel reaction kettle, and crystallize at 150°C for 168 hours. After the crystallization is completed, the solid is suction filtered and washed with deionized water, then vacuum-dried at 120°C for 10 hours, and then Calcined at 550° C. for 6 hours in a muffle furnace to remove the organic template agent, and obtain MFI sheet molecular sieves with a hierarchical pore structur...

Embodiment 2

[0039] (1) Mix 0.3g sodium hydroxide, 0.0513g sodium metaaluminate, 1.552g four-head rigid Bola surfactant (C 6-6-8 Br 4 ) and 22.5mL of water were stirred to obtain a milky white solution, and the stirring was continued at 60°C for 1 hour;

[0040] (2) Slowly add 6.643g tetraethyl orthosilicate (98%, J￡K) dropwise to the milky white solution prepared in step (1) under magnetic stirring at 60°C to obtain a silica-alumina gel, and after aging at room temperature for 10 minutes, Keep the silica-alumina gel at 60°C and continue to stir for 6h;

[0041] (3) Put the product of step (2) into a sealed stainless steel reaction kettle, and crystallize at 150°C for 168 hours. After the crystallization is completed, the solid is suction filtered and washed with deionized water, then vacuum-dried at 120°C for 10 hours, and then Calcined at 550° C. for 6 hours in a muffle furnace to remove the organic template agent, and obtain MFI sheet molecular sieves with a hierarchical pore structur...

Embodiment 3

[0043] (1) Mix 0.36g sodium hydroxide, 0.062g sodium metaaluminate, 1.946g four-head rigid Bola type surfactant (C 6-6-10 Br 4 ) and 27mL of water were stirred to obtain a milky white solution, and the stirring was continued at 60°C for 1 hour;

[0044] (2) Slowly add 7.972g tetraethyl orthosilicate (98%, J￡K) dropwise to the clear solution obtained in step (1) under magnetic stirring at 60°C to obtain a silica-alumina gel. After aging at room temperature for 10 minutes, the The silica-alumina gel was kept at 60°C and continued to stir for 6h;

[0045] (3) Put the product of step (2) into a sealed stainless steel reaction kettle, and crystallize at 150°C for 168 hours. After the crystallization is completed, the solid is suction filtered and washed with deionized water, then vacuum-dried at 120°C for 10 hours, and then Calcined at 550° C. for 6 hours in a muffle furnace to remove the organic template agent, and obtain MFI sheet molecular sieves with a hierarchical pore struc...

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Abstract

The invention discloses a method for preparing an MFI micro-mesoporous lamellar molecular sieve with different interlayer spacings. The method comprises the following steps of: mixing and stirring sodium hydroxide, sodium meta-aluminate, four-head rigid Bola type surfactant and deionized water to get a milky white solution; cooling a product to room temperature, dropping tetraethyl orthosilicate, aging at room temperature for 5-10min and then stirring; placing the product in a homogeneous reactor, crystallizing at the temperature of 140 DEG C-150 DEG C for 5d-9d, performing suction filtration and washing with deionized water on a solid after the end of crystallization, performing vacuum drying, and further roasting in a Muffle furnace to get the micro-mesoporous MFI lamellar molecular sieve with the different interlayer spacings, wherein the interlayer spacings are 4.8nm-6.3nm. The obtained product has a micro-mesoporous structure with mesopores and crystalline micropores and can avoid the defects of a single pore structure, and the lamellar structure with the different interlayer spacings can be suitable for reactant molecules with different sizes and can expand the applications of the product in adsorption separation and other fields.

Description

technical field [0001] The invention relates to a zeolite molecular sieve, in particular to a method for preparing MFI medium-micro-double-hole molecular sieves with different layer spacings by using four-headed rigid Bola-type surfactants with different chain lengths as templates. Background technique [0002] ZSM-5 molecular sieve is a microporous molecular sieve with MFI configuration, which has a two-dimensional ten-membered ring channel structure. Due to the unique pore structure, high hydrothermal stability and strong acidity of ZSM-5 zeolite, it has been widely used in petroleum processing, fine chemical industry, catalysis, adsorption and separation and other fields. However, due to the limitation of the pore size of microporous molecular sieves (less than 2nm), on the one hand, it is difficult for some macromolecular reactants to enter the pores of the molecular sieve; The formation of carbon deposits seriously shortens the life of molecular sieves, which limits th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 段倩倩奚红霞李超
Owner SOUTH CHINA UNIV OF TECH
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