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Preparation method of mesoporous-microporous dual pore ZSM-5 zeolite nano sheet

A ZSM-5, meso-micro bi-porous technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of skeleton structure damage and crystallinity reduction, and achieve low cost. , the process is simple, the effect of good application prospects

Active Publication Date: 2019-01-15
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although dealumination and desiliconization methods can effectively introduce mesopores into microporous molecular sieves, the removal of silicon or aluminum will easily lead to the decrease of crystallinity and the destruction of the skeleton structure.

Method used

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  • Preparation method of mesoporous-microporous dual pore ZSM-5 zeolite nano sheet
  • Preparation method of mesoporous-microporous dual pore ZSM-5 zeolite nano sheet
  • Preparation method of mesoporous-microporous dual pore ZSM-5 zeolite nano sheet

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) 1gBola type double head quaternary ammonium salt surfactant and 0.162g sodium hydroxide, 0.031g sodium metaaluminate (44.7wt%Na 2 O,52wt%Al 2 o 3 , J&K) was dissolved in 13ml deionized water, stirred and mixed to obtain a mixed solution;

[0040] (2) Slowly add 3.8 g of ethyl orthosilicate (98 wt%, J&K) dropwise to the mixed solution obtained in step (1) under the condition of 55° C. and 300 rpm constant speed stirring, and continue stirring for 11 h until a gel solution is formed;

[0041] (3) Quickly transfer the gel solution obtained in step (2) to an autoclave, hydrothermally crystallize at 140°C for 130 hours, wash with deionized water three to four times after the crystallization reaction, and dry at 120°C for 10 hours;

[0042] (4) The product dried in step (3) was placed in a muffle furnace and calcined at 540° C. for 7 hours in an air atmosphere to remove the template agent, thereby obtaining a medium-micro-porous ZSM-5 zeolite nanosheet molecular sieve. ...

Embodiment 2

[0044] (1) 1g Bola type double head quaternary ammonium salt surfactant and 0.177g sodium hydroxide, 0.0386g sodium metaaluminate (44.7wt%Na 2 O,52wt%Al 2 o 3 , J&K) was dissolved in 15ml deionized water, stirred and mixed to obtain a mixed solution;

[0045] (2) Slowly add 4.2 g of ethyl orthosilicate (98wt%, J&K) dropwise to the mixture obtained in step (1) under the condition of 60° C. and 300 rpm constant speed stirring, and continue stirring for 10 h until a gel solution is formed;

[0046] (3) Quickly transfer the gel solution obtained in step (2) to an autoclave, conduct hydrothermal crystallization at 150°C for 120 hours, wash with deionized water three to four times after the crystallization reaction, and dry at 120°C for 10 hours;

[0047] (4) The product dried in step (3) was placed in a muffle furnace and calcined at 550° C. for 5 hours in an air atmosphere to remove the template agent, thereby obtaining a medium-micro-porous ZSM-5 zeolite nanosheet molecular sie...

Embodiment 3

[0049] (1) 1gBola type double-ended quaternary ammonium salt surfactant and 0.19g sodium hydroxide, 0.042g sodium metaaluminate (44.7wt%Na 2 O,52wt%Al 2 o 3 , J&K) was dissolved in 16ml deionized water, stirred and mixed to obtain a mixed solution;

[0050] (2) Slowly add 4.4 g of ethyl orthosilicate (98 wt%, J&K) dropwise to the mixture obtained in step (1) under the condition of 65° C. and 300 rpm constant speed stirring, and continue stirring for 9 hours until a gel solution is formed;

[0051] (3) Quickly transfer the gel solution obtained in step (2) to an autoclave, conduct hydrothermal crystallization at 155°C for 110 hours, wash with deionized water three to four times after the crystallization reaction, and dry at 120°C for 10 hours;

[0052] (4) The product dried in step (3) was placed in a muffle furnace and calcined at 550° C. for 5 hours in an air atmosphere to remove the template agent, thereby obtaining a medium-micro-porous ZSM-5 zeolite nanosheet molecular s...

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Abstract

The invention discloses a preparation method of a mesoporous-microporous dual pore ZSM-5 zeolite nano sheet. According to the method, sodium meta-aluminate is taken as the aluminum source, ethyl n-silicate is taken as the silicon source, a Bola type amphiphilic molecule with dual quaternary ammonium heads is taken as the template; and the mesoporous-microporous dual pore ZSM-5 zeolite nano sheet is synthesized through a hydrothermal method under an alkaline condition. The Bola type dual head quaternary ammonium surfactant can form ZSM-5 micro pores, moreover, the hydrophobic tail chains of thesurfactant can inhibit the growth of microcrystal, and thus uniform and sequenced mesopores are formed. The nano sheet has a 90 degree intersected intergrowth structure and has a card house shape. The repeatability is good, and the synthesized ZSM-5 zeolite nano sheet has the advantages of a common zeolite molecular sieve such as good hydrothermal stability, high acid catalytic activity, and thelike. Moreover, the nano sheet is beneficial for the reactions that macro molecules participate in. The mass transfer limitation of a single-channel zeolite molecular sieve is broken through, and theapplication value of zeolite molecular sieves in fields such as catalysis, adsorption separation, and the like, is greatly increased.

Description

technical field [0001] The invention belongs to the field of inorganic materials, and in particular relates to a method for preparing medium and micro double-hole ZSM-5 zeolite nano flakes. Background technique [0002] The MFI framework contains two sets of different channels, namely, 10-membered ring straight channels along the b-axis, with a diameter of The 10-membered ring sinusoidal channel on the a-c plane and perpendicular to the b-axis has a pore diameter of Two sets of 10-membered ring channels cross each other to form a three-dimensional channel network system. ZSM-5 is a microporous molecular sieve with MFI structure. Due to its unique pore structure, unique shape selectivity, strong acidity and high hydrothermal stability, it is widely used in petroleum processing, coal chemical industry and Fine chemical industry and other fields. However, due to the limitation of the small pore size (less than 2nm) of traditional microporous molecular sieves, there are ser...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2004/03C01P2002/01C01P2002/80C01P2002/72C01P2006/17
Inventor 奚红霞郑轲颜欣刘宝玉张凯
Owner SOUTH CHINA UNIV OF TECH
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