Method for directly preparing meso-porous molecular sieves by hydrothermal process in system using meso-porous silica as silicon source precursor without meso-porous template

A technology of mesoporous silica and mesoporous template, applied in chemical instruments and methods, molecular sieves and alkali exchange compounds, borocarbonane silicone crystalline aluminum silicate zeolite, etc. It can reduce the problem of lowering and consume a lot of energy, and achieve the effect of large mesopore volume, high crystallinity, and avoiding the reduction of the degree of crystallization.

Inactive Publication Date: 2019-05-07
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above methods have many shortcomings, for example, the removal of the mesoporous template requires a lot of energ

Method used

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  • Method for directly preparing meso-porous molecular sieves by hydrothermal process in system using meso-porous silica as silicon source precursor without meso-porous template
  • Method for directly preparing meso-porous molecular sieves by hydrothermal process in system using meso-porous silica as silicon source precursor without meso-porous template
  • Method for directly preparing meso-porous molecular sieves by hydrothermal process in system using meso-porous silica as silicon source precursor without meso-porous template

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Experimental program
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Effect test

Embodiment 1

[0031] Disperse 0.813g tetrapropylammonium hydroxide aqueous solution (the mass fraction of tetrapropylammonium hydroxide solute is 25%), 0.931g tetrapropylammonium bromide is dispersed in 4.79g deionized water, and stir uniformly for 1 hour at room temperature to reach the system Uniform; then 0.031g sodium metaaluminate (of which Al 2 O 3 =41wt%) add the above solution, stir for 30min until the dispersion is uniform, add 0.6g of mesoporous silica balls (the diameter of the mesoporous silica beads is 80-200nm), stir for 2h until the system is uniform, and fill it with In a stainless steel reaction kettle lined with polytetrafluoroethylene, crystallize in an oven at 170°C for 72 hours. After the crystallization reaction is completed, the crystallization reaction product is obtained, which is then washed with deionized water to neutrality and dried in the air at 50°C. Porous ZSM-5 molecular sieve raw powder; the obtained mesoporous ZSM-5 molecular sieve raw powder is calcined in ...

Embodiment 2

[0035] Disperse 1.22g tetrapropylammonium hydroxide aqueous solution (the mass fraction of tetrapropylammonium hydroxide solute is 25%), 0.798g tetrapropylammonium bromide is dispersed in 4.49g deionized water, and stir uniformly at room temperature for 1 hour to reach the system Uniform; then 0.031g sodium metaaluminate (of which Al 2 O 3 =41wt%) add the above solution, stir for 30min until the dispersion is uniform, add 0.6g of mesoporous silica balls, stir for 2h until the system is uniform, put it into a stainless steel reactor with PTFE lining to 170℃ oven After the crystallization reaction is completed for 72 hours, the crystallization reaction product is obtained, and then washed with deionized water to neutrality, and dried in the air at 50°C to obtain the original mesoporous ZSM-5 molecular sieve powder; the obtained mesoporous ZSM- 5. The original molecular sieve powder is calcined in the air at 500℃ for 8 hours to obtain ZSM-5 molecular sieve; the molar ratio of the e...

Embodiment 3

[0039] Disperse 0.407g tetrapropylammonium hydroxide aqueous solution (the mass fraction of tetrapropylammonium hydroxide solute is 25%), 1.064g tetrapropylammonium bromide is dispersed in 5.10g deionized water, and stir uniformly for 1 hour at room temperature to reach the system Uniform; then 0.031g sodium metaaluminate (of which Al 2 O 3 =41wt%) add the above solution, stir for 30min until the dispersion is uniform, add 0.6g of mesoporous silica balls, stir for 2h until the system is uniform, put it into a stainless steel reactor with PTFE lining to 170℃ oven After the crystallization reaction is completed for 72 hours, the crystallization reaction product is obtained, and then washed with deionized water to neutrality, and dried in the air at 50°C to obtain the original mesoporous ZSM-5 molecular sieve powder; the obtained mesoporous ZSM- 5. The original molecular sieve powder is calcined in the air at 500℃ for 8 hours to obtain ZSM-5 molecular sieve; the molar ratio of the ...

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Abstract

A method for directly preparing meso-porous molecular sieves in situ by a hydrothermal process in a system using meso-porous silica as a silicon source precursor without a meso-porous template belongsto the technical field of preparation of molecular sieves. Molecular sieve crystals are formed and grown on a meso-porous substrate with tetrapropylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium bromide and tetraethylammonium bromide as a micro-porous template and the meso-porous silica as the silicon source to synthesize the meso-porous molecular sieves having a good crystallization degree, a high micro-pore specific surface area, a large external specific surface area and a large micro-pore volume. The ZSM-5 and Beta molecular sieves synthesized in the invention havea large meso-porous volume, greatly improve the mass transfer rate in the field of molecular sieve catalysis, and have a broad industrial prospect.

Description

Technical field [0001] The invention belongs to the technical field of molecular sieve preparation, and specifically relates to a method for in-situ preparation of mesoporous molecular sieve without mesoporous template agent in a system where mesoporous silica is a silicon source precursor. Background technique [0002] Since the 1980s, molecular sieves with hierarchical pores such as mesoporous macropores have gradually attracted attention. Because of their larger external specific surface area, more exposed active sites, and faster diffusion and mass transfer rate, It shows excellent properties and applications in the fields of catalysis, ion exchange, sensors, optical devices and biomedicine. Since molecular sieve research is closely related to industrial development, the exploration of new synthetic routes for multi-porous molecular sieves has become the focus of modern scientific research. There are many factors and methods to control the synthesis of hierarchical molecular...

Claims

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Application Information

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IPC IPC(8): C01B39/40C01B39/48
Inventor 于吉红王煜瑶
Owner JILIN UNIV
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