Preparation method of ZSM-5 nanosheet aggregate grown through directional piling

A technology of ZSM-5 and nano-flakes, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve the problem of uncontrollable growth direction of ZSM-5 aggregates, and shorten the crystallization time , Reduce synthesis energy consumption, uniform particle size

Active Publication Date: 2020-12-22
CHINA NAT OFFSHORE OIL CORP +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the crystal growth direction of ZSM-5 aggregates synthesized by Silicate-1 seeds cannot be controlled, and the crystals are piled up in a disordered state

Method used

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  • Preparation method of ZSM-5 nanosheet aggregate grown through directional piling
  • Preparation method of ZSM-5 nanosheet aggregate grown through directional piling
  • Preparation method of ZSM-5 nanosheet aggregate grown through directional piling

Examples

Experimental program
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Effect test

Embodiment 1

[0060]This embodiment provides a method for preparing ZSM-5 nano flake agglomerates, the preparation method includes:

[0061]The silica sol, tetrapropylammonium bromide, ethylamine and deionized water were mixed according to a molar ratio of 1:0.2:1.2:18. The mixing was stirring and mixing in a water bath at 30°C for 30 minutes, and the resulting mixed solution was heated at 100 Crystallize at ℃ for 36 hours to obtain nano crystallite emulsion;

[0062]The sodium hydroxide and aluminum sulfate octahydrate are mixed and dissolved in water, and silica sol is added dropwise to obtain a silica-aluminum hybrid gel. The silica-aluminum hybrid gel is stirred in a 30°C water bath for 30 minutes, and the silica sol, The molar ratio of inorganic base, aluminum source and water is 1:0.01:0.08:10;

[0063]The nano-microcrystalline emulsion was added dropwise to the silica-aluminum hybrid gel and stirred for 30 minutes. The addition amount of the nano-microcrystalline emulsion was 0.7 of the mass of sil...

Embodiment 2

[0067]This embodiment provides a method for preparing ZSM-5 nano flake agglomerates, the preparation method includes:

[0068]The silica sol, tetrapropylammonium bromide, triethanolamine and deionized water were mixed according to a molar ratio of 1:0.3:1.4:18, and the mixing was stirring and mixing in a water bath at 30°C for 30 minutes, and the resulting mixed solution was heated at 90 Crystallize at ℃ for 36 hours to obtain nano crystallite emulsion;

[0069]The sodium hydroxide and aluminum sulfate octahydrate are mixed and dissolved in water, and silica sol is added dropwise to obtain a silica-aluminum hybrid gel. The silica-aluminum hybrid gel is stirred in a 30°C water bath for 30 minutes, and the silica sol, The molar ratio of inorganic base, aluminum source and water is 1:0.01:0.10:25;

[0070]The nano-microcrystalline emulsion was added dropwise to the silica-aluminum hybrid gel and stirred for 30 minutes. The addition amount of the nano-microcrystalline emulsion was 0.8 of the mas...

Embodiment 3

[0074]This embodiment provides a method for preparing ZSM-5 nano flake agglomerates, the preparation method includes:

[0075]The silica sol, tetrapropylammonium bromide, ethylenediamine, and deionized water were mixed according to a molar ratio of 1:0.4:1.8:25, and the mixing was stirring and mixing in a water bath at 30°C for 30 minutes, and the resulting mixed solution Crystallize at 120°C for 24 hours to obtain nanocrystalline emulsion;

[0076]Sodium carbonate and aluminum sulfate octahydrate are mixed and dissolved in water, and silica sol is added dropwise to obtain a silica-aluminum hybrid gel. The silica-aluminum hybrid gel is stirred in a water bath at 30°C for 30 minutes. The molar ratio of alkali, aluminum source and water is 1:0.01:0.14:25;

[0077]The nano-microcrystalline emulsion was added dropwise to the silica-aluminum hybrid gel and stirred for 30 minutes. The addition amount of the nano-microcrystalline emulsion was 0.5 of the mass of silica in the silica-aluminum hybrid ...

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Abstract

The invention provides a preparation method of a ZSM-5 nanosheet aggregate grown through directional piling. The method comprises the following steps: mixing a silicon source, a template agent, organic amine and water, and crystallizing the obtained mixed solution to obtain a nano-microcrystalline emulsion; mixing and dissolving inorganic alkali and an aluminum source in water, and dropwise addingsilica sol to obtain silicon-aluminum mixed gel; and dropwise adding the nano-microcrystalline emulsion into the silicon-aluminum mixed gel, sequentially carrying out pre-crystallization and high-temperature crystallization, carrying out solid-liquid separation, and performing calcining to obtain the ZSM-5 nano-sheet aggregate. The ZSM-5 nanosheet aggregate prepared by the preparation method is uniform in particle size, and ZSM-5 crystals that form particles are stacked in order; and the preparation method is simple to operate and low in cost, and has wide industrial application prospects.

Description

Technical field[0001]The invention belongs to the field of multi-porous molecular sieves, and relates to a preparation method of ZSM-5 molecular sieves, in particular to a preparation method of ZSM-5 nano flake aggregates grown in directional stacking.Background technique[0002]ZSM-5 molecular sieve has good selectivity due to its highly constrained binary cross-channel system, and has a wide range of applications as a catalyst or catalyst carrier in the petrochemical field. The single pore structure of ZSM-5 molecular sieve tends to limit its application in catalytic reactions involving macromolecules. The catalyst is prone to deactivation and its service life is greatly reduced. For example, the crystal size of ZSM-5 molecular sieve synthesized by the traditional microporous template tetrapropylammonium bromide (TPABr) or tetrapropylammonium hydroxide (TPAOH) hydrothermally is often larger than 1μm (Microporous Mesoporous Mater., 2019, 276, 146-153 ).[0003]The introduction of mesop...

Claims

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Application Information

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IPC IPC(8): C01B39/40B82Y30/00B82Y40/00B01J29/40C07C5/367C07C15/04C07C15/06C07C15/073C07C15/08
CPCC01B39/40B82Y30/00B82Y40/00B01J29/405C07C5/367C01P2004/03C01P2002/72C01P2006/17C01P2002/80C07C15/04C07C15/06C07C15/073C07C15/08Y02P20/52
Inventor 李孝国米晓彤常洋侯章贵张永坤李永恒曹辉
Owner CHINA NAT OFFSHORE OIL CORP
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