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Preparation method of nano-beta zeolite molecular sieve

A molecular sieve and beta zeolite technology, which is applied in the field of preparation of nano-beta zeolite molecular sieves, can solve the problems of uneven product particle size, time-consuming and complicated preparation methods, etc.

Inactive Publication Date: 2015-05-20
LIAONING UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, in the current preparation method of nano-beta zeolite, the particle size of the obtained product is not uniform, and the preparation method is time-consuming and complicated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 0.15 g NaAlO 2 , 0.2 g NaOH, 10 ml of tetraethylammonium hydroxide solution with a mass fraction of 20% and 8 ml of water were stirred evenly, then 3 g of silicon-based mesoporous molecular sieve MCM-41 containing mesoporous template was added under stirring, and stirred at room temperature for 5 After h, a reaction mixture was obtained. The reaction mixture was transferred into a closed autoclave, and hydrothermally crystallized at 140°C for 24 h. The reaction kettle was taken out, and the white precipitate at the bottom of the reaction kettle was separated, washed twice with water, and dried at 40°C for 8 h. The dried white powder was calcined at 550 °C for 6 h to obtain nano-beta zeolite molecular sieves.

Embodiment 2

[0019] 0.2 g NaAlO 2 , 0.25 g NaOH, 15 ml tetraethylammonium hydroxide solution with a mass fraction of 20% and 10 ml water were stirred evenly, then 7 g of silicon-based mesoporous molecular sieve SBA-15 containing mesoporous template was added under stirring, and stirred at room temperature for 10 After one hour, a reaction mixture was obtained, and the reaction mixture was transferred into a closed autoclave, and hydrothermally crystallized at 110°C for 48 h, and the reaction kettle was taken out, and the white precipitate at the bottom of the reaction kettle was separated, washed twice with water, and dried at 60°C for 8 h. The dried white powder was calcined at 550 °C for 5 h to obtain nano-beta zeolite molecular sieves.

Embodiment 3

[0021] 0.15 g NaAlO 2 , 0.2 g NaOH, 12 ml of tetraethylammonium hydroxide solution with a mass fraction of 20% and 16 ml of water were stirred evenly, then 3 g of silicon-based mesoporous molecular sieve MCM-48 containing mesoporous template was added under stirring, and stirred at room temperature for 12 After h, a reaction mixture was obtained, and the reaction mixture was transferred into a closed autoclave, and hydrothermally crystallized at 160° C. for 72 h. The reaction kettle was taken out, and the white precipitate at the bottom of the reaction kettle was separated, washed twice with water, and dried at 40° C. for 20 h. The dried white powder was calcined at 700 °C for 7 h to obtain nano-beta zeolite molecular sieves.

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Abstract

The invention relates to a preparation method of a nano-beta zeolite molecular sieve. The preparation method comprises the following steps of: preparing a solution from an aluminum source, sodium hydroxide, a tetraethylammonium cation source and water, taking a silica-based mesoporous molecular sieve containing a mesoporous template agent as a silicon source, adding the silicon source into the solution, and stirring to obtain a reaction mixture, wherein the molar ratios of all raw materials in the reaction mixture are as follows: SiO2 / Al2O3=20-550, Na2O / SiO2=0.01-0.15, TEA+ / SiO2=0.01-0.40 and H2O / SiO2=2-30; stirring the reaction mixture for 5-24h at room temperature, then transferring the reaction mixture into a closed reaction kettle, and performing constant-temperature treatment at the temperature of 110-180 DEG C for 14-96h; then taking the reaction mixture out of the reaction kettle, and naturally cooling in the air; and separating white precipitates in the reaction kettle, washing for 2-5 times, then drying at the temperature of 40-80 DEG C for 6-24h, and roasting the white powder obtained by drying at the temperature of 500-700 DEG C for 4-8h to obtain the nano-beta zeolite molecular sieve. The preparation method has the advantages that the particle size of the obtained product is uniform, and the preparation method is simple.

Description

technical field [0001] The invention belongs to a preparation method of beta zeolite, and in particular relates to a preparation method of nanometer beta zeolite molecular sieve. Background technique [0002] Beta zeolite was first synthesized in 1967 by Wadlinger of Mobil Corporation. It exhibits good thermal stability, acid resistance, coking resistance and catalytic activity in many catalytic reactions, and is widely used in various petroleum refining and petrochemical industries such as hydrocracking, isomerization, alkylation and olefin hydration. In the process [3-5]. As an important catalytic material, β zeolite has attracted extensive attention in its synthesis and characterization. However, the catalytic stability of large-grain zeolite beta is poor, so the development of the preparation method of nano-beta zeolite has become a research focus of zeolite molecular sieves in recent years. [0003] Nano zeolites refer to zeolites with crystal grain size between 1-10...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 李君华张丹张启俭石广强
Owner LIAONING UNIVERSITY OF TECHNOLOGY