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MOR molecular sieve with high silica-alumina ratio and preparation method thereof

A high-silicon-aluminum ratio, molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problems of long crystallization time, high crystallization temperature, and low crystallinity, and reduce crystallization temperature, reduce production cost, and improve the effect of silicon-aluminum ratio

Active Publication Date: 2021-11-02
QINGDAO UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a high silicon-aluminum ratio MOR molecular sieve and its preparation method to solve the problem of low silicon-aluminum ratio in MOR molecular sieves in the prior art, high crystallization temperature and long crystallization time, low crystallinity, and organic templates. Or high cost and environmental pollution caused by the use of fluoride ions

Method used

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  • MOR molecular sieve with high silica-alumina ratio and preparation method thereof
  • MOR molecular sieve with high silica-alumina ratio and preparation method thereof
  • MOR molecular sieve with high silica-alumina ratio and preparation method thereof

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preparation example Construction

[0030] The invention provides a method for preparing a high silicon-aluminum ratio MOR molecular sieve, comprising the following steps:

[0031] (1) Mix silicon source, aluminum source, sodium hydroxide, and water, and age to obtain a gel;

[0032] (2) freezing the gel and drying it in vacuum to obtain a gel powder;

[0033] (3) mixing the gel powder with water, hydrothermally crystallizing in a high-pressure reactor, washing the product until neutral, and drying to obtain a hydrothermally crystallized product;

[0034] (4) Mix the hydrothermal crystallization product with a solution with a pH of 5-13, perform post-treatment, and dry at 100-120° C. for 6-12 hours to obtain a high silicon-aluminum ratio MOR molecular sieve.

[0035] In the present invention, the silicon source in step (1) is preferably white carbon black, ultrafine SiO 2 , silica sol, tetraethyl orthosilicate or water glass, and the aluminum source is preferably aluminum nitrate, aluminum sulfate, sodium meta...

Embodiment 1

[0051] This embodiment provides a method for preparing a high silicon-aluminum ratio MOR molecular sieve, comprising the following steps:

[0052] (1) Dissolve 3.45g of granular sodium hydroxide in 30mL of water, then add 2.312g of sodium metaaluminate, and stir to a clear solution, then slowly add 67.96g of silica sol (25wt%) dropwise to the clear solution, at 25 ℃ stirring and aging for 4 hours to obtain a gel;

[0053] (2) Freezing the gel with liquid nitrogen, freezing at -35°C for 24h, introducing an ice crystal template, and then drying at 0°C for 12h under a vacuum of 3Pa to obtain a gel powder;

[0054] (3) Put 2g of gel powder in 10mL of water and stir evenly, and place it in a high-pressure reactor for hydrothermal crystallization at 120°C for 24 hours, then raise the temperature to 160°C for hydrothermal crystallization for 48 hours; after the reaction, centrifuge the solid sample 1. After washing to neutrality, drying at 120°C for 12 hours to obtain a hydrothermal...

Embodiment 2

[0058] This embodiment provides a method for preparing a high silicon-aluminum ratio MOR molecular sieve, comprising the following steps:

[0059] (1) Dissolve 4.83g of granular sodium hydroxide in 30mL of water to obtain sodium hydroxide solution, which is divided into two parts, one of which is 10mL of sodium hydroxide solution, add 0.04g of pseudo-boehmite, and stir until clear solution, add 1.22g of white carbon black to another 20mL sodium hydroxide solution, and stir until a clear solution, slowly add 10mL of clear solution to 20mL of clear solution, stir and age at 60°C for 12h to obtain a gel ;

[0060] (2) Freezing the gel with liquid nitrogen, freezing it at -80°C for 12 hours, introducing an ice crystal template, and then drying it at -10°C for 18 hours under a vacuum of 5 Pa to obtain a gel powder;

[0061] (3) Put 3g of gel powder in 4mL of water and stir evenly, and place it in a high-pressure reactor for hydrothermal crystallization at 100°C for 12h; after the ...

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Abstract

The invention belongs to the technical field of molecular sieve materials, and discloses an MOR molecular sieve with a high silica-alumina ratio and a preparation method thereof. The preparation method comprises the following steps: mixing a silicon source, an aluminum source, sodium hydroxide and water, aging, freezing gel obtained by aging, introducing an ice crystal template agent, carrying out vacuum drying, carrying out hydrothermal crystallization in water, and carrying out post-treatment on a hydrothermal crystallization product in a solution with a pH value of 5-13 to obtain the MOR molecular sieve with the high silica-alumina ratio. The MOR molecular sieve with a high silica-alumina ratio is prepared by using a cheap and environment-friendly ice crystal template method, the crystallization temperature required by synthesis of the molecular sieve can be obviously reduced and the crystallization time of the molecular sieve can be shortened by introducing the ice crystal template, and the MOR molecular sieve can be prepared by adopting a common silicon source and an aluminum source without additionally adding a template or a guiding agent, the production cost is greatly reduced, the emission of waste water and waste gas is reduced, and the method has a relatively good application prospect.

Description

technical field [0001] The invention relates to the technical field of molecular sieve materials, in particular to a high silicon-aluminum ratio MOR molecular sieve and a preparation method thereof. Background technique [0002] Mordenite (MOR) molecular sieve is an important catalytic and adsorption separation material, which is widely used in reaction processes such as isomerization, alkylation, esterification, etherification and cracking in petroleum refining and fine chemical industry. The main channel structure of mordenite is a straight channel of 12-membered rings (0.65×0.70nm) and 8-membered rings (0.26×0.57nm) connected to each other along the c-axis direction, and there are also 8-membered rings connected to it along the b-axis direction. Ring (0.34×0.48nm) channels. The silicon-aluminum ratio of traditional MOR molecular sieves (SiO 2 / Al 2 o 3 The molar ratio) is only 10, the acidity is relatively weak, and a relatively high reaction temperature is required w...

Claims

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Application Information

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IPC IPC(8): C01B39/26B01J29/18B01J37/10
CPCC01B39/26B01J29/18B01J37/10C01P2002/72C01P2004/03C01P2006/17C01P2002/60Y02P20/52
Inventor 李琢赵尚庆李海威于建强张妍杜辉杨晓龙彭彦华
Owner QINGDAO UNIV
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