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Method for preparing ZSM-5 zeolite molecular sieve microspheres

A kind of technology of zeolite molecular sieve, ZSM-5

Inactive Publication Date: 2012-07-18
LIAONING UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing methods all have the disadvantages of insufficient mechanical strength of zeolite microspheres and complicated and cumbersome preparation steps.

Method used

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  • Method for preparing ZSM-5 zeolite molecular sieve microspheres
  • Method for preparing ZSM-5 zeolite molecular sieve microspheres
  • Method for preparing ZSM-5 zeolite molecular sieve microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 1.5 ml of polymethylsiloxane and disperse it in 15 ml of absolute ethanol and stir evenly to obtain solution I for later use; weigh 0.02 g of NaAlO 2 Dissolve 0.06g NaOH in 35ml of distilled water, then add 19ml of tetrapropylammonium hydroxide 25% aqueous solution, stir evenly, add 6ml of tetraethyl orthosilicate dropwise, stir at room temperature for 3 hours to obtain a transparent solution, then add 12ml of solution I, After stirring at room temperature for 5 hours, a translucent solution was obtained. The product was transferred to a closed reaction kettle, and after crystallization at 90°C for 4 days, the reaction kettle was taken out to cool naturally. Vacuum drying for 36 hours, followed by calcination in a muffle furnace at 400°C for 5 hours to obtain ZSM-5 zeolite molecular sieve microspheres.

Embodiment 2

[0024] Take 2.5 ml of polymethylsiloxane and disperse it in 24ml of n-propanol and stir it evenly to obtain solution I for later use; weigh 0.08g of NaAlO 2 Dissolve 0.12g NaOH in 75ml of distilled water, then add 17ml of n-butylamine, stir evenly, add dropwise 10ml of tetraethyl orthosilicate, stir at room temperature for 6 hours to obtain a transparent solution, then add 20ml of solution I, and stir at room temperature for 12 hours to obtain half Transparent solution, transfer the product into a closed reaction kettle, crystallize at 180°C for 5 days, take out the reaction kettle to cool naturally, separate the product in the kettle, wash with ethanol for 3 times, wash with water twice, vacuum dry at 50°C for 24h, and dry at 600°C ℃ in a muffle furnace for 5 h to obtain ZSM-5 zeolite molecular sieve microspheres.

Embodiment 3

[0026] Disperse 4.5 ml of methyltriethoxysilane in 35 ml of ethanol and stir to obtain solution I for later use; weigh 0.10 g of NaAlO 2 Dissolve 0.28g NaOH in 155ml distilled water, then add 40ml tetrapropylammonium hydroxide 25% aqueous solution, stir evenly, add 14ml tetraethyl orthosilicate dropwise, stir at room temperature for 9 hours to obtain a transparent solution, then add 16ml solution I, After stirring at room temperature for 24 hours, a translucent solution was obtained. The product was transferred into a closed reaction kettle, and after crystallization at 150°C for 7 days, the reaction kettle was taken out to cool naturally, and the product in the kettle was separated, washed with ethanol for 3 times, then washed with water twice, and vacuumed at 60°C. Dry for 12 hours, and bake in a muffle furnace at 550° C. for 7 hours to obtain ZSM-5 zeolite molecular sieve microspheres.

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Abstract

The invention discloses a method for preparing ZSM-5 zeolite molecular sieve microspheres. The ZSM-5 zeolite molecular sieve microspheres are prepared by using methyl-containing organo-siloxane and tetraethoxysilane as silicon sources by a one-step method; the microspheres consist of small ZSM-5 zeolite particles; by changing the adding amount of the methyl-containing siloxane, the size of the microspheres can be adjusted in a range of 3-8 mu m; and the ZSM-5 zeolite molecular sieve microspheres are uniform in size, high in dispersibility, easy to prepare massively, and can be applied in the aspects of catalysis, adsorption, separation and the like.

Description

technical field [0001] The invention relates to a preparation method of ZSM-5 zeolite molecular sieve microspheres, belonging to the field of zeolite molecular sieve materials. Background technique [0002] ZSM-5 zeolite molecular sieve was first synthesized by the Mobil Company of the United States in 1972 [U.S.P3702886]. Its channel arrangement is characterized by the intersection of straight cylindrical channels and transverse sinusoidal channels. , The long axis is 0.7±0.07 nm, the cross section of the sinusoidal channel is approximately circular, and the diameter is 0.55 nm. It has a well-developed microporous structure and high catalytic activity, and is widely used in many fields such as adsorption, catalysis, separation analysis, ion exchange and sensors. [0003] In the catalytic reaction, nano-ZSM-5 zeolite molecular sieves can effectively increase the diffusion rate of reaction molecules in it and have been widely studied. However, in the preparation process, nan...

Claims

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Application Information

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IPC IPC(8): C01B39/40
Inventor 李君华张丹张启俭
Owner LIAONING UNIVERSITY OF TECHNOLOGY
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