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Preparation method of nano layered ZSM (Zeolite Molecular Sieve)-5 zeolite molecular sieve

A ZSM-5, nano-layered technology is applied in the field of preparation of nano-layered ZSM-5 zeolite, which can solve the problems of high cost and complicated process, and achieves reduced pollution, high product purity and crystallinity, and reduced synthesis cost. Effect

Inactive Publication Date: 2013-04-17
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that it needs to synthesize a special macromolecular surfactant, the process is complicated, and the cost is too high
At present, the synthesis of zeolite with hierarchical pore structure has not been reported by taking advantage of the space limitation of microemulsion system and the self-assembly of surfactants in it.

Method used

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  • Preparation method of nano layered ZSM (Zeolite Molecular Sieve)-5 zeolite molecular sieve
  • Preparation method of nano layered ZSM (Zeolite Molecular Sieve)-5 zeolite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Embodiment 1: According to 1Al 2 o 3 :100SiO2 2 :1Na 2 O:10TPA 2 O:1000H 2 The molar ratio of O, 0.35g sodium aluminate, 30g tetraethyl orthosilicate, 23g tetrapropyl ammonium hydroxide (25wt%), 0.01g sodium hydroxide and 3.0g deionized water were stirred evenly at room temperature to obtain Transparent zeolite precursor solution. Take 2g of the prepared zeolite precursor solution (the rest of the zeolite precursor solution is used as a conventional hydrothermal synthesis system, which is directly crystallized, compared with the method in the present invention), and slowly added to 10g of n-heptane, 5g of hexadecyl In a solution composed of trimethylammonium bromide and 3g n-butanol, stir at 60°C to obtain a microemulsion system, and the final mass ratio is zeolite precursor solution: oil phase: surfactant: co-surfactant = 1:5 :2.5:1.5. The prepared solution was transferred into a crystallization kettle, sealed and crystallized at 120°C for 48h. After the crysta...

Embodiment 2

[0013] Example 2: The zeolite precursor solution was prepared as in Example 1. Mix 4.8g of zeolite precursor solution, 4.8g of n-heptane, 6g of cetyltrimethylammonium bromide and 2.4g of n-butanol at 60°C, and stir until the system is uniform. The prepared solution was transferred into a crystallization kettle, sealed and crystallized at 120°C for 48h. The crystallization kettle was taken out, cooled rapidly, and the product was separated by centrifugation, washed to neutrality, dried at 110°C, and characterized by XRD and SEM techniques. The results showed that the product was ZSM-5 zeolite molecular sieve. SEM results show that the sample is nano-layered, and the thickness of the thin layer is 32nm. Nitrogen adsorption results show that its specific surface area is 558m 2 / g, the pore volume is 0.20cm 3 / g.

Embodiment 3

[0014] Example 3: The zeolite precursor solution was prepared as in Example 1. Mix 4.8g of zeolite precursor solution, 4.8g of n-heptane, 6g of cetyltrimethylammonium bromide and 2.4g of n-butanol at room temperature, and stir until the system is uniform. The prepared solution was transferred into a crystallization kettle, sealed and crystallized at 90°C for 72h. The crystallization kettle was taken out, cooled rapidly, and the product was separated by centrifugation, washed to neutrality, dried at 110°C, and characterized by XRD and SEM techniques. The results showed that the product was ZSM-5 zeolite molecular sieve. SEM results show that the sample is nano-layered, and the thickness of the thin layer is 28nm.

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Abstract

The invention relates to a method for preparing a nano layered ZSM (Zeolite Molecular Sieve)-5 zeolite molecular sieve by using a micro-emulsion. The preparation method comprises the following preparation steps of: preparing a zeolite pecursor solution in an oxide molar ratio of Al2O3 to SiO2, TPA2O, Na2O and H2O as 1:(100-400):(1-100):(300-3000); mixing the prepared zeolite pecursor solution with an oil phase, a surfactant and a co-surfactant in a certain ratio to prepare a W / O (water-in-oil) micro-emulsion, then transferring the prepared micro-emulsion to a crystallization kettle, sealing and statically crystallizing for 6-72 hours at a temperature of 90-120 DEG C. The thin layer of the molecular sieve prepared by the invention has a thickness of about 30nm, a regular shape and a crystallization degree of greater than 90%; the used organic phase can be repeatedly used by separating after the synthetic process of the molecular sieve ends, so that the synthetic cost is reduced; and the method disclosed by the invention is an environmentally-friendly synthetic method.

Description

technical field [0001] The invention relates to a preparation method of ZSM-5 zeolite molecular sieve, in particular to a preparation method of nano-layered ZSM-5 zeolite with multi-level pore structure by adopting a microemulsion method. Background technique [0002] ZSM-5 zeolite molecular sieve is a molecular sieve (US3702886) developed by Mobil Corporation in 1972. It is a zeolite with a unique three-dimensional pore structure and acid strength distribution. The characteristics of high stability and catalytic activity have been widely used in catalytic cracking in refineries, methanol conversion in coal chemical industry, and toluene disproportionation (Breck D W, Zeolite Molecular Sieves [M], John Wiley & Sons: New York, 1974 ). At present, the ZSM-5 catalysts used in industry are generally large crystals with a size of micron. Due to the small pore size of ZSM-5 zeolite (about 0.55nm), the reactant or product molecules are prone to deep reactions in the pores, which w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38B82Y30/00B82Y40/00
Inventor 吉向飞杨吉庆
Owner SHANXI UNIV
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