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Multistage meso-porous ZSM-5 catalyst as well as preparation method and application method thereof

A ZSM-5 and catalyst technology, which is applied in the field of multi-level mesoporous ZSM-5 catalysts, can solve the problems of pore structure distortion, damage, collapse and the like, and achieve the effect of a simple preparation method

Inactive Publication Date: 2015-03-25
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method uses the same cationic template as the synthetic all-silicon M-41 series molecular sieve, and the synthesized silicon source is mesoporous SiO with short-range order and long-range disorder. 2 , in the process of hydrothermal in-situ crystallization, due to the strong crystallization conditions of zeolite crystallization, these unstable mesopore phases may be destroyed during the crystallization process, and the pore structure is distorted or even collapsed (K. R. Kloestra et al., Chem . Commun. 1997, 2281-2282)

Method used

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  • Multistage meso-porous ZSM-5 catalyst as well as preparation method and application method thereof
  • Multistage meso-porous ZSM-5 catalyst as well as preparation method and application method thereof
  • Multistage meso-porous ZSM-5 catalyst as well as preparation method and application method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Preparation of Hierarchical Mesoporous ZSM-5 Zeolite Catalyst ((MeO) 3 SiC 3 h 6 (Me 2 )C 12 N + Cl - as template), marked as HP-ZSM-5(1).

[0020] (1) Na 2 SiO 3 , NaAlO 2 , NaOH, TPAOH, (MeO) 3 SiC 3 h 6 (Me 2 )C 12 N + Cl - , mixed with water, the molar ratio is 1SiO 2 / 0.05Al 2 o 3 / 0.15Na 2 O / 0.17TPAOH / 0.035(MeO) 3 SiC 3 h 6 (Me 2 )C x N + Cl - / 25H 2 O. After stirring evenly, aging at 100°C for 2h. Then transfer to a polytetrafluoroethylene-lined stainless steel kettle, and crystallize at 100° C. for 5 days at a stirring speed of 22 rpm.

[0021] (2) The product obtained in step (1) was washed with water, and the solid obtained after centrifugation was dried at 50°C for 12 hours.

[0022](3) The product after drying in step (2) was heated in a muffle furnace at a rate of 1°C / min to 550°C for 5 hours and calcined to remove the organic template to obtain the catalyst.

Embodiment 2

[0024] Preparation of Hierarchical Mesoporous ZSM-5 Zeolite Catalyst ((MeO) 3 SiC 3 h 6 (Me 2 )C 14 N + Cl - as template), marked as HP-ZSM-5(2).

[0025] (1) Ethyl silicate, pseudoboehmite (70%Al 2 o 3 ), NaOH, TPAOH, (MeO) 3 SiC 3 h 6 (Me 2 )C 14 N + Cl - Mix with water, the molar ratio is 1SiO 2 / 0.07Al 2 o 3 / 0.15Na 2 O / 0.24TPAOH / 0.045(MeO) 3 SiC 3 h 6 (Me 2 )C x N + Cl - / 28H 2 O. After stirring evenly, aging at 100°C for 2.5h. Then transfer to a polytetrafluoroethylene-lined stainless steel kettle, and crystallize at 120° C. for 7 days at a stirring speed of 25 rpm.

[0026] (2) The product obtained in step (1) was washed with water, and the solid obtained after centrifugation was dried at 60°C for 12 hours.

[0027] (3) The product after drying in the step (2) was heated in a muffle furnace at a rate of 1°C / min to 570°C for 8 hours and calcined to remove the organic template to obtain the catalyst.

Embodiment 3

[0029] Preparation of Hierarchical Mesoporous ZSM-5 Zeolite Catalyst ((MeO) 3 SiC 3 h 6 (Me 2 )C 16 N + Cl - as template), labeled as HP-ZSM-5(3).

[0030] (1) Ethyl silicate, aluminum isopropoxide, NaOH, TPAOH, (MeO) 3 SiC 3 h 6 (Me 2 )C 16 N + Cl - Mix with water, the molar ratio is 1SiO 2 / 0.08Al 2 o 3 / 0.15Na 2 O / 0.36TPAOH / 0.055(MeO) 3 SiC 3 h 6 (Me 2 )C 16 N + Cl - / 30H 2 O. After stirring evenly, aging at 100°C for 3h. Then transfer to a polytetrafluoroethylene-lined stainless steel kettle, and crystallize at 140° C. for 6 days at a stirring speed of 40 rpm.

[0031] (2) The product obtained in step (1) was washed with water, and the solid obtained after centrifugation was dried at 65°C for 12 hours.

[0032] (3) The product dried in step (2) was heated in a muffle furnace at a rate of 1°C / min to 620°C and calcined for 8 hours to remove the organic template to obtain the catalyst.

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Abstract

The invention discloses a multistage meso-porous ZSM-5 catalyst as well as a preparation method and an application method thereof. The preparation method comprises the following steps: with trimethoxysilane quaternary ammonium salt and alkyl lumiflavin oxygen silicon propyl dimethyl ammonium chloride (Cx(MeO)3SiMe2NH4Cl) as a cationic meso-porous template agent and tripropyl ammonium hydroxide (TPAOH) as a microporous template agent, synthesizing multistage porous aluminosilicate ZSM-5 zeolites. The multistage meso-porous ZSM-5 catalyst has the characteristics of high acidity, multistage meso-porous property, bimodal distribution (3.2nm+12.7.5nm) of meso-pores within a distribution range of 2-50nm, good crystallinity, good anti-coking activity, good catalytic cracking activity, simpleness in preparation method and capability of being expanded to synthesis of other silica-alumina zeolites and all-silicon zeolites.

Description

technical field [0001] The invention relates to a catalyst, in particular to a multi-level mesoporous ZSM-5 catalyst for catalytically cracking naphtha and its preparation and application method. Background technique [0002] The development of petroleum catalytic cracking (FCC) catalyst is an important technical field of petroleum refining industry. Zeolite catalyst is currently the mainstream FCC catalyst. Microporous zeolite has high specific surface area and pore volume. Although the existence of a large number of micropores (<2nm) helps to improve shape selectivity, the microporous structure also has disadvantages, and the molecular diffusion of reactants The rate of entering the micropores of the crystal is very slow. At the same time, during the catalytic process, the products and reactants will generate unnecessary adsorption on the micropores. The steric effect makes it difficult for the reactant molecules to reach some micropores, reducing the effective pore vol...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J35/10C10G11/05
Inventor 陈丽娟向育军
Owner HUNAN UNIV OF SCI & TECH
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