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Hierarchical pore zeolite molecular sieve as well as preparation method and application thereof

A zeolite molecular sieve and multi-stage pore technology, applied in the field of molecular sieves, can solve the problems of reduced MTO catalytic life, increased alkali treatment cost, zeolite framework collapse, etc., and achieves the effects of good framework preservation, high mesopore volume and complete morphology.

Active Publication Date: 2021-07-30
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2010, Olsbye et al. first tried to carry out alkali treatment on SSZ-13 zeolite with CHA topology. After alkali treatment, the crystallinity of SSZ-13 zeolite decreased sharply, the zeolite framework collapsed and the framework aluminum was greatly reduced, which led to MTO catalysis. Reduced lifespan
However, this type of organic pore directing agent is relatively expensive, and its addition will greatly increase the cost of alkali treatment

Method used

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  • Hierarchical pore zeolite molecular sieve as well as preparation method and application thereof
  • Hierarchical pore zeolite molecular sieve as well as preparation method and application thereof
  • Hierarchical pore zeolite molecular sieve as well as preparation method and application thereof

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Effect test

Embodiment 1

[0067] This embodiment provides a method for preparing a hydrogen-type hierarchically porous H-SSZ-13 zeolite molecular sieve, which includes the following steps:

[0068] (1) Roast SSZ-13 zeolite raw powder (Si / Al=23) at high temperature at 550°C for 10h, and the heating rate during the roasting process is 1°C / min to obtain Na-SSZ-13 zeolite raw powder, which is placed in Dehydration was completed in a vacuum oven at 160° C. for 4 hours.

[0069] (2) Weigh 3g of the dehydrated Na-SSZ-13 zeolite powder in the above step (1), place it in a closed container, then add a sufficient amount of diethylamine, stir for 1h, and make the Na-SSZ-13 zeolite powder fully The zeolite skeleton is protected by absorbing diethylamine; then the raw zeolite powder is separated by suction filtration, and the obtained solid sample is placed in a fume hood for a period of time to volatilize the diethylamine on the surface of the zeolite.

[0070] (3) Pour the Na-SSZ-13 zeolite raw powder obtained i...

Embodiment 2

[0074] This embodiment provides a method for preparing a hydrogen-type hierarchically porous H-SSZ-13 zeolite molecular sieve, which includes the following steps:

[0075] (1) Roast SSZ-13 zeolite raw powder (Si / Al=23) at high temperature at 550°C for 10h, and the heating rate during the roasting process is 1°C / min to obtain Na-SSZ-13 zeolite raw powder, which is placed in Dehydration was completed in a vacuum oven at 180° C. for 2 hours.

[0076] (2) Weigh 3g of the dehydrated Na-SSZ-13 zeolite powder in the above step (1), place it in a closed container, then add a sufficient amount of diethylamine, stir for 1h, and make the Na-SSZ-13 zeolite powder fully The zeolite skeleton is protected by absorbing diethylamine; then the raw zeolite powder is separated by suction filtration, and the obtained solid sample is placed in a fume hood for a period of time to volatilize the diethylamine on the surface of the zeolite.

[0077] (3) Pour the Na-SSZ-13 zeolite raw powder obtained i...

Embodiment 3

[0081] This embodiment provides a method for preparing a hydrogen-type hierarchically porous H-SSZ-13 zeolite molecular sieve, which includes the following steps:

[0082] (1) Roast SSZ-13 zeolite raw powder (Si / Al=23) at high temperature at 550°C for 10h, and the heating rate during the roasting process is 1°C / min to obtain Na-SSZ-13 zeolite raw powder, which is placed in Dehydration was completed in a vacuum oven at 180° C. for 2 hours.

[0083] (2) Weigh 3g of the dehydrated Na-SSZ-13 zeolite powder in the above step (1), place it in a closed container, then add a sufficient amount of diethylamine, stir for 1h, and make the Na-SSZ-13 zeolite powder fully The zeolite skeleton is protected by absorbing diethylamine; then the raw zeolite powder is separated by suction filtration, and the obtained solid sample is placed in a fume hood for a period of time to volatilize the diethylamine on the surface of the zeolite.

[0084](3) Pour the Na-SSZ-13 zeolite raw powder obtained in...

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Abstract

The invention provides a hierarchical pore zeolite molecular sieve as well as a preparation method and application thereof. The preparation method comprises the following steps: roasting SSZ-13 zeolite at a high temperature to obtain Na-SSZ-13 zeolite; mixing the Na-SSZ-13 zeolite with a small molecular amine compound for full adsorbing; carrying out suction filtration and separation on the Na-SSZ-13 zeolite, and carrying out alkali treatment by adopting alkali liquor after small molecular amine compounds on the surface of the Na-SSZ-13 zeolite are volatilized; washing a centrifugal solid sample collected after the alkali treatment with water to be neutral, performing drying, and then carrying out acid pickling treatment by adopting acid liquor; and washing a centrifugal solid sample collected after the acid pickling treatment to be neutral, and performing drying to obtain the hierarchical pore zeolite molecular sieve. According to the method, the SSZ-13 zeolite is subjected to the alkali treatment to construct a multistage pore channel, meanwhile, a zeolite framework of the SSZ-13 zeolite can be well protected, the mesoporous volume is higher, the mass transfer capacity is higher, and the SSZ-13 zeolite shows more excellent catalytic performance, higher diene selectivity and lower carbon deposition rate in a methanol-to-olefin reaction.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves, and relates to a multi-stage pore zeolite molecular sieve and its preparation method and application. Background technique [0002] Zeolite molecular sieve is a typical solid acid catalyst, and its catalytic performance mainly depends on the adsorption, reaction, desorption and diffusion behavior of various species in the active sites in the zeolite micropores during the reaction process. Therefore, the mass transfer efficiency and the utilization efficiency of active sites in the micropores of zeolite molecular sieve directly affect the rate of catalytic reaction. How to make up for the structure and mass transfer defects of traditional microporous zeolite molecular sieves, reduce the factors that negatively affect the mass transfer of micropores, and improve the utilization efficiency of catalysts have become key issues and research hotspots in the utilization of new catalytic material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48C01B39/04B01J29/70B01J35/10C07C1/20C07C11/04C07C11/06
CPCC01B39/48C01B39/04B01J29/70C07C1/20C01P2002/72C01P2004/03C01P2006/17C07C2529/70B01J35/617B01J35/633C07C11/04C07C11/06Y02P30/40
Inventor 朱小春高羽刘孟杨子瑶申宝剑
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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