A kind of preparation method of hierarchical pore zeolite molecular sieve

A zeolite molecular sieve, multi-stage pore technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolite, etc., to achieve the effects of preventing damage, improving diffusion performance, and preventing excessive desiliconization

Active Publication Date: 2021-12-21
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although the above work introduces mesoporous EU-1 molecular sieves through post-treatment methods, its external specific surface area is less than 70m 3 / g, there is still a lot of room for improvement

Method used

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  • A kind of preparation method of hierarchical pore zeolite molecular sieve
  • A kind of preparation method of hierarchical pore zeolite molecular sieve
  • A kind of preparation method of hierarchical pore zeolite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 10g EU-1 (SiO 2 / Al 2 o 3 molar ratio=80:1) Molecular sieve raw powder, according to the 3°C / min temperature rise program to 370°C for 5h, weigh 5g of the sample after the roasting, according to the liquid-solid weight ratio of 20:1 and 1.0mol / L hydrochloric acid solution After mixing and stirring evenly, treat at 150°C for 24h. After the reaction is over, filter and wash until neutral, and dry at 120°C for 12h; mix the dried sample with 0.8mol / L tetramethylammonium hydroxide solution according to the liquid-solid weight ratio of 20 : 1 mix, stir evenly, add 1gCTAB, react at 120°C for 24h, filter and wash to neutral pH, dry at 120°C for 12h, and bake at 550°C for 300 minutes to obtain a hierarchically porous EU-1 molecular sieve product, remember S1.

Embodiment 2

[0031] Take 10g EU-1 (SiO 2 / Al 2 o 3 molar ratio=30:1) Molecular sieve raw powder, roasted at 550 °C for 3 hours according to the temperature rise program of 5 °C / min, weighed 5 g and 0.8 mol / L of the sample after roasting and mixed with hydrochloric acid solution according to the liquid-solid weight ratio of 10:1 , treated at 120°C for 18 hours, the reaction was completed, the pH was filtered and washed to neutral, and dried at 120°C for 12 hours; the dried sample was mixed with 1.0mol / L ammonia solution according to the liquid-solid weight ratio of 30:1, and 3gCTAB was added after stirring evenly. React at 150°C for 30 hours, filter and wash until neutral, dry at 120°C for 12 hours, and calcine at 550°C for 300 minutes to obtain a hierarchically porous EU-1 molecular sieve product, remember sample S2.

Embodiment 3

[0033] Take 10g EU-1 (SiO 2 / Al 2 o 3 molar ratio=40:1) Molecular sieve raw powder, according to the 4°C / min temperature rise program to 450°C for 4.5h, weigh 5g and 0.1mol / L of the sample after the roasting and mix with acetic acid solution according to the liquid-solid weight ratio of 15:1 Mix and treat at 130°C for 16 hours. After the reaction is completed, filter and wash the pH to neutral, and dry at 120°C for 12 hours; mix the dried sample with 0.5mol / L tetraethylammonium hydroxide solution according to the liquid-solid weight ratio of 25:1, After stirring evenly, add 3g of CTAB, react at 140°C for 36h, filter and wash until neutral, dry at 120°C for 12h, and calcined at 550°C for 300 minutes to obtain a hierarchically porous EU-1 molecular sieve product, remember sample S3.

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Abstract

The invention relates to the technical field of molecular sieve preparation, and discloses a preparation method of a multi-stage pore zeolite molecular sieve; the specific surface area of ​​the multi-stage pore EU-1 molecular sieve is improved; specifically, the template agent part of the EU-1 molecular sieve raw powder is firstly controlled by temperature Removal; then at 100-150°C, place the treated EU-1 molecular sieve in an acidic solution for 12-48h, and then at 80-180°C, place it in an alkaline solution dissolved in CTAB for 2 Roasting after 48h to obtain multi-level porous EU-1 molecular sieve; the present invention aims at the post-treatment defect of one-dimensional EU-1 molecular sieve, by controlling the roasting temperature and acid treatment, combined post-treatment of desiliconization and CTAB-assisted secondary crystallization The preparation of the multi-stage molecular sieve is simple and easy, and the external specific surface area of ​​the formed multi-stage EU-1 molecular sieve is increased, the diffusion performance of the molecular sieve is improved, and the catalytic activity is further improved.

Description

technical field [0001] The invention relates to the technical field of molecular sieve preparation, in particular to a method for preparing a multi-stage pore zeolite molecular sieve. Background technique [0002] EU-1 molecular sieve has a one-dimensional microporous channel structure, which contains a 10-membered ring straight channel and a 12-membered ring side pocket perpendicular to it. The unique channel structure makes it exhibit excellent catalytic performance in the xylene isomerization reaction. As one of the few molecular sieves that has been industrially produced, how to further improve its catalytic performance has become an important topic for relevant researchers. [0003] In recent years, multi-level pore molecular sieves have become a hot topic in molecular sieve research. By introducing mesoporous structures into the structure of microporous molecular sieves, the surface area of ​​molecular sieves is increased, which is conducive to the diffusion of product...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04B01J29/70
CPCC01B39/04B01J29/7023C01P2002/72
Inventor 李晓峰张燕挺刘春滋窦涛
Owner TAIYUAN UNIV OF TECH
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