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Nanocluster mesoporous ZSM-5 molecular sieve and preparation method thereof

A ZSM-5, nano-cluster technology, applied in nanotechnology, crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of long time, complicated process, etc., and achieve low cost , Simple operation, high crystallinity effect

Active Publication Date: 2022-07-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this patent, the molecular sieve crystallization process adopts three-stage temperature control, the process is relatively complicated, and the time is long. The synthesized molecular sieve is suitable for MTO reaction, and does not involve ZSM-5 molecular sieve for catalytic cracking.

Method used

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  • Nanocluster mesoporous ZSM-5 molecular sieve and preparation method thereof
  • Nanocluster mesoporous ZSM-5 molecular sieve and preparation method thereof
  • Nanocluster mesoporous ZSM-5 molecular sieve and preparation method thereof

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Embodiment approach

[0052] According to the nano-cluster mesoporous ZSM-5 molecular sieve and synthesis method provided by the present invention, an implementation method includes the following steps:

[0053] (1) The template agent and deionized water are mixed uniformly, and then the silicon source is added, and stirred at 30°C-50°C for 0.5-3.0 h; wherein the molar ratio of the template agent and the silicon source calculated as silica is 0.1-0.5: 1. The molar ratio of water and silicon source in terms of silica is 80-120:1;

[0054] (2) Add alkali metal hydroxide to deionized water to dissolve, then add aluminum source, and stir at room temperature preferably at 20-30°C for 0.5-2.0 h; wherein, the molar ratio of water and alkali metal hydroxide is 75-300:1 For example 140-250, H 2 O / Al 2 O 3 Molar ratio = 600-1500;

[0055] (3) The product of step (2) is slowly added to the product of step (1), mixed uniformly, and preferably stirred at room temperature at 25-30° C. for 1.0-5.0 h to obtain...

Embodiment 1

[0066] (1) Weigh 103 grams of tetrapropylammonium hydroxide (concentration 25.0% by weight), add 758 grams of deionized water, stir at room temperature for 10 min, then add 110 grams of ethyl orthosilicate, and stir for 2.0 h;

[0067] (2) Weigh 2.5 grams of sodium hydroxide particles, add 244 grams of deionized water to completely dissolve the sodium hydroxide, then add 16.0 grams of aluminum nitrate, and stir at 25 ° C for 1.0 h;

[0068] (3) slowly adding the solution of step (2) into step (1), mixing evenly, and stirring at 25°C for 4.0h;

[0069] (4) Transfer the precursor liquid into the synthesis kettle, and dynamically crystallize it at 170°C for 48h;

[0070] (5) After crystallization, centrifugal filtration, washing, drying, and calcination at 550° C. for 4 h.

Embodiment 2

[0072] (1) Weigh 53 grams of tetrapropylammonium bromide (25.0%), add 700 grams of deionized water, stir at room temperature for 10min, then add 100 grams of methyl orthosilicate, and stir for 5.0h under 30°C water bath conditions;

[0073] (2) Weigh 2.5 grams of sodium hydroxide particles, add 180 grams of deionized water to completely dissolve the sodium hydroxide, then add 4.0 grams of sodium aluminate, and stir at room temperature for 2.0h;

[0074] (3) adding the solution of step (2) into step (1), mixing uniformly, and stirring at room temperature for 4.0h;

[0075] (4) Transfer the precursor liquid into the synthesis kettle, and dynamically crystallize it at 180°C for 24h;

[0076] (5) After crystallization, centrifugal filtration, washing, drying, and calcination at 500° C. for 6 h.

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Abstract

The invention belongs to the technical field of ZSM-5 molecular sieve preparation, and relates to a nanocluster mesoporous ZSM-5 molecular sieve and a preparation method thereof.The nanocluster mesoporous ZSM-5 molecular sieve particles are formed by stacking nanocrystals and have intercrystalline pores formed by stacking the nanocrystals, the average grain size of the nanocrystals is 80-120 nm, and the average grain size of the nanocrystals is 80-120 nm. The most probable aperture of the macropores of the nanocluster mesoporous ZSM-5 molecular sieve is 250 to 350 nm, and the most probable aperture of the mesopores of the nanocluster mesoporous ZSM-5 molecular sieve is 13 to 17 nm. The preparation method comprises the following steps: forming slurry containing a template machine and a silicon source under certain conditions, forming slurry containing alkali and an aluminum source, mixing the slurry containing the template machine and the silicon source and the slurry containing alkali and the aluminum source under certain conditions to form a synthetic liquid, crystallizing and recycling. The ZSM-5 molecular sieve has relatively good performance.

Description

technical field [0001] The invention relates to a nano-cluster mesoporous ZSM-5 molecular sieve and a preparation method thereof. Background technique [0002] Zeolite molecular sieve is a kind of microporous crystalline material with framework structure, with pore structure of specific size and shape, large specific surface area and strong adjustable acid properties. It is widely used in the process of petroleum refining and processing. Such as catalytic cracking, alkane isomerization, catalytic reforming and toluene disproportionation and other catalytic reactions. Catalytic materials are the core of new catalysts. In order to achieve the shape-selective properties of molecular sieve catalysts, reduce the loss of catalyst activity, and achieve high activity under the premise of high selectivity, it is urgent to develop shape-selective catalysts with better performance. [0003] ZSM-5 belongs to the orthorhombic crystal system, and the unit cell parameters are The number...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40B82Y40/00
CPCC01B39/40B82Y40/00C01P2004/64C01P2004/62C01P2006/16C01P2004/61C01P2004/03C01P2004/04Y02P20/52
Inventor 韩蕾林伟宋海涛王鹏王丽霞周翔赵留周王若瑜王振波
Owner CHINA PETROLEUM & CHEM CORP
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