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Preparation method of nanocrystalline zsm-5 zeolite cluster and nanocrystalline zsm-5 zeolite cluster prepared by the method

A ZSM-5, nanocrystalline technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of high-speed centrifugation, template price restriction, catalyst deactivation and so on

Inactive Publication Date: 2016-01-06
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The size of ZSM-5 zeolite as a catalyst support is usually in the micron range, and it has good catalytic activity for reaction materials involving small molecules, but coking, which is limited by diffusion control, is still a key factor for catalyst deactivation
Nano-zeolites (<100nm) have high catalytic activity and short molecular diffusion channels, and have important applications in molecular sieve membrane reactors; however, nano-powders are used as catalysts directly because of the need for high-speed centrifugation for separation and recovery, and so far are rarely used in industry. have practical application
Although in recent years, hierarchical porous molecular sieves using various templates as mesoporous or macroporous pore-forming agents have been continuously synthesized, the price of templates is the key to restricting practical applications.
[0003] So far, this field has not developed a method that combines the catalytic activity of nano zeolite and the advantages of easy separation of particles from the synthesis system and reaction system when used without any external mesoporous or macroporous templates, and has more industrial application value. A method for zeolite nanocrystal clusters

Method used

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  • Preparation method of nanocrystalline zsm-5 zeolite cluster and nanocrystalline zsm-5 zeolite cluster prepared by the method
  • Preparation method of nanocrystalline zsm-5 zeolite cluster and nanocrystalline zsm-5 zeolite cluster prepared by the method
  • Preparation method of nanocrystalline zsm-5 zeolite cluster and nanocrystalline zsm-5 zeolite cluster prepared by the method

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preparation example Construction

[0025] In the first aspect of the present invention, a kind of preparation method of nanocrystalline ZSM-5 zeolite cluster is provided, and the method comprises the following steps:

[0026] 1) Preparation of high-concentration precursor solution: mix ethyl silicate and aluminum isopropoxide and add a certain amount of deionized water, stir evenly, add tetrapropylammonium hydroxide to the above system, at 20-60°C Stir until clear liquid;

[0027] 2) Low-temperature hydrothermal nucleation stage: Stir the high-concentration precursor solution obtained in step 1) in an oil bath at 95-100°C for 1-2 days to generate a large number of nanocrystals, and the number of nanocrystals is controlled in the system The concentration of NaOH, the molar ratio of the system is: 1 mole of aluminum isopropoxide: 50 moles of ethyl silicate: 9 moles of tetrapropyl ammonium hydroxide: 7.5-12 moles of sodium hydroxide: 2300-2400 moles of water, the reaction vessel It is a Duran bottle with good sea...

Embodiment 1

[0040]Mix 0.3066g of aluminum isopropoxide and 15.624g of ethyl silicate and add 26g of water to stir at room temperature for 1 hour, then add 10.98g of tetrapropylammonium hydroxide (25% by weight) dropwise, and then add 0.72g of NaOH dropwise after 2 hours The mixed solution with 30g of water was stirred at 40°C for 3-6 hours to become a clear solution, and transferred to an oil bath at 100°C to continue stirring for 2 days. The above reaction was carried out in a 250ml Duran bottle with good sealing performance. After the above solution was cooled to room temperature, 90ml of water and 24g of ethanol were added, and the mixed system was placed in a hydrothermal kettle at 150°C to continue crystallization for 24 hours, and the powder obtained by suction filtration was dried in an oven at 100°C for 10 hours, and the system The molar ratio is: 1 mole of aluminum isopropoxide: 50 moles of ethyl silicate: 9 moles of tetrapropylammonium hydroxide: 12 moles of sodium hydroxide: 174...

Embodiment 2-3

[0042] According to the method of Example 1, the consumption of NaOH was adjusted to 0.54g and 0.45g respectively, keeping other parameters unchanged. The SEM figures of embodiment 2 and embodiment 3 are respectively figure 1 In C, D and E, F, as shown, similarly, the obtained material is a nanocrystalline cluster with a particle size of 500-800nm, and a nanocrystalline particle size of 30-80nm forms a near-spherical cluster according to a certain orientation. The TEM (transmission electron microscope) and HRTEM (high resolution transmission electron microscope) pictures of embodiment 2 are shown in figure 2 as shown, figure 2 The HRTEM and electron diffraction patterns show that the small grains grow into ellipsoidal clusters with a size of about 500nm according to a certain orientation. It can be seen that when NaOH is adjusted within a certain range, the microstructure of the material is still nanocrystalline clusters, and high concentration of sodium hydroxide can redu...

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Abstract

The invention relates to a preparation method of nanocrystalline ZSM-5 zeolite cluster, and the nanocrystalline ZSM-5 zeolite cluster prepared by the method, and provides the preparation method of the nanocrystalline ZSM-5 zeolite cluster. The method comprises the steps of: 1) preparing precursor liquid; 2) carrying out low-temperature hydrothermal nucleation; 3) carrying out high-temperature hydrothermal growth; and 4) separating, washing, drying and calcining. The invention also provides the nanocrystalline ZSM-5 zeolite cluster prepared by the method.

Description

technical field [0001] The invention belongs to the field of inorganic material synthesis. Specifically, the present invention relates to a method for preparing nanocrystalline ZSM-5 zeolite clusters. In this method, by adjusting the concentration of sodium hydroxide (NaOH), a large amount of nucleation of a high-concentration precursor solution is made under low-temperature hydrothermal conditions, and then the High-temperature hydrothermal further crystallization promotes the growth of zeolite, and zeolite clusters with a size of 500-1000nm are prepared without any mesoporous or macroporous template. Each zeolite cluster is composed of small crystals with particles of about 30-80nm The particles grow according to a certain orientation, and the specific surface area of ​​the material is 300-370m 2 / g, the pore volume is 0.1-0.27cm 3 / g. Background technique [0002] ZSM-5 zeolite belongs to MFI type molecular sieve, Pnma space group, ten-membered ring intersecting channe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/38
Inventor 朱颜华子乐施剑林
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI