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Preparation method of nanometer Zn/Al ZSM-5 molecular sieve

A molecular sieve and nanotechnology, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of high cost, serious pollution, high toxicity, etc., and achieve reduced production cost and good nanometer characteristics , to solve the effect of high toxicity

Active Publication Date: 2012-11-28
HEILONGJIANG UNIV
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Problems solved by technology

[0004] The present invention aims to solve the problems of high cost, high toxicity, and serious pollution in the preparation of Zn / AlZSM-5 molecular sieves by the high dosage of template agent used in the existing isomorphic replacement method, so as to provide a seed crystal-guided method with low dosage of template agent. The Method of Nano Zn / AlZSM-5 Molecular Sieve

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  • Preparation method of nanometer Zn/Al ZSM-5 molecular sieve
  • Preparation method of nanometer Zn/Al ZSM-5 molecular sieve
  • Preparation method of nanometer Zn/Al ZSM-5 molecular sieve

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specific Embodiment approach 1

[0021] Specific embodiment one: the preparation method of a kind of nanometer Zn / AlZSM-5 molecular sieve of the present embodiment is realized through the following steps:

[0022] 1. Preparation of precrystallized seed crystals: a. Weigh 1 part of aluminum isopropoxide, 24 to 115 parts of tetrapropylammonium hydroxide aqueous solution, 21 to 83 parts of ethyl orthosilicate and 1.6~5.7 parts of deionized water; Wherein, the mass percent concentration of tetrapropyl ammonium hydroxide in the tetrapropyl ammonium hydroxide aqueous solution is 30%; b, aluminum isopropoxide and tetrapropyl ammonium hydroxide are added to deionized water In deionized water, stir for 10 to 30 minutes at a stirring speed of 300 to 500 r / min; c. Add ethyl orthosilicate dropwise to the liquid obtained in step b at the same stirring speed, and all ethyl orthosilicate Continue to stir for 2 hours after the dropwise addition to obtain a mixed gel; d. Place the mixed gel obtained in step c in a stainless s...

specific Embodiment approach 2

[0029] Specific embodiment 2: The difference between this embodiment and specific embodiment 1 is that the crystallization temperature in step d of step 2 is 135-155° C., and the crystallization time is 10-15 hours. Other steps and parameters are the same as those of specific embodiment 1. .

specific Embodiment approach 3

[0030] Specific embodiment 3: This embodiment differs from specific embodiment 1 or 2 in that: the crystallization temperature in step d of step 2 is 150°C, the crystallization time is 12h, and other steps and parameters are the same as specific embodiment 1 or 2 .

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Abstract

The invention discloses a preparation method of a nanometer Zn / Al ZSM-5 molecular sieve, relates to the preparation method of a nanometer molecular sieve, and aims to solve the problems that the nanometer Zn / Al ZSM-5 molecular sieve is prepared by the existing method, the template agent usage amount is high, the template removing agent roasting time is long, the cost is high, the toxicity is high, and the pollution is serious. The preparation method comprises the following steps of: preparing gel by aluminum isopropoxide, tetrapropylammonium hydroxide, tetraethoxysilane and deionized water, and crystallizing the gel so as to obtain a pre-crystallized seed crystal; and adding the pre-crystallized seed crystal which takes up 1%-5% of the total mass of the gel into a mixed gel prepared by zinc nitrate hexahydrate, sodium hydroxide, partial sodium aluminate, deionized water and silica sol, thereby obtaining the nanometer Zn / Al ZSM-5 molecular sieve through centrifugation, washing, drying, roasting and cooling after crystallization. The nanometer Zn / Al ZSM-5 molecular sieve disclosed by the invention is low in template agent usage amount, short in template removing agent roasting time, low in cost, low in toxicity, and tiny in pollution. The nanometer Zn / Al ZSM-5 molecular sieve disclosed by the invention is suitable for production of the nanometer molecular sieve.

Description

technical field [0001] The present invention relates to the preparation method of nanometer molecular sieve. Background technique [0002] ZSM-5 molecular sieve has become one of the most important molecular sieve catalytic materials today due to its unique pore structure, adjustable acid sites, good hydrothermal stability and excellent shape-selective catalysis, and is widely used in petroleum processing and petrochemical industry , Coal chemical industry and fine chemical industry. Compared with micron-sized ZSM-5 molecular sieves, nano ZSM-5 molecular sieves have larger specific surface area and shorter pore size due to smaller crystal grains, which can effectively reduce the diffusion resistance of reactants and products in the pores. Improve the reactivity and anti-coking deactivation ability of the catalyst, especially in the process of the shape-selective alkylation of aromatics and the aromatization of olefins to produce petrochemical products and clean fuel oil, sh...

Claims

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Application Information

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IPC IPC(8): C01B39/40
Inventor 吴伟王高亮闫鹏飞昝望王文静
Owner HEILONGJIANG UNIV
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