Synthesis method of particle-size-controllable needle-shaped ZSM-5 molecular sieve

A technology of ZSM-5 and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of cumbersome preparation process, long crystallization time, and large environmental pollution. Achieve the effects of reducing environmental pollution, reducing synthesis costs, and avoiding cumbersome steps

Active Publication Date: 2019-04-26
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the prior art obtains zeolites with different particle sizes, especially acicular nano ZSM-5 zeolite molecular sieves. The preparation process is cumbersome, the crystallization time is long, the cost is high, the environment is polluted, and it is not easy to industrialize.

Method used

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  • Synthesis method of particle-size-controllable needle-shaped ZSM-5 molecular sieve
  • Synthesis method of particle-size-controllable needle-shaped ZSM-5 molecular sieve

Examples

Experimental program
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Embodiment 1

[0029] Synthesis method: Add 15g of water, 0.051g of aluminum sulfate octadecahydrate, 12g of tetrapropylammonium hydroxide, and 16g of cyclohexylamine into the reaction kettle, and after stirring evenly, slowly add 15g of it drop by drop during the stirring process with a mass fraction of 40% Silica sol, described silica sol is processed by adding 2.3g sodium hydroxide in advance, the average molecular weight D of silica sol recorded by small angle X-ray diffraction method is 12000, and D is divided by repeating unit SiO 2 Calculate the molecular weight of 60, control the degree of silicon polymerization to obtain 200, stir for 30 minutes, and age the gel at room temperature. After that, crystallize at 180°C for 2 days under stirring at 150rpm, after cooling to room temperature, wash and centrifuge with deionized water for 3 times, and dry at 80°C for 12 hours to obtain the final product Z-1.

[0030] figure 1 It is the XRD spectrogram of the product obtained in Example 1, i...

Embodiment 2

[0032] Using the same conditions as in Example 1, after stirring evenly, slowly add 6.93g ethyl orthosilicate dropwise during the stirring process, and the ethyl orthosilicate is treated by adding 3g sodium hydroxide in advance to control the degree of silicon polymerization to 80, stirred for 30min, and aged at room temperature. After that, it was crystallized at 180°C and 150rpm for 2 days, cooled to room temperature, washed and centrifuged with deionized water for 3 times, and dried at 80°C for 12 hours to obtain the final product Z-2. According to the XRD characterization results of the sample, it can be seen that the product has the characteristic diffraction peak of ZSM-5, and the SEM photo of the obtained product shows that the sample presents a needle-shaped morphology, and the particle diameter is 100-200 nanometers.

Embodiment 3

[0034] Using the same conditions as in Example 1, after stirring evenly, slowly add 2 g of silicon powder dropwise during the stirring process, and the silicon powder is treated by adding 2.5 sodium hydroxide in advance to control the degree of silicon polymerization to 100, stir for 30 minutes, and Gel aging. After that, it was crystallized at 180°C and 150rpm for 2 days, cooled to room temperature, washed and centrifuged with deionized water for 3 times, and dried at 80°C for 12 hours to obtain the final product Z-3. According to the XRD characterization results of the sample, it can be seen that the product has the characteristic diffraction peak of ZSM-5, and the SEM photos of the obtained product show that the sample presents a needle-like shape, and the particle diameter is 1-2 microns.

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Abstract

The invention belongs to the technical field of zeolite molecular sieve synthesis, and particularly relates to a synthesis method of a particle-size-controllable needle-shaped ZSM-5 molecular sieve. The particle size and shape of zeolite are important factors affecting the catalytic property of the molecular sieve. According to the synthesis method, by simply adjusting the polymerization degree ofa silicon source and an aluminum source and adopting a mixed template agent, the particle size of the zeolite can be controlled effectively, and meanwhile, the needle-shaped zeolite is obtained. Thesynthesis method is very simple and convenient in synthesis step and very easy to industrialize. A sample XRD and an SEM display change of the silicon polymerization degree so that the particle size of the zeolite can be controlled effectively.

Description

technical field [0001] The invention belongs to the technical field of zeolite molecular sieve synthesis, in particular to a method for synthesizing acicular ZSM-5 molecular sieves with controllable particle size. Background technique [0002] Zeolite is a kind of microporous crystalline aluminosilicate (aluminosilicate), the skeleton of which is usually composed of silicon-oxygen tetrahedrons and aluminum-oxygen tetrahedrons connected to each other by covalent bonds (the general chemical formula is [M 2 (I),M(II)]O·Al 2 o 3 · nSiO2 2 mH 2 O, (wherein M(I) and M(II) are monovalent and divalent metals (usually Na, Ca, Ka, etc., n is the zeolite silicon-aluminum ratio)). ZSM-5 zeolite belongs to the second generation zeolite and has a typical MFI structure. Due to its special two-dimensional straight pore system and intersecting pore structure, high hydrothermal stability, shape selectivity, and lipophilic and hydrophobic capabilities, ZSM-5 has gradually developed into t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03C01P2004/10
Inventor 史静滕加伟徐建军
Owner CHINA PETROLEUM & CHEM CORP
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