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Method for effectively controlling particle size of ZSM-5 by virtue of silicon polymerization degree and aluminum polymerization degree

A ZSM-5, polymerization degree technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, nanotechnology, etc., can solve the problems of cumbersome preparation process, large environmental pollution, and difficulty in industrialization. , to achieve the effect of reducing environmental pollution, avoiding cumbersome steps, and suitable for industrialization

Active Publication Date: 2017-05-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The key technical problem to be solved by the present invention is that the prior art obtains zeolites with different particle sizes, especially 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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  • Method for effectively controlling particle size of ZSM-5 by virtue of silicon polymerization degree and aluminum polymerization degree
  • Method for effectively controlling particle size of ZSM-5 by virtue of silicon polymerization degree and aluminum polymerization degree
  • Method for effectively controlling particle size of ZSM-5 by virtue of silicon polymerization degree and aluminum polymerization degree

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Synthetic method: Add 15g of water, 0.051g of aluminum sulfate octadecahydrate, and 12g of tetrapropylammonium hydroxide into the reaction kettle. After stirring evenly, slowly add 5g of silica sol with a mass fraction of 40% during the stirring process, and add Sodium hydroxide, control the degree of polymerization of silicon to 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.

[0028] figure 1 It is the XRD spectrogram of the product obtained in Example 1, it can be seen that the product has the characteristic diffraction peak of ZSM-5, and has a higher crystallinity. figure 2 It is the SEM photo of the product obtained in Example 1. It can be seen that the sample presents a spherical shape, and the particle size is 3 microns.

Embodiment 2

[0030] Using the same conditions as in Example 1, after stirring evenly, slowly add 6.93 g of ethyl orthosilicate dropwise during the stirring process, add sodium hydroxide, control the degree of silicon polymerization to 80, stir for 30 minutes, and age the gel 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 ZSM-5 characteristic diffraction peaks, image 3 It is the SEM photo of the product obtained in Example 2, indicating that the sample presents a spherical shape, and the particle size is 100-200 nanometers.

Embodiment 3

[0032] Using the same conditions as in Example 1, after stirring evenly, slowly add 2 g of silicon powder dropwise during the stirring process, add sodium hydroxide, control the degree of polymerization of silicon to 100, stir for 30 minutes, and age the gel 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-3. According to the XRD characterization results of the sample, it can be seen that the product has ZSM-5 characteristic diffraction peaks, Figure 4 It is the SEM photograph of the product obtained in Example 3, indicating that the sample presents a spherical shape, and the particle size is 2 microns.

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Abstract

The invention belongs to the technical field of zeolite molecular sieve synthesis, and particularly discloses a method for effectively controlling the particle size of a ZSM-5 zeolite molecular sieve by virtue of different silicon polymerization degrees and aluminum polymerization degrees. The particle size of a zeolite is an important influence factor for the catalytic performance of a molecular sieve. The particle size of the zeolite can be effectively controlled mainly by simply regulating silicon source and aluminum source polymerization degrees. Synthesis steps of the method are very convenient and easy for industrialization. Samples XRD and SEM show that the particle size of the zeolite is effectively controlled by changing the silicon polymerization degree.

Description

technical field [0001] The invention belongs to the technical field of zeolite molecular sieve synthesis, in particular to a method for effectively controlling the particle size of a ZSM-5 zeolite molecular sieve by utilizing the degree of silicon polymerization and the degree of aluminum polymerization. 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 se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40B82Y40/00
CPCC01B39/40C01P2002/72C01P2004/03C01P2004/32C01P2004/61C01P2004/62C01P2004/64
Inventor 史静滕加伟徐建军何万仁
Owner CHINA PETROLEUM & CHEM CORP
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