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Method for synthesizing molecular sieve of ZSM-5 zeolite in small crystal grain

A synthesis method, the technology of ZSM-5, is applied in the directions of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., which can solve the difficulty of reducing crystallization temperature, prolonging crystallization time, and ZSM-5 molecular sieve. and other problems, to achieve the effect of uniform grains, short synthesis time and small grains

Inactive Publication Date: 2009-01-28
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

ZSM-5 molecular sieves synthesized by conventional methods generally have larger crystal grains, and the grain size is generally about 2-5 μm. However, it is very difficult to synthesize ZSM-5 molecular sieves with small grains by conventional methods.
[0012] Existing methods for synthesizing small-grain ZSM-5 zeolite molecular sieves have their own disadvantages: either adding certain salts or other substances; or using expensive sodium-free reagents or organic templates, or needing to reduce crystallization temperature, prolong the crystallization time; or add surfactants; or use inert mesoporous materials as space-limited substances

Method used

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  • Method for synthesizing molecular sieve of ZSM-5 zeolite in small crystal grain
  • Method for synthesizing molecular sieve of ZSM-5 zeolite in small crystal grain
  • Method for synthesizing molecular sieve of ZSM-5 zeolite in small crystal grain

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take 60 grams of ethyl orthosilicate, add 100 grams of deionized water to it, make it fully dissolved, then add 2 grams of sulfuric acid, adjust the pH value of the solution to 1.0, 7.2 grams of tetrapropylammonium bromide, stir well at 25 ° C Hydrolyze for 6 hours to make solution A; add 4.5 grams of aluminum sulfate to 95 grams of water to make solution B, and slowly add solution B to solution A. Then add 0.5 gram of NaOH solids, and add 2.0 grams of ZSM-5 molecular sieve seed crystals, stir after adding, make the mol ratio of the total composition of the mixture be (Na 2 O): (SiO 2 ): (Al 2 o 3 ): (H 2 O): Q = 5: 40: 1: 40: 0.1, packaged in a high-pressure hydrothermal kettle, crystallized at 160°C for 20 hours, washed the resulting product to neutrality, centrifuged, dried, and roasted to obtain ZSM-5 zeolite Molecular sieve raw powder. attached figure 1 The XRD pattern of the small-grain sample obtained in this case and the standard ZSM-5 zeolite molecular si...

Embodiment 2

[0032] Repeat the operating steps of Example 1, the difference is that the silicon source is methyl orthosilicate, the results are shown in the attached image 3 , as can be seen from the figure, the obtained product is a small crystal ZSM-5 zeolite molecular sieve, see attached table 1.

Embodiment 3

[0034]The operation steps of Example 1 were repeated, except that the silicon source was hydrolyzed at pH=2.0, and as a result, a ZSM-5 molecular sieve with small crystal grains could also be obtained, see attached table 1.

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Abstract

This invention relates to a method for synthesizing ZSM-5 zeolite molecular sieve, especially a method for rapidly synthesizing ZSM-5 zeolite molecular sieve with small grains. The method comprises: (1) adjusting the pH value of a mixture of silicon source and deionized water with an acid solution, stirring for hydrolysis, and adding organic templating agent to obtain solution A; (2) dissolving aluminum source with deionized water to obtain solution B; (3) dropping solution B into solution A slowly, and adding molecular sieve seed crystal; (4) placing the mixture into a hydrothermal kettle, crystallizing, washing the product, centrifuging, drying and torrefying to obtain ZSM-5 zeolite molecular sieve with small grains. The method is simple and time efficient, and the obtained ZSM-5 zeolite molecular sieve has small and uniform grains.

Description

technical field [0001] The invention relates to a method for synthesizing a ZSM-5 zeolite molecular sieve, in particular to a method for rapidly synthesizing a small-grain ZSM-5 zeolite molecular sieve. Background technique [0002] The ZSM-5 zeolite molecular sieve (USP 3702886, 1972) invented by Mobil Petroleum Company of the United States has been widely used in petrochemical processes such as shape-selective catalysis, isomerization, disproportionation, and alkylation. However, due to its narrow pores and high diffusion resistance of reactants or products, zeolite catalytic materials are increasingly unable to meet the needs of more and more macromolecules and liquid phase reactions in the fields of fine chemicals, while small-grain zeolites are due to their outer surface. The increase increases the number of acid sites on the outer surface, and because the diffusion path on the inner surface is shortened, the catalytic activity is higher, and the efficiency of the catal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/40
Inventor 王军任晓乾陆由东吴雅静
Owner NANJING TECH UNIV
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