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ZSM-5 molecular sieve and preparation method thereof

A ZSM-5, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of complex surfactants and cumbersome processes, achieve difficult agglomeration and improve utilization. rate, the effect of reducing the internal diffusion resistance

Inactive Publication Date: 2019-08-23
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The surfactant used in this preparation method is complicated, and the process is also very loaded down with trivial details

Method used

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  • ZSM-5 molecular sieve and preparation method thereof
  • ZSM-5 molecular sieve and preparation method thereof
  • ZSM-5 molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] The present embodiment provides a kind of preparation method of ZSM-5 molecular sieve, it comprises the following steps:

[0057] Get 1.45g ammonium fluoride (content≧96.0wt%), add 40.10g deionized water, after dissolving, add 2.45g aluminum sulfate (content≧99.0wt%), 14.61g tetrapropyl ammonium hydroxide (content 25.0wt%) %), after mixing uniformly, add 23.67g silica gel (content 94.0wt%), stir well, make gel reaction mixture;

[0058] The gel reaction mixture was aged at 80°C for 16 hours;

[0059] Put the above-mentioned gel reaction mixture into a reaction kettle, put the reaction kettle into an oven, crystallize at 140° C. for 28 hours, filter, wash and dry to obtain ZSM-5 molecular sieve.

[0060] The obtained ZSM-5 molecular sieve is characterized by XRD technology, and the obtained XRD pattern is as follows figure 1 As shown, it is characterized by SEM, and the SEM picture is obtained as figure 2 As shown, the measured silicon-aluminum ratio of the above-men...

Embodiment 2

[0062] The present embodiment provides a kind of preparation method of ZSM-5 molecular sieve, it comprises the following steps:

[0063] Take 9.72g sodium fluoride (content≧99.0wt%), add 81.00g deionized water, after dissolving, add 5.01g aluminum sulfate (content≧99.0wt%), 9.57g tetrapropylammonium bromide (content≧99.0 wt%), after mixing evenly, add 47.34g silica gel (content 94.0wt%), stir evenly, make the gel reaction mixture;

[0064] The gel reaction mixture was aged at 50°C for 24 hours;

[0065] Put the above gel reaction mixture into a reaction kettle, put the reaction kettle into an oven, crystallize at 180° C. for 20 hours, filter, wash and dry to obtain ZSM-5 molecular sieve.

[0066] The obtained ZSM-5 molecular sieve is characterized by XRD technology, and the obtained XRD pattern is as follows image 3 As shown, it is characterized by SEM, and the SEM picture is obtained as Figure 4 As shown, the measured silicon-aluminum ratio of the above-mentioned ZSM-5 i...

Embodiment 3

[0068] The present embodiment provides a kind of preparation method of ZSM-5 molecular sieve, it comprises the following steps:

[0069] Take 7.73g hydrofluoric acid (content≧40.0wt%), add 79.89g deionized water, after dissolving, add 4.98g aluminum sulfate (content≧99.0wt%), 9.60g tetrapropylammonium bromide (content≧99.0 wt%), after mixing uniformly, add 47.42g white carbon black (content 94.0wt%), stir well, obtained gel reaction mixture;

[0070] The gel reaction mixture was aged at 60°C for 22 hours;

[0071] Put the above gel reaction mixture into a reaction kettle, put the reaction kettle into an oven, crystallize at 190° C. for 18 hours, filter, wash and dry to obtain ZSM-5 molecular sieve.

[0072] The obtained ZSM-5 molecular sieve was characterized with a zeolite, and it was measured that the silicon-aluminum ratio of the above-mentioned ZSM-5 was 97.4, the relative crystallinity was 98%, and the morphology was thin-plate type.

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Abstract

The invention provides a preparation method of a sheet ZSM-5 molecular sieve. The method includes: in a gel preparation process, mixing a silicon source, an aluminum source, a template agent and an additive, and performing stirring at 10-50DEG C for 1-20h; conducting standing aging for 10-30h at 10-90DEG C; putting the prepared gel reaction mixture into a reaction kettle, then putting the reactionkettle into an oven, conducting crystallization at 100-220DEG C for 4-30h, then taking the product out, and carrying out filtering, washing and drying to obtain the ZSM-5 molecular sieve product. Themethod provided by the invention synthesizes the ZSM-5 molecular sieve under a solid like phase condition, and the obtained ZSM-5 molecular sieve product is sheet shaped, and has a relative crystallinity of 90-110%, and an SiO2 / Al2O3 molar ratio of less than or equal to 100.

Description

technical field [0001] The invention relates to a method for preparing thin-plate ZSM-5 molecular sieves with high crystallinity and a silicon-aluminum molar ratio≦100 by using additives under solid-like conditions, and belongs to the technical field of preparation of inorganic materials and catalysts. Background technique [0002] ZSM-5 molecular sieve has unique pore structure, thermal / hydrothermal stability, high solid acidity and excellent shape selectivity, and has been widely used in industrial processes such as aromatization, isomerization and alkylation. Modified high-silicon ZSM-5 molecular sieves are often used as additives in catalytic cracking catalysts to increase the production of propylene in liquefied gas. In some industrial reactions, the shape selectivity of ZSM-5 is used to obtain para-substituted alkylbenzenes. ZSM-5 molecular sieve has also been proved to be a very effective material for the catalytic effect of MTP / MTO reaction. Since the grain size and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03
Inventor 郭成玉李兆飞郭广娟沈宜泓刘其武邢昕崔岩庞新梅李发永
Owner PETROCHINA CO LTD
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