Preparation of binderless ZSM-11 zeolite

A ZSM-11, binder-free technology, applied in the direction of crystalline aluminosilicate zeolite, borane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of reduced effective surface area, easy deactivation and aggregation, and small zeolite size and other problems, to achieve the effect of accelerating the transformation speed, avoiding the nucleation growth period, and reducing the grain size

Active Publication Date: 2009-01-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the size of zeolite is too small, which is not very convenient in practical application, and has disadvantages such as difficult recovery, easy deactivation and aggregation. It is necessary to add a binder during the molding process, which reduces the effective surface area and introduces diffusion restrictions.

Method used

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  • Preparation of binderless ZSM-11 zeolite
  • Preparation of binderless ZSM-11 zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～3

[0014] Use tetrabutylammonium hydroxide (TBAOH) solution, tetraethylorthosilicate (TEOS) and water according to (TBA) 2 O: 6.22TEOS: 163H 2 The molar ratio of O was mixed and stirred evenly, aged and refluxed at 95° C. for three days to obtain the ZSM-11 seed crystal directing agent.

[0015] Take by weighing 200 grams of white carbon black, 12.5 grams of scallop powder, 36 grams of silicon-containing alumina powder (containing SiO 2 The mass percentage is 26%) and 51 grams of ZSM-11 seed crystal directing agent, adding an aqueous solution containing 20 grams of NaOH, and then adding 475 grams of silica sol (40% by weight) for kneading and drying to obtain a cylindrical precursor.

[0016] 40 grams of the cylindrical precursor prepared above and 80 grams of tetrabutylammonium hydroxide (TBAOH) solution with a concentration of 8% by mass were mixed and placed in a crystallization kettle at 160°C for hydrothermal treatment for 3 days, 5 days and 7 days. The product was washed...

Embodiment 4～6

[0018] Take by weighing 100 grams of diatomaceous earth and 140 grams of white carbon black, add 7.5 grams of field turnip powder, 36 grams of aluminum sulfate [Al 2 (SO 4 ) 3 18H 2 O] and 60 grams of the seed directing agent prepared in [Example 1-3], and then add 300 grams of silica sol (40% by weight) to knead into a cylindrical shape and dry.

[0019] 40 grams of the above-prepared cylindrical precursor and 80 grams of 10% tetrabutylammonium hydroxide (TBAOH) solution were mixed and placed in a crystallization kettle at 140° C. for 5 days, 8 days and 10 days. The product was washed and dried with distilled water and then calcined at 550°C in an air atmosphere. The XRD patterns of the products all show that the crystalline phase is ZSM-11 zeolite, and the baseline is straight, indicating that no amorphous substance is contained. The SEM photos of the product show that the particle size of the ZSM-11 zeolite is less than 100 nanometers.

Embodiment 7～10

[0021] Use tetrabutylammonium hydroxide (TBAOH) solution, tetrabutylammonium bromide (TBABr), tetraethylorthosilicate (TEOS) and water according to 2TBAOH: TBABr: 15TEOS: 450H 2 The molar ratio of O was mixed and stirred uniformly, aged and refluxed at 100° C. for four days to obtain the ZSM-11 seed crystal directing agent.

[0022] Take by weighing 250 grams of white carbon black, add 12 grams of scallop powder, 27.8 grams of aluminum sulfate [Al 2 (SO 4 ) 3 18H 2 O], 10 grams of NaOH and 80 grams of seed directing agent, and then add 400 grams of silica sol (40% by weight) for kneading into a cylindrical shape for drying.

[0023] 40 grams of the cylindrical precursor prepared above and 80 grams of tetrabutylammonium hydroxide (TBAOH) solution with a concentration of 8% by mass were mixed and placed in a crystallization kettle at 180°C for hydrothermal treatment for 2 days, 4 days and 6 days. The product was washed and dried with distilled water and then calcined at 550...

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Abstract

The invention relates to a method for preparing no-binding agent ZSM-11 zeolite, which mainly aims at overcoming the defects of difficult recovery, easy deactivation and easy aggregation existing in the practical application of the zeolite powder and the problems of small effective surface area and limited diffusion due to the addition of the binding agent in the forming process. In the invention, at least one of diatomaceous earth, carbon white, silicasol or water glass is taken as a silicon source, at least one of aluminum oxide, aluminum salt or aluminate is taken as an aluminum source, and proper quantity of necessary crystal seed guiding agents are added and subjected to pugging, extrusion and forming so as to obtain a precursor mixture with the mass ratio of XNa2O:YAl2O3:100SiO2, wherein x is between 0.5 and 14, and y is between 0 and 6, and the precursor mixture is subjected to hydrothermal crystallization treatment in the water solution containing tetrabutyl ammonium positive ions and converted to the no-binding agent ZSM-11 zeolite. The technical proposal of the invention better resolves the problems, and can be applied to the industrial preparation of the ZSM-11 zeolite molecular sieve catalyst.

Description

technical field [0001] The invention relates to a preparation method of binder-free ZSM-11 zeolite. Background technique [0002] Zeolite molecular sieves have uniform and ordered micropores, large specific surface area, and high hydrothermal stability, and are widely used in the field of catalysis. Zeolite has a shorter intracrystalline diffusion channel length and a larger outer surface, which is conducive to increasing the contact opportunity between the reactant and the active site in the micropore, thereby improving the performance of the zeolite, and showing unique advantages in the reaction , such as unique macromolecular selectivity, higher catalytic activity and longer catalyst life. However, the size of zeolite is too small, which is not very convenient in practical application. It has disadvantages such as difficult recovery, easy deactivation and aggregation. Binders need to be added during the molding process. As a result, the effective surface area is reduced ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/36
Inventor 王德举刘仲能李学礼李则俊
Owner CHINA PETROLEUM & CHEM CORP
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