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Preparation of zeolite binderless ZSM-5

A binder-free, ZSM-5 technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of easy deactivation, diffusion limitation, and difficult recovery of zeolite powder and other problems, to achieve the effect of high mechanical strength and good technical effect

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

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to solve the disadvantages of difficult recovery, easy deactivation and aggregation of zeolite powder in practical application in the prior art, and the addition of binder in the molding process will cause effective surface area reduction and diffusion limitation. problem, provide a new method for preparing binder-free ZSM-5 zeolite

Method used

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  • Preparation of zeolite binderless ZSM-5
  • Preparation of zeolite binderless ZSM-5
  • Preparation of zeolite binderless ZSM-5

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～3

[0016] Take by weighing 200 grams of white carbon black, 80 grams of HZSM-5 zeolite ((SiO 2 / Al 2 o 3 The molar ratio is 120, the grain size is about 800 nanometers), 45 grams of silicon-containing alumina powder (containing SiO 2 The mass percentage is 26%) and 15 grams of NaOH, then add 580 grams of silica sol (40% by weight), and add an appropriate amount of water for kneading and extruding into a cylindrical shape.

[0017] A mixture of 12 grams of ethylenediamine and 3 grams of distilled water was added to the reaction kettle in advance, and 40 of the above-mentioned cylindrical precursors were placed in the reaction kettle above the porous stainless steel mesh and sealed at 160°C for 3 days, 5 days and 7 days. After the product was taken out, it was washed with distilled water, dried and calcined at 550°C for 4h in an air atmosphere. The XRD pattern shows that the products are all ZSM-5 zeolites, and the straight baseline of the XRD pattern shows that the raw material...

Embodiment 4～6

[0019] The cylindrical precursor prepared above [Examples 1-3] was calcined in an air atmosphere at 550°C for 4 hours, and 40 grams and 80 grams of NaOH containing 1.66% by mass and 11.05% by mass of tetrapropyl bromide were taken respectively. Solutions of ammonium (TPABr) were subjected to hydrothermal treatment at 160 °C for 3 days, 5 days and 7 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-5 zeolite, the baseline is flat, indicating that there is basically no amorphous substance, and the BET specific surfaces are 334.8, 344.6 and 355.0 square meters per gram. The sample treated for 5 days showed the agglomeration of small ZSM-5 zeolite crystals of about 100 nanometers into spherical particles of about 2 microns, which were interlaced and grown together.

Embodiment 7～10

[0021] Take by weighing 200 grams of white carbon black, 80 grams of NaZSM-5 zeolite ((SiO 2 / Al 2 o 3 The molar ratio is 60, the grain size is about 300 nanometers) and 26 grams of sodium aluminate (containing Al 2 o 3 The mass percentage is 43%) 15 grams of NaOH, then add 410 grams of silica sol (40% by weight), and add an appropriate amount of water for kneading and extruding into a cylindrical shape.

[0022] A mixture of 7 grams of ethylamine, 7 grams of ethylenediamine and 10.5 grams of distilled water was added to the reaction kettle in advance, and 50 grams of the cylindrical product prepared above was placed in the reaction kettle and sealed above the porous stainless steel mesh, and then the gas-solid phase was carried out at 180 ° C. 2 days, 3 days, 5 days, 7 days of treatment. After the product was taken out, it was washed with distilled water, dried in the air and then calcined at 550°C in an air atmosphere. XRD patterns show that the products are all ZSM-5 z...

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Abstract

The invention relates to a method for preparing no-binding agent ZSM-5 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, the ZSM-5 zeolite crystal seeds are added or not, the materials are formed to obtain a precursor mixture with the mass ratio of XNa2O:YAl2O3:100SiO2, wherein x is between 0 and 16, and y is between 0 and 6, and the precursor mixture is subjected to hydrothermal crystallization in a water solution containing tetrabutyl ammonium positive ions or a water solution of organic amine, or subjected to gas-solid phase crystallization in the mixed vapors of organic amine and water and converted to the no-binding agent ZSM-11 forming zeolite. The technical proposal of the invention better resolves the problems, and can be applied to the industrial preparation of the ZSM-5 zeolite molecular sieve catalyst.

Description

technical field [0001] The invention relates to a method for preparing binder-free ZSM-5 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. Small-grain zeolite has a shorter intracrystalline diffusion channel length and a larger outer surface, which is beneficial to increase the contact opportunity between the reactants and the active sites in the micropores, thereby improving the performance of the zeolite. Unique advantages, such as unique macromolecular selectivity, high catalytic activity and long catalyst life, etc. 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 and diffusion re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38
Inventor 王德举刘仲能李学礼吴征
Owner CHINA PETROLEUM & CHEM CORP
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