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Method for preparing multi-level porous channel beta zeolite

A beta zeolite and pore channel technology, which is applied in the field of beta zeolite preparation, can solve the problems of chained active site destruction, uneven crystal size, and wide distribution of mesopore size of titanium silicalite, and achieves the effect of reducing processes and saving raw materials.

Inactive Publication Date: 2009-09-23
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The emergence of secondary pores promotes molecular diffusion, but the problem is the destruction of the crystal structure and supercages and the partial destruction of linked active sites, and the distribution of secondary pores is also random and disordered
Schmidt et al. used mesoporous carbon black to prepare titanium silicalite (TS-1), which improved the catalytic performance of titanium silicalite in ethylene epoxidation reaction (Chem.Commun, 2000, 2157-2158), but obtained titanium silicalite The mesopore size distribution of zeolite is wide and difficult to control, and the crystal size is also very uneven

Method used

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  • Method for preparing multi-level porous channel beta zeolite
  • Method for preparing multi-level porous channel beta zeolite
  • Method for preparing multi-level porous channel beta zeolite

Examples

Experimental program
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Effect test

Embodiment approach 1

[0035] Take 7.5g MCM-41 (SiO 2 / Al 2 o 3 =25), add phenol and formaldehyde (phenol to formaldehyde molar ratio is 8) by equal volume impregnation method, polymerize 8h in oven at 125 DEG C, the obtained phenolic resin polymer is carbonized under the protection of nitrogen, and the carbonization program is heating rate 2 DEG C / Min was raised from room temperature to 700°C, and then cooled naturally to room temperature at a constant temperature for 5 hours. The resultant was a composite of mesoporous and carbon materials. Take 2 g of the compound and place it in a crucible, add 3.0 g (wt.48%) of tetraethylammonium hydroxide solution, and place it at room temperature for 10 h, then put the crucible into a reaction kettle filled with 5 ml of water, and place it at 170 After crystallization at ℃ for 3 days, the resulting solid was washed with water, filtered, dried at 100 ℃, and calcined at 550 ℃ for 8 hours to obtain a white multi-stage zeolite beta powder, which was designated...

Embodiment approach 2

[0037] Take 7.5g MCM-41 (SiO 2 / Al 2 o 3 =50), add sucrose solution (2.5g sucrose: 0.28g concentrated sulfuric acid: 6.0g water) by equal volume impregnation method, polymerize in oven at 125°C for 8h, the gained polymer is carbonized under nitrogen protection, and the carbonization program is heating rate 2 ℃ / min increased from room temperature to 700 °C, and then cooled naturally to room temperature at a constant temperature for 5 hours. The resultant was a composite of mesoporous and carbon materials. Get this compound 2g and place in the crucible, add 0.096g sodium metaaluminate (wt.41%), 0.68g tetraethylammonium bromide and 2.0g (wt.48%) tetraethylammonium hydroxide Solution, after standing at room temperature for 10 hours, put the crucible into a reaction kettle containing 3ml of water, crystallize at 170°C for 3 days, wash the obtained solid with water, filter, dry at 100°C, and roast at 550°C for 8 hours to obtain a white multi-level channel β Zeolite powder, the pr...

Embodiment approach 3

[0039] Take 6.5g MCM-48 (SiO 2 / Al 2 o 3 =30), add phenol and formaldehyde (phenol to formaldehyde molar ratio is 8) by equal volume impregnation method, polymerize 8h in oven at 125 DEG C, the obtained phenolic resin polymer is carbonized under the protection of nitrogen, and the carbonization program is heating rate 2 DEG C / Min was raised from room temperature to 700°C, and then cooled naturally to room temperature at a constant temperature for 5 hours. The resultant was a composite of mesoporous and carbon materials. Get 2g of the compound and place it in a crucible, add 2.5g (wt.48%) of tetraethylammonium hydroxide solution, leave it at room temperature for 10h, then put the crucible into a reaction kettle filled with 5ml of water, After crystallization at 170°C for 4 days, the resulting solid was washed with water, filtered, dried at 100°C, and calcined at 550°C for 8 hours to obtain a white multi-stage zeolite beta powder, which was designated as M48B-1.

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Abstract

The invention provides a method for preparing multi-level porous channel beta zeolite, and belongs to the technical field of preparation and application of the zeolite. The method is characterized in that: carbon grains which are generated under restriction of the sequent meso-porous channels are taken as a hard mold board, and added with a small molecular organic ammonium soft mold board to convert the meso-porous silicon-aluminum coating the carbon grain into the meso-porous beta zeolite in situ, and the meso-porous beta zeolite is calcined to remove the soft and hard mold boards so as to obtain the multi-level porous channel containing beta zeolite. Compared with the zeolite obtained by directly taking the meso-porous carbon as the mold board, the multi-level porous channel beta zeolite synthesized by the method does not need to remove the meso-porous silicon-aluminum first and then introduce the silicon-aluminum species synthesizing the zeolite, thereby reducing complicated working procedures as well as saving raw materials. The method has the advantages of greatly lowering diffusional resistance, reducing secondary reaction, and having better catalytic property and huge potential application values in fields such as petrochemical industry, fine chemical industry, and the like.

Description

technical field [0001] The invention discloses a preparation method of multi-stage channel beta zeolite, which belongs to the fields of catalytic cracking, catalytic cracking, hydrocracking and fine chemical industry, and specifically relates to a preparation method of multi-stage channel beta zeolite. Background technique [0002] Fluid catalytic cracking (FCC) is one of the most important processes in the oil refining industry. The simple catalyst formulation currently used in this process is difficult to meet the increasing requirements of commercial and environmental protection. A key factor to improve the conversion depth of heavy oil catalytic cracking and the yield of light oil is that the catalyst should have a suitable pore distribution and acidity distribution. , the catalytic material is required to provide heavy oil molecules with a "relay" catalytic cracking pore structure from large to small. Therefore, researching and synthesizing molecular sieve materials wi...

Claims

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Application Information

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IPC IPC(8): C01B39/00
Inventor 李玉平窦涛李晓峰周升张卿杨冬花
Owner TAIYUAN UNIV OF TECH
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