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Hierarchical-porous zeolite preparation method

A pore zeolite and multi-level pore technology is applied in the field of preparing multi-level pore zeolite to achieve the effects of reducing the dosage, avoiding the problem of phase separation and reducing the reaction cost.

Inactive Publication Date: 2016-06-22
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method with universality, simple and extensive sources of raw materials, stable reaction process, and easy operation, to prepare hierarchically porous zeolite materials simply, safely and efficiently; A large amount of expensive zeolite crystallizers can be used to prepare porous and zeolite defects that meet the requirements

Method used

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Examples

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Effect test

Embodiment 1

[0026] Add sodium aluminate (0.15 g), sodium hydroxide (0.54 g), CTAB (3.64 g), tetraethyl orthosilicate (17.2 ml), and deionized water (92.3 ml) in the reaction flask in sequence, at 40 °C React for 30 minutes, add 10ml MFI zeolite seed solution (TBAOH and SiO 2The molar ratio is 0.05), add in 20 minutes, and then continue to stir for 2 hours. After the reaction is completed, cool to room temperature, filter and separate the solid, and dry at 55°C. The proportion of dry powder, at 170 ℃, alkali steam treatment for 24 hours, the alkali solution is the aqueous solution of ethylenediamine (6ml ethylenediamine dissolved in 15ml water). The obtained product is washed with water, dried, and calcined at 550° C. to obtain a hierarchically porous zeolite. The molar ratio of the silicon-aluminum element of the final product obtained is Si / Al=43. The product was analyzed and characterized through pore structure, figure 1 N for the above-mentioned hierarchical pore zeolite 2 Adsorptio...

Embodiment 2

[0028] Add aluminum sulfate (0.15 g), sodium hydroxide (0.7 g), CTAB (3.64 g), white carbon black (4.6 g), and deionized water (92.3 ml) to the reaction flask in sequence, and react at 40°C for 30 minutes , add 10ml MFI zeolite seed solution (TPAOH and SiO 2 The molar ratio is 0.15), the addition was completed in 30 minutes, and then continued to stir for 2 hours. After the reaction was completed, cool to room temperature, filter and separate the solid, and dry at 55°C. The dry powder and the alkali solution corresponded to 1 The proportion of dry powder in grams, at 140 ° C, alkali steam treatment for 48 hours, the lye is an aqueous solution of ethylenediamine / triethylamine (50ml ethylenediamine, 23ml triethylamine dissolved in 10ml water). The obtained product was washed with water, dried, and calcined at 550°C to obtain a hierarchically porous zeolite. The molar ratio of the silicon-aluminum element of the obtained product is Si / Al=85; the product is analyzed and character...

Embodiment 3

[0030] Add sodium aluminate (0.15 g), sodium hydroxide (0.7 g), P123 (2 g), tetraethyl orthosilicate (18 ml), and deionized water (92.3 ml) to the reaction flask in sequence, at 40 °C React for 30 minutes, add 10ml MFI zeolite seed solution (TBAOH and SiO 2 The molar ratio is 0.2), add in 50 minutes, and then continue to stir for 2 hours. After the reaction is completed, cool to room temperature, filter and separate the solid, and dry at 55°C. The dry powder and alkali solution correspond to 1.2ml of alkali solution The proportion of dry powder in grams, at 170°C, alkali steam treatment for 24 hours, the alkali steam is tetrabutylammonium hydroxide / ammonia mixed aqueous solution (1ml tetrabutylammonium hydroxide aqueous solution (10wt.%), 2ml concentrated ammonia solution in 10ml water). The obtained product was washed with water, dried, and calcined at 550°C to obtain a hierarchically porous zeolite. The molar ratio of silicon to aluminum in the product is Si / Al=88. The pro...

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Abstract

The invention discloses a hierarchical-porous zeolite preparation method.A hierarchical-porous zeolite material is prepared according to alkali vapor thermal treatment method by taking various alkali vapors as mineralizing agents for zeolitization and taking amorphous mesoporous / macroporous materials as precursors.The applicable amorphous mesoporous / macroporous materials serving as the precursors relate to amorphous porous inorganic precursors of various mesoporous / macroporous molecular sieves, and the applicable hierarchical-porous zeolites relate to MFI zeolite, beta zeolite, Y zeolite and silicatite-1 zeolite.The hierarchical-porous zeolite preparation method is a first embodiment of hierarchical-porous zeolite preparation according to the alkali metal vapor thermal treatment method and is equivalent or higher in HF and wider in zeolite preparation applicability as compared with the prior art.

Description

technical field [0001] The invention belongs to the technical field of preparation of zeolite, and in particular relates to a preparation method of multi-level pore zeolite. Background technique [0002] Zeolite is a crystalline microporous aluminosilicate with large specific surface area, high hydrothermal stability, good ion exchange performance and rich and adjustable surface physicochemical properties. Hierarchical zeolite materials not only have the advantages of microporous zeolite molecular sieves (strong hydrothermal stability and acidity), but also have the characteristics of mesoporous molecular sieves (good diffusivity), making them widely used in adsorption, separation, catalysis and other fields. Value. Therefore, the synthesis of hierarchically porous zeolites has received more and more attention. The synthesis of such materials can traditionally be prepared by acid-base treatment (de-siliconization or dealumination), or co-synthesis by dual-template mesoporo...

Claims

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Application Information

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IPC IPC(8): C01B39/02
CPCC01B39/02C01P2006/14
Inventor 李华肖佳佳
Owner SUZHOU UNIV
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