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Method for preparing beta zeolite with multilevel pore canals

A beta zeolite and channel technology, which is applied in the field of preparation of multi-level channel beta zeolite, can solve problems such as unsuitable catalytic materials, and achieve the effects of enriching internal specific surface area, easy selectivity and huge application value

Active Publication Date: 2007-07-25
CHINA PETROLEUM & CHEM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, considering that the pore wall of this material is in an amorphous state, it is not suitable as a catalytic material itself.

Method used

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  • Method for preparing beta zeolite with multilevel pore canals
  • Method for preparing beta zeolite with multilevel pore canals
  • Method for preparing beta zeolite with multilevel pore canals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Stir 30ml of methyl orthosilicate, 6g of polyethylene glycol and 30ml of 0.01mol / L acetic acid solution evenly, seal it, and stir at 0°C for 50min. The obtained sol was poured into a polytetrafluoroethylene test tube or a glass tube, and aged in a water bath at 30°C for one day to obtain a wet silica gel column. Then soak the silica gel column with 0.01mol / L ammonia water to prepare mesopores. Then soak the column with 0.1mol / L nitric acid solution, distilled water, 30% ethanol / water ethanol solution and Tween 80 for 6 hours, finally dry and roast to obtain the silica gel monolithic column B 1 .

Embodiment 2

[0036] According to the mass ratio of 1.25 sucrose: 0.14H 2 SO 4 : 5 water to make a solution, put the silica gel monolithic column B1 into it and soak for 30 minutes, then dry at 100°C for 6 hours, 160°C for 6 hours, repeat the process of soaking, drying, and polymerization once, and then carbonize at 900°C for 4 hours to obtain carbon Silicon composite sample C1.

Embodiment 3

[0038] Raw materials: 0.031 g of sodium aluminate, 0.055 g of sodium hydroxide, 1.85 g of tetraethylammonium hydroxide solution, and 0.65 g of carbon-silicon complex.

[0039] Experimental process: Mix and stir sodium aluminate, sodium hydroxide, and tetraethylammonium hydroxide solution evenly, then pour this solution into a reaction kettle equipped with C1, stir to make it fully wet, seal the reaction kettle and place in Crystallization at 150°C for 48 hours. Cool after crystallization, filter and wash, then put into an oven and dry at 100-110°C for 3-4 hours, and then burn the resultant in a muffle furnace at 600°C for 5 hours to obtain the product multi-stage channel zeolite beta sample , denoted as A1.

[0040] The XRD spectrum of sample A1 is shown in Figure 2. It can be seen from the figure that there are three peaks at 2θ angles of 7.7°, 21.5°, and 22.4°, and these three peaks are characteristic peaks of zeolite beta, indicating that the preparation The crystal form ...

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Abstract

This invention discloses a method for preparing multi-level porous beta-zeolite. The method comprises: soaking monolithic silica gel column in sucrose solution, drying, polymerizing, carbonizing to obtain C-Si composite, wetting the C-Si composite with a mixed solution of Al source, inorganic alkali, organic amine and water, crystallizing, and recovering the product. In this method, carbon material can effectively protect the porous structure of monolithic silica gel column from damage during crystallization process. The obtained beta-zeolite has multi-level pores, including micrometer-scale macropores, mesopores and micropores. The macropores can shorten the diffusion distances of reactive molecules, reduce the pressure decrease of the equipment, raise the unit processing capacity of the equipment, and make the adjustment and control of the product selectivity easier. The mesopores can provide large inner specific surface area, which is meaningful to the catalytic reaction of macromolecules.

Description

technical field [0001] The present invention relates to a method for synthesizing zeolite, and more particularly relates to a method for preparing multi-stage channel beta zeolite. Background technique [0002] According to the pore size of molecular sieves, the International Union of Pure and Applied Chemistry defines them into three categories: those with a pore size less than 2nm are called microporous molecular sieves, those with a pore size between 2 and 50nm are called mesoporous or mesoporous molecular sieves, and those with a pore size larger than 50nm called macroporous molecular sieves. [0003] Due to the specific selectivity of crystalline microporous molecular sieves to the size and shape of guest molecules, they have been widely used in the fields of catalysis, separation and purification. Although studies have shown that microporous zeolites have many potential chemical functions, their relatively narrow and long channels not only limit the diffusion of react...

Claims

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Application Information

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IPC IPC(8): C01B39/02B01J29/06
Inventor 赵天波童扬传宗保宁沈楠雷骞
Owner CHINA PETROLEUM & CHEM CORP
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