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Method for preparing beta zeolite through kaolin microsphere in-situ crystallization

A beta zeolite and kaolin microsphere technology, applied in the field of zeolite molecular sieve synthesis, can solve the problems of long usage of template agent, high cost, limited large-scale production, etc., and achieves a wide range of feeding materials, a simple preparation process, and good reproducibility. Effect

Inactive Publication Date: 2013-10-23
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Beta zeolite is a new type of zeolite material with excellent performance. Its high-cost template usage and long production cycle have limited its large-scale production. In the trend of using clay as all or part of the raw materials to synthesize molecular sieves, beta Zeolites have also been slow to develop due to cost concerns

Method used

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  • Method for preparing beta zeolite through kaolin microsphere in-situ crystallization
  • Method for preparing beta zeolite through kaolin microsphere in-situ crystallization
  • Method for preparing beta zeolite through kaolin microsphere in-situ crystallization

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Experimental program
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Effect test

Embodiment 1

[0024] Dissolve 0.43g NaOH in 15.84g tetraethylammonium hydroxide solution (25%), and stir evenly. Then slowly add 5.0 g of high soil microspheres with vigorous stirring, continue stirring for 1 h after the addition, and then perform the second feeding, slowly add 4.09 g of coarse-pore silica gel under vigorous stirring, and continue stirring for 2 h. The whole reaction process was carried out in a water bath at 65°C, and the system was sealed to prevent moisture from evaporating. After thorough stirring, the mixture was transferred into a self-pressurized stainless steel reactor with a polytetrafluoroethylene liner, and crystallized at 140°C for 48h. After the reaction, the solid product was isolated, washed with deionized water until neutral, dried overnight at 120°C, and roasted at 550°C to obtain a sodium beta zeolite product.

[0025] The molar ratio of raw materials in the reaction system is: SiO 2 / Al 2 o 3 =60,Na 2 O / SiO 2 = 0.057, TEA + / SiO 2 =0.3,H 2 O / SiO ...

Embodiment 2

[0027] Dissolve 0.36 g of NaOH in 13.24 g of tetraethylammonium hydroxide solution (25%), and stir the solution evenly under magnetic stirring. Then slowly add 5.0 g of high soil microspheres with vigorous stirring, continue stirring for 1 h after the addition, and then perform the second feeding, slowly add 3.19 g of coarse-pore silica gel under vigorous stirring, and continue stirring for 2 h. The whole reaction process was carried out in a water bath at 65°C, and the system was sealed to prevent moisture from evaporating. After thorough stirring, the mixture was transferred into a self-pressurized stainless steel reactor with a polytetrafluoroethylene liner, and crystallized at 140°C for 48h. After the reaction, the solid product was isolated, washed with deionized water until neutral, dried overnight at 120°C, and roasted at 550°C to obtain a sodium beta zeolite product.

[0028] The molar ratio of raw materials in the reaction system is: SiO 2 / Al 2 O3=50,Na 2 O / SiO ...

Embodiment 3

[0030] Dissolve 0.28g of NaOH in 10.59g of tetraethylammonium hydroxide solution (25%), and stir the solution evenly under magnetic stirring. Then slowly add 5.0 g of high soil microspheres with vigorous stirring, continue stirring for 1 h after the addition, and then perform the second feeding, slowly add 2.29 g of coarse-pore silica gel under vigorous stirring, and continue stirring for 2 h. The whole reaction process was carried out in a water bath at 65°C, and the system was sealed to prevent moisture from evaporating. After thorough stirring, the mixture was transferred into a self-pressurized stainless steel reactor with a polytetrafluoroethylene liner, and crystallized at 140°C for 48h. After the reaction, the solid product was isolated, washed with deionized water until neutral, dried overnight at 120°C, and roasted at 550°C to obtain a sodium beta zeolite product.

[0031] The molar ratio of raw materials in the reaction system is: SiO 2 / Al 2 o 3 =40,Na 2 O / SiO ...

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Abstract

The invention relates to a method for preparing beta zeolite by taking kaolin microsphere as a raw material. The method comprises the following steps of: taking the roasted kaolin microsphere as a main silicon aluminium source; adding a part of coarse pore silica gel as a supplement silicon source; adding to an aqueous solution with a sodium source and a tetraethylammonium cation source to mix uniformly; and crystallizing at 120-180 DEG C for 24-60 h. The reaction system comprises the following compositions according to mol ratio: SiO2 / Al2O3 is 5-100; and Na2O / SiO2 is 0.029-0.31. According tothe method disclosed by the invention, on the premise of not damaging the external form of the kaolin microsphere, the roasted kaolin microsphere is adopted as the silicon aluminium source to performin-situ crystallization so that the beta zeolite is synthesized; the reaction is carried out under an ultra-thick system; the crystallization time is short; the product concentration is high; and theobtained beta zeolite can be directly used for FCC (Fluid Catalytic Cracking) reaction by slight modifying.

Description

[0001] Involved areas [0002] The invention relates to a method for preparing beta zeolite by in-situ crystallization of kaolin microspheres, and belongs to the technical field of zeolite molecular sieve synthesis. The raw material mainly involved in the synthesis of beta zeolite is kaolin microspheres, and beta zeolite products with relatively high crystallinity are obtained on the basis of its in-situ crystallization. Background technique [0003] Beta zeolite is the only zeolite with a three-dimensional twelve-membered ring straight channel system among high silica zeolites, and it is the only zeolite with a chiral pore network structure with mesopore diameter. Since 1967, Wadlinger of the Mobil Petroleum Company of the United States reported the synthesis of beta zeolite for the first time. Since (US3308069), beta zeolite has a very important application prospect in the petrochemical field because of its unique properties in many aspects. Its main catalytic reactions inc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/06C01B39/52
Inventor 郭士岭陈宜俍禹子洋徐军卫冬燕韩丽李晓旭
Owner ZHENGZHOU UNIV