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Beta zeolite granule possessing multiple grade pore passage and its preparation method

A beta zeolite and pore technology, applied in the field of beta zeolite and its preparation, can solve the problems of difficult filtration, long time, low single-pot yield, etc., and achieve good product repeatability, short crystallization time, and high single-pot yield Effect

Active Publication Date: 2006-05-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a result, a large amount of the outer surface of the zeolite will inevitably be bonded to alumina, which makes it difficult to fully exert the effect on the small-grained zeolite characterized by a large outer area and externalization of the active center.
Therefore, no matter the zeolite in the prior art is large crystal grain or small crystal grain, when it is used as part of the catalyst component, it has certain deficiencies.
In addition, in the preparation method of zeolite beta in the prior art, the amount of template agent (tetraethylammonium hydroxide) is large, the solid-to-liquid ratio of the feed is low, the single-pot yield is low, the crystallization temperature is high, and the time is long, and miscellaneous crystals are prone to appear. Poor reproducibility of results, difficult filtration and low yield

Method used

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  • Beta zeolite granule possessing multiple grade pore passage and its preparation method
  • Beta zeolite granule possessing multiple grade pore passage and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] With 78g sodium aluminate (laboratory preparation contains Al 2 o 3 19.9m%, containing Na 2 O 21.44m%), 435g tetraethylammonium hydroxide aqueous solution (the product of industrial production, concentration 1.4N), coarse porous silica gel particle 288g (Qingdao ocean chemical plant production, containing SiO 2 95%) and 120g of purified water are mixed evenly, and reacted in a 2-liter stainless steel reactor at 100°C for 20 hours under sufficient continuous stirring conditions, and then raised to 150°C for crystallization for 40 hours. Ammonium solution, based on the ammonium nitrate concentration in the system being 2 mol / L, was stirred at 95°C for 1 hour and then filtered, and ammonium salt treatment was carried out again according to the above conditions. Then filter, wash with water, dry, remove organic ammonium by three-stage temperature-controlled roasting, dehydrate at a constant temperature of 200°C for 2 hours, decompose organic ammonium at 400°C for 3 hours,...

Embodiment 2

[0020] With 80g sodium aluminate (laboratory preparation contains Al 2 o 3 18.90m%, containing Na 2 O 24.11m%), 382g tetraethylammonium hydroxide aqueous solution (industrial product, concentration 1.55N), coarse porous silica gel particle 280g (Qingdao Ocean Chemical Factory produces SiO 2 95.2m%) and 158g of purified water are mixed evenly. Other conditions were the same as in Example 1 to obtain zeolite beta B-2.

Embodiment 3

[0022] With 80kg sodium aluminate (industrial preparation, containing Al 2 o 3 19.55m%, containing Na 2 O21.17m%), 459kg tetraethylammonium hydroxide (industrial product, concentration 1.35N) coarse-pore silica gel particles 288kg (Qingdao ocean chemical plant production, containing SiO 2 97m%) and 140kg of purified water, after fully mixing, under the continuous stirring condition in 1000 liters of stainless steel crystallization kettles, below with embodiment 1, obtain beta zeolite, B-3.

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Abstract

The invention relates to a beta zeolite particle with multistage openings, the mole ratio of SiO2 / Al2O3 being 80-120, the mean particle size being 0.1-0.5um, opening capacity being 0.35-0.50ml / g, and aperture collectively distributing at three-stage 0.1-1.7nm, 1.7-6.0nm and 10.0-90.0nm. In the beta zeolite preparing process, it uses optimization-condition hydrothermal synthesis method, after synthesis process, firstly proceeding ammonium salt processing procedure to prepare zeolite, then proper-conditioned acid treatment and hydrothermal treatment to prepare final beta zeolite. The prepared beta zeolite having three openings of different aperture, compared with the prior art, it can increase highly the utilization ratio of outer surface of fine grain, decrease diffusion resistance, and improve reaction selectivity. The invented process is simple, the cost is low, and the product repetitiveness is good. The beta zeolite can be used as catalyst for hydrocracking, and so on.

Description

technical field [0001] The invention relates to a beta zeolite and a preparation method thereof, in particular to a beta zeolite particle with a multi-level pore structure and a preparation method thereof. Background technique [0002] Beta zeolite is a high-silica zeolite (US3,308,069) with a three-dimensional pore structure successfully developed by Mobil Corporation of the United States in the 1960s. Catalytic performance, has broad application prospects in petroleum and chemical industry. Industrial application results show that β zeolite has high hydrocracking activity and hydroisomerization performance, and can be used for hydrocracking, hydroisomerization, hydrofinishing, hydrodewaxing, Diesel decondensation and other processes. [0003] The narrow pores inside the zeolite grains increase the diffusion resistance and reduce the reaction performance. After the crystal grains become smaller, the outer surface expands and the internal diffusion rate increases, which h...

Claims

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Application Information

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IPC IPC(8): C01B39/02C01B39/04
Inventor 张奎喜尹泽群阮彩安黄薇赵红谷明镝
Owner CHINA PETROLEUM & CHEM CORP
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