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Method for preparing beta zeolite in small crystal grain

A technology of beta zeolite and small crystal grains is applied in the field of preparing small crystal beta zeolite, which can solve the problems of large amount of template agent and low molecular sieve yield, and achieves low amount of template agent, high single-pot yield and low synthesis cost. Effect

Active Publication Date: 2008-04-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is that in the prior art, due to the large amount of water used in the raw material mixture, the amount of template agent used is large and the yield of molecular sieve is low. A new method for preparing small-grain beta zeolite is provided.

Method used

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  • Method for preparing beta zeolite in small crystal grain

Examples

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Comparison scheme
Effect test

preparation example Construction

[0022] Preparation of zeolite beta reference

[0023] A beta zeolite reference was synthesized following the method disclosed in the examples in US3308069.

[0024] In 26.2 grams of 25% by weight TEAOH (commercially available), add 1.05 grams of sodium aluminate (containing Al 2 o 3 43% by weight, containing Na 2 (239% weight, industrial product), then add 38.8 grams of silica sol (containing SiO 2 26% by weight, industrial product), stirring was continued for 1 hour. Transfer to a stainless steel reaction kettle, crystallize at 150°C for 3 days, take it out and cool, filter, wash, and dry at 140°C to obtain zeolite beta.

[0025] The molar ratio of feeding each component is:

[0026] 1Al 2 o 3 ·38SiO2 2 5 (TEA) 2 O·1.5Na 2 O·532H 2 o

[0027] Taking this sample as a reference sample, the crystallinity measured by XRD is taken as 100%. The crystallinity of the examples of the present invention and the comparative samples are compared with the reference sample by ...

Embodiment 1～3

[0048] According to the method provided by the invention to synthesize nano-sized zeolite beta

[0049] Raw material is

[0050] (A), silica sol: containing SiO 2 40% by weight, industrial product.

[0051] (B), sodium aluminate: containing Al 2 o 3 43% by weight, a commercially available product.

[0052] (C), tetraethylammonium hydroxide: content 35% by weight, industrial product.

[0053] Take 42.1 grams of tetraethylammonium hydroxide solution, add 2.372 grams of sodium aluminate and 75 grams of silica sol under stirring, stir evenly, transfer to a stainless steel reaction kettle, and carry out crystallization reaction according to a certain heating program. The crystallization temperatures are 120, 100, and 80°C, respectively. Suction filtration, washing, and drying are carried out after crystallization. X-ray diffraction analysis shows that the product is pure zeolite beta. The chemical composition is analyzed by chemical analysis method, and the grain size is ob...

Embodiment 1

[0057] The XRD diffraction results of the zeolite beta prepared in Example 1 are shown in Table 2.

[0058] Table 2

[0059] 2θ

[0060] By adopting the method of the invention, the synthesized zeolite does not contain miscellaneous crystals.

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Abstract

This invention relates to a method for preparing beta-zeolite with fine grains. The method comprises: (1) adopting silica sol with high SiO2 content as the Si source, sodium aluminate as the Al source, and tetraethyl ammonium cations as the templating agent; (2) performing hydrothermal crystallization at 80-160 deg.C for 1-8 days to obtain beta-zeolite with fine grains. The method solves the problems of low yield of molecular sieve and large amount of templating agent consumption caused by large amount of water consumption, and can be used in industrial manufacture of beta-zeolite.

Description

technical field [0001] The present invention relates to a method for preparing small-crystal beta zeolite. Background technique [0002] Ultrafine particles usually refer to tiny solid particles with a size less than a few hundred nanometers. They are a type of mesoscopic substance between atomic clusters and macroscopic objects. Decrease and increase sharply, showing obvious volume effect, surface effect and quantum size effect, so that ultrafine particles become new materials with unique physical and chemical properties. As the grain size of molecular sieves decreases, the proportion of surface atoms, the specific surface area and surface energy of grains increase rapidly. The specific surface is large, the number of surface atoms is large, that is, there are many surface active centers, and the catalytic efficiency is high, which is beneficial to eliminate the diffusion effect, and the orifice is not easy to be blocked. In some specific catalytic reactions, nano-sized m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 谢在库祁晓岚孔德金朱志荣左煜
Owner CHINA PETROLEUM & CHEM CORP