Method for synthesizing granular beta molecular sieve with montmorillonoid

A technology of beta molecular sieve and montmorillonite, which is applied in the field of high-yield synthesis of small particle beta molecular sieves, can solve the problems of synthesizing beta molecular sieves and synthesizing beta molecular sieves without natural mineral raw materials, and achieves the improvement of single-pot yield and reduction of raw materials. cost effect

Inactive Publication Date: 2010-06-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on the synthesis of β molecular sieves using natural mineral raw materials, and there is no report on the synthesis of β molecular sieves using montmorillonite as a raw material.

Method used

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  • Method for synthesizing granular beta molecular sieve with montmorillonoid
  • Method for synthesizing granular beta molecular sieve with montmorillonoid
  • Method for synthesizing granular beta molecular sieve with montmorillonoid

Examples

Experimental program
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Effect test

Embodiment 1

[0054] Using commercially available montmorillonite (Beipiao Yongsheng Bentonite Co., Ltd.) as raw material, take 45 g of the purified montmorillonite, and mix the montmorillonite with HNO 3 、CH 3 COOH and H 4 Mixed acid solution composed of EDTA (HNO in acid solution 3 、CH 3 COOH and H 4 The mass fractions of EDTA are 10%, 10% and 5% respectively) soaked in 60°C for 3h, washed, dried, pulverized to 10μm, and roasted at 800°C in a muffle furnace at a heating rate of 4°C / min for 4h to obtain activated Montmorillonite.

Embodiment 2

[0056] Using commercially available montmorillonite (Beipiao Yongsheng Bentonite Co., Ltd.) as raw material, take 45 g of the purified montmorillonite, and mix the montmorillonite with HNO 3 、CH 3 COOH and H 4 Mixed acid solution composed of EDTA (HNO in acid solution 3 、CH 3 COOH and H 4 The mass fractions of EDTA are 15%, 5% and 5% respectively) soaked in 60°C for 3h, washed, dried, pulverized to 10μm, and roasted at 850°C in a muffle furnace at a heating rate of 4°C / min for 2h to obtain activated Montmorillonite.

Embodiment 3

[0058] Soak 45 g of activated montmorillonite in Example 1 with 70 mL of tetraethylammonium hydroxide with a concentration of 25 wt % at 50° C. for 6 h. After that, 2g of sodium hydroxide, 0.5g of sodium chloride, 1.44g of potassium chloride, 40mL of distilled water, 40mL of tetraethylammonium hydroxide with a concentration of 25wt%, and 30g of white carbon black were put into a beaker and stirred at 80°C for 3h. into a gel mixture. The gel was transferred to a stainless steel reactor for static crystallization at 140°C for 48 hours. After the crystallization is completed, cool, filter to remove the mother liquor, wash and dry the filter cake to obtain a crystallized product. According to X-ray measurement, its phase belongs to beta molecular sieve, the relative crystallinity of beta molecular sieve in the product is 80%, and the crystal grain of molecular sieve reaches 80-120nm. The single-pot yield reaches more than 70wt%.

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Abstract

The invention relates to a method for synthesizing a granular beta molecular sieve with montmorillonoid, comprising the following steps: acidification treatment and high-temperature roasting are carried out to the montmorillonoid, and the montmorillonoid which is acidified is soaked and heated by template agents, and then the montmorillonoid which is activated is used as raw material to provide total or partial aluminum source, and then the granular beta molecular sieve is prepared by adding template agents and carrying out hydrothermal crystallization; in the invention, the prepared beta molecular sieve grows on the surface of the montmorillonoid closely, so as to form a similar core-shell structure, and the catalytic reaction efficiency is improved by shortening the diffused route of reactants and product molecules in a molecular sieve crystal. The method not only expands the raw material range for synthesizing the beta molecular sieve, but also further reduces the preparation cost of the beta molecular sieve with a crystal seed method.

Description

field of invention [0001] The invention belongs to molecular sieve and its preparation technology. Specifically, it relates to a method for synthesizing small-particle β molecular sieves with high yield by using natural mineral montmorillonite to provide all or part of the aluminum source and part of the silicon source required for the synthesis of β molecular sieves. Background technique [0002] β molecular sieve was first synthesized in 1967 by Wadlinger et al. of Mobil Corporation of the United States by the classic hydrothermal crystallization method (US3308069). Since the silicon source used is silica sol, which has a large water content, the dosage of template agent is relatively large, resulting in high production cost of β molecular sieve. At the same time, due to the large volume of the entire reaction solution and the long crystallization time, problems such as low production efficiency are brought about, which are unfavorable for large-scale industrial productio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 凌凤香张志智张喜文孙万付秦波
Owner CHINA PETROLEUM & CHEM CORP
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