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Preparation method for Beta zeolite molecular sieve with enriched chiral polymorph A

A beta zeolite and molecular sieve technology is applied in the field of preparation of chiral A-shaped enriched beta zeolite molecular sieves, which can solve the problems of slow crystallization rate and long crystallization period.

Active Publication Date: 2018-04-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the crystallization rate is slow and the crystallization period is long under acidic conditions

Method used

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  • Preparation method for Beta zeolite molecular sieve with enriched chiral polymorph A
  • Preparation method for Beta zeolite molecular sieve with enriched chiral polymorph A
  • Preparation method for Beta zeolite molecular sieve with enriched chiral polymorph A

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preparation example Construction

[0026] According to the present invention, a kind of preparation method of chiral A form enriched Beta zeolite molecular sieve is provided, wherein, the method comprises:

[0027] (1) mixing the silicon source, template agent tetraethylammonium hydroxide and water, and hydrolyzing the resulting mixed solution;

[0028] (2) making the hydrolyzed mixed solution into a gel and drying to obtain dry glue;

[0029] (3) mixing the dry glue, polyethylene glycol and fluorine source, and subjecting the resulting mixture to hydrothermal crystallization;

[0030] (4) The obtained hydrothermal crystallization product is subjected to solid-liquid separation, and the obtained solid phase is dried and optionally calcined.

[0031] The method of the present invention prepares the Beta zeolite molecular sieve with higher content of the A form by adding polyethylene glycol and a fluorine source to the prepared initial dry glue, and subjecting the obtained mixture to hydrothermal crystallization...

Embodiment 1

[0052] This example is used to illustrate the preparation of the chiral form A-enriched Beta zeolite molecular sieve of the present invention.

[0053] 4.50g tetraethyl ammonium hydroxide aqueous solution and 2.22g mass fraction 35% tetraethylammonium hydroxide aqueous solution and 4.5g distilled water are mixed in reaction container, container is sealed with parafilm and stirred for 5 hours, makes tetraethyl silicate Completely hydrolyzed.

[0054] Remove the sealing film, continue to stir the resulting mixture in the fume hood for 6 hours, volatilize the ethanol and water in the system to form a jelly, and transfer it to a freezer (material temperature 20°C, cold trap temperature -60°C) in a dryer Freeze-dried for 3 days, at this time the H of the system 2 O and SiO 2 The molar ratio is less than 1, and the dry glue quality is 2.15g.

[0055] Mix 2.15g of dry glue with 3.6g of PEG-400 and 0.2g of ammonium fluoride and grind it into a uniform powder (100 mesh), then transf...

Embodiment 2

[0059] This example is used to illustrate the preparation of the chiral form A-enriched Beta zeolite molecular sieve of the present invention.

[0060] 4.50g tetraethyl ammonium hydroxide solution and 2.23g mass fraction 35% tetraethylammonium hydroxide aqueous solution and 4.5g distilled water are mixed in reaction vessel, container is sealed with parafilm and stirred for 5 hours, and tetraethyl ammonium hydroxide Completely hydrolyzed.

[0061] Remove the parafilm, continue to stir the resulting mixture in a fume hood for 6 hours, volatilize the ethanol and water in the system to form a jelly, and transfer it to a freeze dryer (material temperature 20°C, cold trap temperature -60°C) Freeze-dried for 3 days, at this time the H of the system 2 O and SiO 2 The molar ratio is less than 1, and the dry glue mass is 2.14g.

[0062] Mix 2.14g of dry glue with 1.7g of PEG-2000 and 0.19g of ammonium fluoride and grind it into a uniform powder (100 mesh), then transfer it to a polyt...

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Abstract

The invention relates to the technical field of preparation of Beta zeolite molecular sieves, and discloses a preparation method for a Beta zeolite molecular sieve with enriched chiral polymorph A. The method comprises the following steps: (1) mixing a silicon source, template agent tetraethylammonium hydroxide and water, and performing hydrolysis on the obtained mixed liquid; (2) using the hydrolyzed mixed liquid to prepare a gel, and performing drying to obtain a dry glue; (3) mixing the dry glue, polyethylene glycol and a fluorine source, and performing hydrothermal crystallization on the obtained mixture; and (4) performing solid-liquid separation on the obtained hydrothermal crystallization product, performing drying on the obtained solid phase, and optionally performing roasting. Themethod provided by the invention can prepare the Beta zeolite molecular sieve with the content of the polymorph A of 70% or more.

Description

technical field [0001] The invention relates to the preparation technology of Beta zeolite molecular sieve, in particular to a preparation method of Beta zeolite molecular sieve enriched in chiral A form. Background technique [0002] In 1967, Wadlinger et al. of Mobil Corporation of the United States first developed a large-pore high-silica zeolite with a three-dimensional twelve-member pore structure, and named it Beta zeolite. Due to its special pore structure, Beta zeolite has both acid catalytic properties and structural selectivity, and is widely used in petroleum refining and petrochemical processes such as hydrocracking, isomerization, alkylation, and dewaxing. The structure of Beta zeolite was determined by Treacy, Newsam and Higgins in 1988, respectively. It consists of A-form (also known as polymorph A) and B-form (also known as polymorph B) in a ratio of 44:56. Form A has chirality, and there is a helical channel in the c-axis direction, while form B does not h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 闫文付鲁婷婷王永睿慕旭宏
Owner CHINA PETROLEUM & CHEM CORP