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Preparation method of mesopore molecular sieve containing beta zeolite secondary structural unit

A secondary structural unit, mesoporous molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of high price of organic templates, narrow range of silicon-aluminum ratio, and complicated synthesis process, so as to save the synthesis process and save energy. The effect of large adjustment range, acidity and acidity improvement

Active Publication Date: 2013-01-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although they have improved the acidity and stability of MCM-41 molecular sieves to a certain extent, the synthesis process is relatively complicated and must undergo the synthesis of precursors.
Especially in the synthesis of Beta zeolite secondary structural units, there are many problems such as high price and large dosage of organic templates, narrow range of silicon-aluminum ratio, long crystallization time, etc.

Method used

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  • Preparation method of mesopore molecular sieve containing beta zeolite secondary structural unit
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  • Preparation method of mesopore molecular sieve containing beta zeolite secondary structural unit

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Embodiment 1

[0030] Industrially synthesized NaBeta(SiO 2 / Al 2 o 3 Molecular molar ratio is 25, the following are all SiO 2 / Al 2 o 3 Both are molecular molar ratios) 5.2g of zeolite is dispersed in 200mL 4M HCl solution to form a hydrogel. After stirring at room temperature for 1h, put it into a synthesis kettle, place it at 120°C for 6h, and adjust the pH value to 13 with 6M NaOH after cooling. About; then drop 12.5g of 16wt% cetyltrimethylammonium chloride solution into the hydrogel, stir at 50°C for 40min, and adjust the pH to about 10 with hydrochloric acid; stir evenly and put the material into the lining polytetrafluoroethylene crystallized at 110°C for 4 days; then filtered, washed, and dried at 100°C for 24 hours; and then calcined at 550°C for 8 hours in an air atmosphere to obtain the desired product. The molecular sieve sample whose crystal phase is MCM-41 was obtained by XRD analysis. According to infrared spectrum (IR) analysis, the framework of the MCM-41 product cont...

Embodiment 2

[0032] Industrially synthesized NaBeta(SiO 2 / Al 2 o 3 Molecular molar ratio is 25, the following are all SiO 2 / Al 2 o 3 Both are molecular molar ratio) Zeolite 5.2g is dispersed in 200mL 4M H 2 SO 4In the solution, a hydrogel is formed. After stirring at room temperature for 1 hour, put it into a synthesis kettle, place it at 100°C for 12 hours, and adjust the pH value to about 13 with 6M NaOH after cooling; Drop ammonium chloride solution into the hydrogel, stir at 50°C for 40 minutes, then add 7g of tetraethyl orthosilicate, and hydrochloric acid to adjust the pH to about 10; Crystallize at 130°C for 3 days; then filter, wash, and dry at 100°C for 24 hours; then bake at 550°C for 8 hours in an air atmosphere to obtain the desired product. The molecular sieve sample whose crystal phase is MCM-41 was obtained by XRD analysis. According to infrared spectrum (IR) analysis, the framework of the MCM-41 product contains Beta zeolite secondary structural units.

Embodiment 3

[0034] Industrially synthesized NaBeta zeolite, SiO 2 / Al 2 o 3 =50, 4.2g dispersed in 300mL 0.5MHNO 3 In the solution, a hydrogel is formed, stirred at room temperature for 1h, put into a synthesis kettle, placed at 150°C for 3h, and adjusted to pH 13 with 6M NaOH; then 12.0g 16wt% cetyltrimethylammonium bromide Drop the solution into the hydrogel, stir at 50°C for 40min, and adjust the pH to about 10 with hydrochloric acid; after stirring evenly, put it into a crystallization kettle lined with polytetrafluoroethylene, and crystallize at 110°C for 3 days; then filter, wash, and dry at 100°C Dry at ℃ for 24h; then bake at 550℃ in air atmosphere for 8h to obtain the target product. The molecular sieve sample whose crystal phase is MCM-41 was obtained by XRD analysis. According to infrared spectrum (IR) analysis, the framework of the MCM-41 product contains Beta zeolite secondary structural units.

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Abstract

The invention discloses a preparation method of a mesopore molecular sieve containing a beta zeolite secondary structural unit. The preparation method comprises the following steps of: mixing industrial beta zeolite and an acidic solution to prepare hydrogel; evenly mixing the hydrogel and a template to prepare an MCM-41 molecular sieve synthetic material; and crystallizing under suitable conditions to obtain the MCM-41 molecular sieve product containing the beta zeolite secondary structural unit. Compared with the prior art, the method of the invention has simple process, the synthesized molecular sieve has the structure of an MCM-41 molecular sieve, obviously improves the acidity and the aquathermal stability and can be used in the technical fields of catalytic cracking, hydrogenation cracking, hydrogenation treatment, hydrogenation modification, and the like.

Description

technical field [0001] The invention relates to a method for synthesizing mesoporous molecular sieves, which is a method for synthesizing mesoporous molecular sieves containing Beta zeolite secondary structural units by using beta zeolite (ie Beta zeolite) raw material as a silicon-aluminum source. Background technique [0002] Microporous molecular sieves have a uniform and well-developed microporous structure and strong acidity. They are important shape-selective catalysts in the modern petroleum industry and have a large specific surface area (>350m 2 g -1 ), adjustable pore size (0.2-1.2nm), hydrophilicity, high thermal stability (>500°C) and chemical stability. However, due to the small pore size, it is difficult for large-diameter molecules to enter the pores, and the macromolecules formed in the pores cannot escape quickly, resulting in side reactions, thus limiting its application range. Generally speaking, microporous molecular sieves are suitable for reacti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 张海娟李江红张喜文
Owner CHINA PETROLEUM & CHEM CORP
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