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Preparation method of mesoporous molecular sieve containing L 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 complex synthesis process, achieve large adjustable range, good diesel aromatics hydrogenation sulfur resistance and ring-opening performance , acidity and acidity-enhancing effect

Inactive Publication Date: 2012-05-09
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.

Method used

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  • Preparation method of mesoporous molecular sieve containing L zeolite secondary structural unit
  • Preparation method of mesoporous molecular sieve containing L zeolite secondary structural unit
  • Preparation method of mesoporous molecular sieve containing L zeolite secondary structural unit

Examples

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Effect test

Embodiment 1

[0030] Industrial synthesis of NH 4 Exchanged NH 4 L(SiO 2 / Al 2 o 3 Molecular molar ratio is 10, the following are all SiO 2 / Al 2 o 3 All molecular molar ratios) zeolite 7.2g 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 16.5g 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 MCM-41 product framework cont...

Embodiment 2

[0032] Industrial synthesis of NH 4 Exchanged NH 4 L(SiO 2 / Al 2 o 3 Molecular molar ratio is 10, 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, add 8g of tetraethyl orthosilicate, and adjust the pH to about 10 with hydrochloric acid; stir evenly and put the materials into a crystallization kettle lined with polytetrafluoroethylene. 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...

Embodiment 3

[0034] Industrially synthesized pretreated L zeolite, SiO 2 / Al 2 o 3 =30, 12.2g 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 MCM-41 product framework contains L zeolite secondary structural units.

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Abstract

The invention discloses a preparation method of a mesoporous molecular sieve containing an L zeolite secondary structural unit. The method comprises the following steps of: mixing industrial L zeolite with an acid solution to obtain aqua gel; uniformly mixing the aqua gel with a template to obtain an MCM-41 molecular sieve synthetic material; and crystalizing under appropriate conditions to obtain an MCM-41 molecular sieve product containing the L zeolite secondary structural unit. Compared with the prior art, the method has the advantages that: the process is simple, the synthetic molecular sieve has an MCM-41 molecular sieve structure, and the acidity and hydrothermal stability are enhanced remarkably. The synthetic molecular sieve product can be applied in the technical fields of catalytic cracking, hydrocracking, hydrotreatment, hydrogenation modification and the like.

Description

technical field [0001] The invention relates to a synthesis method of mesoporous molecular sieve, which is a method for synthesizing mesoporous molecular sieve containing L zeolite secondary structural unit by using L zeolite raw material as 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 reactions in which the kinetic diameter...

Claims

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Application Information

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Patent Type & Authority Applications(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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