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A Direct Synthesis Method of Hierarchical Ordered Mesoporous Molecular Sieves

A technology of mesoporous molecular sieve and synthesis method, which is applied in the field of direct synthesis of multi-level ordered mesoporous molecular sieves, can solve the problems of high price, complex process and poor effect, and achieve improved conversion rate, good catalytic activity and simple process effective effect

Inactive Publication Date: 2019-09-17
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the problems of high price, complex process and poor effect in the process of synthesizing multi-level ordered mesoporous molecular sieves in the prior art, and provide a simple and effective direct synthesis method of multi-level ordered mesoporous molecular sieves

Method used

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  • A Direct Synthesis Method of Hierarchical Ordered Mesoporous Molecular Sieves
  • A Direct Synthesis Method of Hierarchical Ordered Mesoporous Molecular Sieves
  • A Direct Synthesis Method of Hierarchical Ordered Mesoporous Molecular Sieves

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Embodiment 1

[0022] A direct synthesis method of multi-stage ordered mesoporous molecular sieves, including the following steps: put the template cetyltrimethylammonium bromide (CTAB) in water, raise the temperature to 70°C, dissolve, and add tetraorthosilicate Ethyl acetate, sodium hydroxide and aluminum sulfate were cooled to room temperature and stirred for 1 hour to obtain the aged gel solution, which was transferred to a stainless steel hydrothermal synthesis reactor and sealed, crystallized at 110°C for 3 days, and then heated to Crystallize at 160°C for 5 days, centrifuge, wash the solid with water, dry, and calcinate at 550°C for 6 hours to obtain a multi-stage ordered mesoporous molecular sieve;

[0023] The molar ratio of the template cetyltrimethylammonium bromide, tetraethyl orthosilicate, sodium hydroxide and aluminum sulfate is 6:2:1:1, and the template cetyltrimethylammonium bromide The mass ratio of ammonium bromide to water is 1:1100; see figure 1 , figure 2 , image 3 , Fi...

Embodiment 2

[0026] A direct synthesis method of multi-stage ordered mesoporous molecular sieves, including the following steps: putting the template cetyltrimethylammonium bromide into water, heating to 65°C, dissolving, adding sodium silicate and potassium hydroxide And sodium aluminate, cooled to room temperature, stirred for 1.5 hours to obtain the aging gel liquid, transferred to the stainless steel hydrothermal synthesis reactor and sealed, crystallized at 100 ℃ for 3 days, raised the temperature to 155 ℃ for crystallization After 6 days of centrifugation, the solid was washed with water, dried, and calcined at 550°C for 6 hours to obtain a multi-level ordered mesoporous molecular sieve;

[0027] The molar ratio of the template cetyltrimethylammonium bromide, sodium silicate, potassium hydroxide and sodium aluminate is 6:50:20:0.1, and the template cetyltrimethyl bromide The mass ratio of ammonium to water is 1:1000.

[0028] It is used in the aldehyde-ketone condensation reaction of ben...

Embodiment 3

[0030] A direct synthesis method of multi-stage ordered mesoporous molecular sieves, including the following steps: putting the template cetyltrimethylammonium bromide into water, heating to 75°C, dissolving, adding water glass, ammonium hydroxide and Tert-butyl aluminum, cooled to room temperature, stirred for 0.5 hours to obtain the aging gel liquid, transferred to the stainless steel hydrothermal synthesis reactor and sealed, crystallized at 90 ℃ for 4 days, and then heated to 150 ℃ for crystallization 7 After centrifugation, the solid was washed with water, dried, and calcined at 550°C for 6 hours to obtain a multi-level ordered mesoporous molecular sieve;

[0031] The molar ratio of the template cetyltrimethylammonium bromide, water glass, ammonium hydroxide and tert-butyl aluminum is 6:70:30:10, and the template cetyltrimethyl bromide The mass ratio of ammonium to water is 1:1200.

[0032] It is used in the aldehyde-ketone condensation reaction of benzaldehyde and 2-hydroxya...

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Abstract

The invention discloses a direct synthesis method of a multistage ordered mesoporous melocular sieve. The method includes the steps: placing template agent hexadecyl trimethyl ammonium bromide into water, raising the temperature to 65-75DEG C for dissolving, adding a silicon source, alkali and an aluminum source, cooling to room temperature, and performing stirring for 0.5-1.5 hours to obtain an aged gel solution; transferring the gel solution to a stainless steel hydrothermal synthesis reactor for sealing, performing crystallization for 3-4 days at 90-110DEG C, raising the temperature once more to 150-160DEG C for crystallization for 5-7 days before performing centrifugation, washing solids with water, and performing drying and calcining to obtain the multistage ordered mesoporous molecular sieve. The direct synthesis method is low in production cost and simple in technology process, the molecular sieve prepared has MFI micropores and an MCM-41 mesoporous structure, high mesoporous order is achieved, the advantages of high hydrothermal stability and mechanical stability and acidity are achieved, and good catalytic activity is achieved; the direct synthesis method is applicable topreparations in petrochemical industry and fine chemicals, adsorption separation and the field of separation of membrane separation and the like.

Description

Technical field [0001] The invention belongs to the field of porous materials and catalysis, and particularly relates to a direct synthesis method of multi-stage ordered mesoporous molecular sieves. Background technique [0002] Due to the advantages of flexible framework structure, controllable framework composition and uniform porosity, molecular sieves exhibit unique physical / chemical properties. In comparison with amorphous materials, they exhibit better ion exchange, stronger acidity, and higher hydrothermal stability. Based on these characteristics, molecular sieves have been applied in fields including industry and aviation, such as purification, absorption, separation and catalysis in petroleum refining, petrochemical and chemical processes. The pores inside the molecular sieve structure, the size of the pores, the size and shape of the channels, and the inherent connectivity may affect their practical applications, because the molecules need to enter the pores, store in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/00B01J29/06C07D311/32B01J20/18B01J20/28B01J20/30B01D71/02
Inventor 郭翔海张景双于川
Owner TIANJIN UNIV