Hierarchical-pore titanium silicon molecular sieve catalyst synthesized with assistance of aerosol and preparation method of hierarchical-pore titanium silicon molecular sieve catalyst

An aerosol, multi-level pore technology, applied in molecular sieve catalysts, hydroxyl addition preparation, chemical instruments and methods, etc., to achieve the effects of mild conditions, high activity and simple methods

Inactive Publication Date: 2013-12-04
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the aerosol-assisted synthesis of titanium-silicon hierarchical porous molecular sieves containing TS-1 nanocrystals has not been reported so far.

Method used

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  • Hierarchical-pore titanium silicon molecular sieve catalyst synthesized with assistance of aerosol and preparation method of hierarchical-pore titanium silicon molecular sieve catalyst
  • Hierarchical-pore titanium silicon molecular sieve catalyst synthesized with assistance of aerosol and preparation method of hierarchical-pore titanium silicon molecular sieve catalyst
  • Hierarchical-pore titanium silicon molecular sieve catalyst synthesized with assistance of aerosol and preparation method of hierarchical-pore titanium silicon molecular sieve catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Mix the TPAOH solution with the silicon source, stir at 30°C for 6h, and at the same time mix the titanium source with the TPAOH solution, stir at 20°C for 3h, the molar ratio of each raw material after the two are mixed is: SiO 2 : TiO 2 :TPAOH:H 2 O=1:0.033:0.2:60, mix and distill alcohol for 2 hours, then put in a kettle and crystallize at 170°C for 4 hours.

[0028] (2) After cooling, the solid obtained by centrifuging the above solution is dispersed in the ethanol solution of CTAB, and a certain amount of silicon source is added dropwise. Stir for 3 hours to mix evenly, form an aerosol with air with a pressure of 10si through an aerosol generator, dry it through a quartz tube at 350°C to obtain a solid, dry it in an air atmosphere, and remove the template agent by roasting to obtain a hierarchical porous titanium-silicon molecular sieve product.

Embodiment 2

[0030] (1) Mix the TPAOH solution with the silicon source, stir at 30°C for 6h, and at the same time mix the titanium source with the TPAOH solution, stir at 20°C for 3h, the molar ratio of each raw material after the two are mixed is: SiO 2 : TiO 2 :TPAOH:H 2 O=1:0.033:0.2:60, mixed for 2 hours, distilled alcohol, put in a kettle and crystallized at 170°C for 4 hours.

[0031] (2) After cooling, add 50ml CTAB ethanol solution dropwise to the above solution, and add silicon source and titanium source: SiO 2 / TiO 2 =30. Stir for 3 hours to mix evenly, form an aerosol with air with a pressure of 10si through an aerosol generator, dry it through a quartz tube at 350°C to obtain a solid, dry it in an air atmosphere, and remove the template agent by roasting to obtain a hierarchical porous titanium-silicon molecular sieve product.

Embodiment 3

[0033] (1) Mix the TPAOH solution with the silicon source, stir at 30°C for 6h, and at the same time mix the titanium source with the TPAOH solution, stir at 20°C for 3h, the molar ratio of each raw material after the two are mixed is: SiO 2 : TiO 2 :TPAOH:H 2 O=1:0.33:0.2:60, mix for 2 hours, distill the alcohol, put in a kettle and crystallize at 170°C for 4 hours.

[0034] (2) After cooling, add 50ml CTAB ethanol solution dropwise to the above solution, and add silicon source and titanium source: SiO 2 / TiO 2 =60. Stir for 3 hours to mix evenly, form an aerosol with air with a pressure of 10si through an aerosol generator, dry it through a quartz tube at 350°C to obtain a solid, dry it in an air atmosphere, and remove the template agent by roasting to obtain a hierarchical porous titanium-silicon molecular sieve product.

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Abstract

The invention discloses a hierarchical-pore titanium silicon molecular sieve catalyst synthesized with the assistance of an aerosol and a preparation method of titanium silicon molecular sieve catalyst, and the titanium silicon molecular sieve catalyst is applied to the catalytic oxidation reaction of cyclohexene. The silicon molecular sieve catalyst is a hierarchical-pore titanium silicon molecular sieve synthesized through an aerosol method, is spherical, contains TS-1 nanometer crystals with MFI micropore structures, and is covered with a porous titanium silicon material. The catalyst can adopt hydrogen peroxide as an oxidant to perform catalytic oxidation on the cyclohexene to synthesize cyclohexene oxide, cyclohexanediol, cyclohexenone and cyclohexanol. The titanium silicon molecular sieve catalyst has the advantages that the preparation process is simple and continuous, the synthesis period is short, the atom utilization ratio is high, the titanium distribution is uniform, and the reaction can be magnified according to a certain ratio. The titanium silicon molecular sieve catalyst provided by the invention has the characteristics of mild reaction conditions, high activity and selectivity, small using amount, and easy recycling.

Description

technical field [0001] The invention belongs to the technical field of aerosol-assisted synthesis and application of molecular sieve materials, and relates to a method for aerosol-assisted synthesis of a titanium-silicon multi-stage molecular sieve catalyst and its application in catalytic oxidation of cyclohexene. Background technique [0002] TS-1 microporous molecular sieve showed good catalytic activity in olefin epoxidation, but its micropore size limited its application in macromolecular reactions. A lot of work at home and abroad is devoted to the synthesis of multi-level pore composite titanium-silicon molecular sieve materials, and it is hoped that such materials can show good catalytic performance in the oxidation of macromolecular olefins. The research on hierarchical molecular sieve materials at home and abroad is mainly focused on the traditional hydrothermal synthesis method. There are few reports on aerosol-assisted synthesis of hierarchical porous molecular s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89C07D301/12C07D303/04C07C27/16C07C29/04C07C35/14C07C45/28C07C49/603
Inventor 熊光郭振东
Owner DALIAN UNIV OF TECH
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