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Core/shell-type micropore /mesoporous composite titanium silicon molecular sieve and preparation method thereof

A silicon molecular sieve and composite titanium technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of unfavorable guest molecular diffusion, etc., and achieve the effects of strong controllability, regular structure, and simple preparation method

Inactive Publication Date: 2016-06-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in these materials, the microporous core and mesoporous shell are in close contact, which is not conducive to the diffusion of guest molecules.

Method used

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  • Core/shell-type micropore /mesoporous composite titanium silicon molecular sieve and preparation method thereof
  • Core/shell-type micropore /mesoporous composite titanium silicon molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Take 0.25g of microporous titanium-silicon molecular sieve TS-1 and disperse it in 40ml of deionized water and 20ml of absolute ethanol, add 0.5g of cetyltrimethylammonium bromide and 0.3g of ammonia water, stir for 0.5h, add 0.05g of m-benzene Diphenol and 0.075g of formaldehyde solution with a mass concentration of 37% were continuously stirred at room temperature for 8 hours, left to stand for 14 hours, the product was filtered out, and dried at 80°C to obtain a microporous titanium-silicon molecular sieve TS-1 coated with a phenolic resin polymer. (TS-1RF). Disperse 0.5g of TS-1RF in 100ml of deionized water and 60ml of absolute ethanol, add 0.05g of cetyltrimethylammonium bromide and 2g of ammonia water, stir at 40°C for 0.5h, add 0.57g of tetraethylsilicate and 0.018 g of n-tetrabutyl titanate, continuously stirred for 15 hours, filtered, dried at 80° C., and calcined at 550° C. for 5 hours in an air atmosphere to obtain a core / shell microporous / mesoporous composi...

Embodiment 2

[0020] Take 0.25g of microporous titanium-silicon molecular sieve TS-1 and disperse it in 40ml of deionized water and 20ml of absolute ethanol, add 0.5g of cetyltrimethylammonium bromide and 0.3g of ammonia water, stir for 0.5h, add 0.1g of m-benzene Diphenol and 0.15g of formaldehyde solution with a mass concentration of 37% were continuously stirred at room temperature for 8 hours, left to stand for 14 hours, filtered out the product, and dried at 80°C to obtain a microporous titanium-silicon molecular sieve TS-1 coated with a phenolic resin polymer (TS-1RF). Disperse 0.5g of TS-1RF in 100ml of deionized water and 60ml of absolute ethanol, add 0.05g of cetyltrimethylammonium bromide and 2g of ammonia water, stir at 40°C for 0.5h, add 0.57g of tetraethylsilicate and 0.018 g of n-tetrabutyl titanate, continuously stirred for 15 hours, filtered, dried at 80° C., and calcined at 550° C. for 5 hours in an air atmosphere to obtain a core / shell microporous / mesoporous composite tita...

Embodiment 3

[0022] Take 0.25g of microporous titanium-silicon molecular sieve TS-1 and disperse it in 40ml of deionized water and 20ml of absolute ethanol, add 0.5g of cetyltrimethylammonium bromide and 0.3g of ammonia water, stir for 0.5h, add 0.2g of m-benzene Diphenol and 0.3g of formaldehyde solution with a mass concentration of 37% were continuously stirred at room temperature for 8 hours, left to stand for 14 hours, filtered out the product, and dried at 80°C to obtain a microporous titanium-silicon molecular sieve TS-1 coated with a phenolic resin polymer (TS-1RF). Disperse 0.5g of TS-1RF in 100ml of deionized water and 60ml of absolute ethanol, add 0.05g of cetyltrimethylammonium bromide and 2g of ammonia water, stir at 40°C for 0.5h, add 0.57g of tetraethylsilicate and 0.018g of n-tetrabutyl titanate, continuously stirred for 15h, filtered, dried at 80°C, and calcined at 550°C for 5h in an air atmosphere to obtain a core / shell microporous / mesoporous composite titanium-silicon mol...

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Abstract

The present invention provides a core / shell-type micropore / mesoporous composite titanium silicon molecular sieve and a preparation method thereof. The composite molecular sieve has a nearly spherical morphology, a specific surface area of 500-700m<2> / g, and a typical core-shell structure, an inner core is microporous titanium silicon molecular sieve TS-1 with a diameter of 200-300nm, an outer shell layer is hexagonal ordered mesoporous titanium-containing silica with the aperture of 2-3nm, a gap is between the inner core and the outer shell, and gap size and outer shell thickness both can be modulated. The composite molecular sieve is prepared by a two-step process, and the microporous titanium silicon molecular sieve TS-1 is first coated with a phenolic resin polymer as a hard template, and then coated with the mesoporous titanium-containing silica. The effects and benefits are as follows: the composite molecular sieve has multi levels of channels, the hollow core-shell structure is conducive to diffusion of guest molecules, and has good use prospects in catalysis, adsorption and separation and other fields, and the preparation process is simple, efficient and highly controllable.

Description

technical field [0001] The invention belongs to the field of material preparation, and in particular relates to a multi-level porous composite titanium-silicon molecular sieve and a preparation method thereof. Background technique [0002] Titanium silicate molecular sieves have excellent catalytic performance for the selective oxidation of organic compounds under mild conditions, and have been widely concerned by researchers. Although traditional microporous titanium-silicon molecular sieves have high activity, their narrow pores limit their application in macromolecular reactions. Although mesoporous titanium silicate molecular sieves have open channels, their inherent activity is low due to their amorphous nature. Therefore, how to combine microporous and mesoporous titanium-silicon catalytic materials to make them complement each other has become a research hotspot in recent years. [0003] At present, the reported microporous composite molecular sieves and their prepa...

Claims

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Application Information

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IPC IPC(8): C01B39/08
Inventor 金长子王彦杰王军虎
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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