Method for preparing double-catalysis center molecular sieve nucleocapsid material with hydrothermal/solvent-thermal system

A technology of molecular sieve and solvothermal, which is applied in the field of preparation of molecular sieve core-shell materials, achieves the effects of tight combination, reduced catalytic cost, and improved reaction efficiency

Inactive Publication Date: 2008-12-03
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, the introduction of dual catalytic centers into molecular sie

Method used

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  • Method for preparing double-catalysis center molecular sieve nucleocapsid material with hydrothermal/solvent-thermal system
  • Method for preparing double-catalysis center molecular sieve nucleocapsid material with hydrothermal/solvent-thermal system
  • Method for preparing double-catalysis center molecular sieve nucleocapsid material with hydrothermal/solvent-thermal system

Examples

Experimental program
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Effect test

Embodiment 1

[0066] Cr-AFI crystals with a size of 20 microns are used as the core part of the molecular sieve core-shell material, and lamellar Ti-AFI nanocrystals are used as the shell part.

[0067] 0.5 g of carefully ground aluminum isopropoxide (Al(OPr i ) 3 ) dissolved in polyethylene glycol (pEG) (5mL) and water (H 2 O) (5mL) mixed system, add phosphoric acid (H 3 PO 4, 85%) (0.215mL), triethylamine (TEA) (0.273mL), chromium chloride (CrCl 3 ·6H 2 O) (0.0391 g), stirred at room temperature for 10 hours to obtain a synthetic sol of Cr-AFI, crystallized at 180 ° C for 12 hours, and synthesized transition metal Cr-doped AFI nuclear molecular sieve crystals with a particle size of 20 to 30 μm (SEM scanning electron microscope). , as the core part of the core-shell material. The substitution amount of Cr was determined to be 1% by ICP, and Cr entered into the AFI skeleton by ultraviolet-visible spectroscopy.

[0068] The prepared Cr-AFI nuclear molecular sieve crystals were ultras...

Embodiment 2

[0074] The Cr-AFI crystal with a size of 20 microns is used as the core part of the molecular sieve core-shell material, and the lamellar V-AFI nanocrystal is used as the shell part.

[0075] Finely ground aluminum isopropoxide (Al(OPr i ) 3 ) 0.5 g dissolved in polyethylene glycol (pEG) (5 mL) and water (H 2 O) (5mL) mixed system, add phosphoric acid (H 3 PO 4 , 85%) (0.215mL), triethylamine (TEA) (0.273mL), chromium chloride (CrCl 3 ·6H 2 O) (0.0391 g), stirred at room temperature for 10 hours to obtain a synthetic sol of Cr-AFI, crystallized at 180 ° C for 12 hours, and synthesized transition metal Cr-doped AFI molecular sieve crystals with a particle size of 20 to 30 μm, as core-shell materials. nuclear part. The substitution amount of Cr was determined to be 1% by ICP, and Cr entered into the AFI skeleton by ultraviolet-visible spectroscopy.

[0076] The prepared Cr-AFI molecular sieve crystals were ultrasonically washed three times with deionized water, and then d...

Embodiment 3

[0081] The Fe-AFI crystal with a size of 20 microns is used as the core part of the molecular sieve core-shell material, and the lamellar Ti-AFI nanocrystal is used as the shell part.

[0082] Finely ground aluminum isopropoxide (Al(OPr i ) 3 ) 0.5 g dissolved in polyethylene glycol (pEG) (5 mL) and water (H 2 O) (5mL) mixed system, add phosphoric acid (H 3 PO 4 , 85%) (0.215mL), triethylamine (TEA) (0.273mL), ferric chloride (FeCl 3 ) (0.0243 g), stirred at room temperature for 10 hours to obtain a sol of Fe-AFI, crystallized at 180 ° C for 12 hours, and synthesized transition metal Fe-doped AFI molecular sieve crystals with a particle size of 20-30 μm as the core part of the core-shell material .

[0083] The prepared Fe-AFI molecular sieve crystals were ultrasonically washed three times with deionized water, and then dried in an oven at 50°C.

[0084] Finely ground aluminum isopropoxide (Al(OPr i ) 3 ) 0.3 g dissolved in polyethylene glycol (pEG) (7mL) and water (H ...

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Abstract

The invention belongs to a preparation technology of a molecular sieve core-shell material, in particular relating to a method for preparing the molecular sieve core-shell material with a double catalytic center by utilizing a water-thermal/solvent-thermal epitaxial growth method. The molecular sieve core-shell material prepared by the method can be respectively doped with different transition metal ions in two parts of a core and a shell according to the catalytic need so as to provide different catalytic centers. The method comprises the following steps that: a method of two-step synthesis is adopted, a molecular sieve crystal doped with transition metal ions A is prepared first, then is added into is a sol system of a molecular sieve crystal doped with transition metal ions B and is subject to water-thermal/solvent-thermal crystallization, and a micropore composite material provided with the double catalytic center can be produced by removing a template under high temperature. The molecular sieve core-shell material can be widely applied in the catalytic field through adjusting and changing the kind of doped metals, and is more suitable for being applied in fields of heterocatalytic reactions needing two-step catalysis, terminal group oxidation reactions of alkane, and structure reforming of long-chain alkane.

Description

technical field [0001] The invention belongs to the preparation technology of molecular sieve core-shell materials, and in particular relates to a method for preparing molecular sieve-like core-shell materials with double catalytic centers by using a hydrothermal / solvothermal epitaxial growth method. technical background [0002] Because zeolite and aluminum phosphate molecular sieve materials have periodic three-dimensional framework and regular pore structure, they are widely used in the fields of catalysis, ion exchange, gas adsorption, separation, host-guest chemistry, microelectronic devices and optical devices. Utilizing these porous materials to fabricate hierarchical composite structures with controllable size, shape, and properties can broaden their applications in other fields. Especially metal-doped molecular sieves can introduce catalytic centers in the three-dimensional framework. The currently used metal-doped molecular sieve materials are all single-site cata...

Claims

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Application Information

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IPC IPC(8): B01J29/83B01J29/40B01J29/00C01B39/00
Inventor 于吉红田大勇闫文付徐如人
Owner JILIN UNIV
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