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porous carbon @pd-al 2 o 3 @ meso tio 2 Microsphere catalyst and its preparation and application

A porous carbon and catalyst technology, applied in the chemical field, can solve the problems of low chemical stability and thermal stability of polymer hollow microspheres, easily damaged structure, large amount of solvent, etc., and achieve good thermal stability and recycling performance , High selectivity, small dosage effect

Active Publication Date: 2020-08-11
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires a long period of polymerization reaction, and the template removal method is an organic solvent extraction method, which takes a long time and consumes a large amount of solvent
The chemical stability and thermal stability of polymer hollow microspheres are not high, and the structure is easily destroyed

Method used

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  • porous carbon @pd-al <sub>2</sub> o <sub>3</sub> @ meso tio <sub>2</sub> Microsphere catalyst and its preparation and application
  • porous carbon @pd-al <sub>2</sub> o <sub>3</sub> @ meso tio <sub>2</sub> Microsphere catalyst and its preparation and application
  • porous carbon @pd-al <sub>2</sub> o <sub>3</sub> @ meso tio <sub>2</sub> Microsphere catalyst and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1. 30%C@0.8%Pd-29.2%Al 2 o 3 @40%m-TiO 2 Preparation of (Pd loading of 0.8%, porous carbon content of 30%, Al 2 o 3 The content is 29.2%, mesoporous TiO 2 content is 40%)

[0020] (1) Dissolve 4 g of glucose in 25 mL of deionized water, add to a 30 mL Teflon-lined hydrothermal kettle, heat at 180°C for 8 hours, centrifuge and wash repeatedly with ethanol until the centrifuged supernatant is colorless, after separating the solution Dry to obtain carbon microspheres. The carbon microspheres were heated to 750 ° C in a tube furnace for 2 h under a nitrogen flow rate of 15 mL / min to form porous carbon microspheres.

[0021] (2) Disperse 0.45g of porous carbon microspheres in 40mL of ethanol, add 5.7mL of 20mmol / L palladium chloride ethanol solution and 1.8g of aluminum isopropoxide, stir at room temperature for 0.5h, heat to 120°C and reflux for 10h , and then concentrate the solution to 25mL, add 10mL of deionized water and stir evenly, then transfer to a 50mL...

Embodiment 2

[0023] Example 2. 35%C@1.0%Pd-28%Al 2 o 3 @36%m-TiO 2 Preparation of (Pd loading 1.0%, porous carbon content 35%, Al 2 o 3 The content is 28%, mesoporous TiO 2 content is 36%)

[0024] (1) Dissolve 4 g of glucose in 25 mL of deionized water, add to a 30 mL Teflon-lined hydrothermal kettle, heat at 180°C for 12 hours, centrifuge and wash repeatedly with ethanol until the centrifuged supernatant is colorless, and separate the solution Dry to obtain carbon microspheres. The carbon microspheres were heated to 780°C in a tube furnace for 2 hours under a nitrogen flow rate of 20mL / min to form porous carbon microspheres.

[0025] (2) Disperse 0.50g of porous carbon microspheres in 40mL of ethanol, add 6.7mL of 20mmol / L palladium chloride ethanol solution and 1.6g of aluminum isopropoxide, stir at room temperature for 0.5h, heat to 120°C and reflux for 10h , and then concentrate the solution to 25mL, add 10mL of deionized water and stir evenly, then transfer to a 50mL polytetra...

Embodiment 3

[0027] Example 3. 40%C@1.2%Pd-20%Al 2 o 3 @38.8%m-TiO 2 Preparation of (Pd loading 1.2%, porous carbon content 40%, Al 2 o 3 The content is 20%, mesoporous TiO 2 content is 38.8%)

[0028] (1) Dissolve 4 g of glucose in 25 mL of deionized water, add to a 30 mL Teflon-lined hydrothermal kettle, heat at 180°C for 16 hours, centrifuge and wash repeatedly with ethanol until the centrifuged supernatant is colorless, after separating the solution Dry to obtain carbon microspheres. The carbon microspheres were heated to 800 ° C in a tube furnace for 2 h under a nitrogen flow rate of 25 mL / min to form porous carbon microspheres.

[0029] (2) Disperse 0.55g of porous carbon microspheres in 40mL of ethanol, add 7.8mL of 20mmol / L palladium chloride ethanol solution and 1.1g of aluminum isopropoxide, stir at room temperature for 0.5h, heat to 120°C and reflux for 10h , and then concentrate the solution to 25mL, add 10mL of deionized water and stir evenly, then transfer to a 50mL po...

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Abstract

The invention discloses a porous carbon@Pd-Al2O3@mesoporous TiO2 microspherical catalyst and preparation and application thereof. The catalyst herein structurally has a core of porous carbon microspheres, an intermediate Al2O3 layer containing nano palladium and an outer layer of mesoporous TiO2. The preparation includes the main steps of preparing porous carbon microspheres and then aluminum solcontaining nano palladium; mixing the hollow carbon microspheres, the aluminum sol containing nano palladium and water, thermally treating the mixture to obtain porous carbon@Pd-Al2O3 microspheres, mixing the porous carbon@Pd-Al2O3 microspheres, tetrabutyl titanate, ethanol and water, subjecting the mixture to hydrolytic polycondensation to obtain porous carbon@Pd-Al2O3@TiO2, and etching via NaOHsolution to obtain porous carbon@Pd-Al2O3@mesoporous TiO2 composite microsphere catalyst. The catalyst that is of sandwich microsphere structure has uniform nano palladium distribution, is applicableto catalytic oxidation of aqueous benzyl alcohol; reactant and product have good diffusibility and high activity under the conditions of zero alkaline aids and normal-pressure oxygen as an oxidant, separation with the product is easy, and the catalyst has good recyclability.

Description

technical field [0001] The invention belongs to the field of chemistry, and specifically relates to a porous carbon @Pd-Al that uses water as a solvent and oxygen as an oxidant under atmospheric pressure to oxidize and clean benzaldehyde to produce benzaldehyde 2 o 3 @mesoporous TiO 2 Preparation and application of microsphere catalysts. Background technique [0002] Benzaldehyde is an important intermediate and industrial raw material, widely used in the production of pharmaceutical intermediates, spices, seasonings, dyes and other fine chemicals. The industrial production of benzaldehyde is by chlorination hydrolysis and toluene oxidation through toluene side chain chlorination followed by hydrolysis. The chlorination hydrolysis method will make the benzaldehyde product contain chlorine so that its application in medicine, food and other industries is limited, and a large amount of harmful gases will be produced in the production process to cause environmental pollution...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44B01J35/10C07C45/38C07C47/54
CPCB01J23/44B01J35/006B01J35/0073B01J35/1061C07C45/38C07C47/54Y02P20/584
Inventor 陈丽娟向育君廖博晏精青佟占鑫石亮
Owner HUNAN UNIV OF SCI & TECH
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