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Supported palladium hierarchical-structure catalytic material, and preparation method and application thereof

A technology of catalytic materials and supported palladium, which is applied in the field of catalytic materials for catalytic coupling reactions and its preparation, can solve the problems of time-consuming and cumbersome synthesis processes, and achieve the effects of simple conditions, strong operability, and difficult recovery

Inactive Publication Date: 2020-06-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the current research, although most supported Pd-based catalyst materials such as three-dimensional multi-level nanomaterials with hollow structures [Energy Environ. However, most of its synthesis processes are tedious and time-consuming, so it will be of great significance to develop a rapid and stable preparation method to obtain highly dispersed Pd-loaded nanocatalytic materials.

Method used

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  • Supported palladium hierarchical-structure catalytic material, and preparation method and application thereof
  • Supported palladium hierarchical-structure catalytic material, and preparation method and application thereof
  • Supported palladium hierarchical-structure catalytic material, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A. Preparation of copper hydroxide nanowire array / copper foam precursor

[0031] Using copper foam with a purity greater than 90% and a size of 3×4 cm as a raw material, the copper foam was cleaned with acetone / ethanol, hydrochloric acid, and deionized water under ultrasound for 3 minutes.

[0032] Weigh 2.28g of ammonium persulfate and 10.0g of sodium hydroxide, dissolve them in 100mL of deionized water, and make a mixed solution, soak the above foamed copper in the mixed solution, react at room temperature for 20min, take it out, and use Wash thoroughly with ionized water and ethanol, and dry in an oven at 60°C to obtain Cu(OH) 2 / CF.

[0033] B.Co(OH) 2 / Cu(OH) 2 / Preparation of CF precursor

[0034] Cu(OH) prepared in step A 2 / CF was cut into a piece of 1cm×1cm×0.5mm, and it was used as the working electrode, the Pt mesh was used as the counter electrode, and the Ag / AgCl electrode (3mol L -1 KCl) as a reference electrode, in 10mL of electrolytic solution con...

Embodiment 2

[0038] A. step is the same as embodiment 1

[0039] B. Preparation of cobalt hydroxide / copper hydroxide nanotube array / copper foam precursor

[0040] The copper hydroxide nanowire array / foam copper that step B makes is cut into the electrode piece that size is 1cm * 1cm * 0.5mm and uses it as working electrode, with Pt net as counter electrode, with Ag / AgCl electrode (3mol L -1 KCl) as a reference electrode, in 10mL of electrolyte containing 0.2182g cobalt nitrate hexahydrate, carry out constant voltage electrodeposition for 300s, and the voltage is -1.0V. Take out the electrode sheet after electrodeposition, remove excess electrolyte on the surface with deionized water, and dry it in an oven at 60°C for later use. Get Co(OH) 2 / Cu(OH) 2 / CF nanotube arrays, slightly smaller size Co(OH) 2 The nanosheets are tightly packed in Cu(OH) 2 nanowire surface.

[0041] C.Pd / Co(OH) 2 / Cu(OH) 2 Preparation of / CF

[0042] Weigh 2.94 mg of sodium chloropalladate and dissolve it i...

Embodiment 3

[0044] A, B step are the same as embodiment 1

[0045] C.Pd / Co(OH) 2 / Cu(OH) 2 Preparation of / CF

[0046] Weigh 4.41mg of sodium chloropalladate and dissolve it in 10mL of deionized water to obtain a solution with a concentration of 1.5mmol / L. The Co(OH) prepared in step B 2 / Cu(OH) 2 After the / CF nanotube array was immersed in it for 40 minutes at room temperature and reacted, it was thoroughly rinsed with deionized water and dried naturally at room temperature. Hollow tubular Pd / Co(OH) supported by Pd nanoparticles with a particle size of 6-8nm can be obtained 2 / Cu(OH) 2 / CF catalytic material.

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Abstract

The invention provides a supported palladium hierarchical-structure catalytic material, and a preparation method and application thereof. According to the invention, foamy copper is used as a substrate, and a composite three-dimensional hierarchical-structure array with a hollow structure is prepared by using an oxidation etching method and an electrochemical deposition method; then, palladium nanoparticles are stably loaded on the three-dimensional multi-stage nanotube array by utilizing an in-situ oxidation-reduction reaction; the catalytic material is expressed as Pd / Co(OH)2 / Cu(OH)2 / CF; andthe catalytic material shows relatively high catalytic activity on a Suzuki-Miyaura reaction under mild reaction conditions, and has good cycling stability. The catalyst has the advantages of simplicity and convenience in preparation, easiness in separation and recovery, high catalytic activity, low cost and the like, and has good application prospects.

Description

Technical field: [0001] The invention relates to a catalytic material for catalytic coupling reaction and its preparation, in particular to a supported palladium multi-level structure catalytic material, its preparation and its application in catalytic Suzuki reaction. Background technique: [0002] Coupling reaction is considered to be one of the most convenient methods to produce biaryl compounds and substituted aromatic compounds in the field of organic synthesis, and can be widely used in the synthesis of various natural products and organic materials. As a novel and typical coupling reaction, the Suzuki–Miyaura reaction can be used to synthesize derivatives of polyenes, styrene and biphenyl, and has mild reaction conditions, easy operation, strong substrate adaptability and Functional group tolerance, easy separation of raw materials and by-products and other advantages. [0003] At present, the use of homogeneous Pd-based catalysts is the most common catalytic method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J35/02C07C1/00C07C15/14C07C41/30C07C43/205C07C67/343C07C69/76C07C253/30C07C255/50B01J35/00
CPCB01J23/8926C07C1/00C07C41/30C07C67/343C07C253/30B01J35/40C07C15/14C07C43/205C07C69/76C07C255/50
Inventor 雷晓东曹艳明孔祥贵蒋美红李嘉力窦彤刘湉祝彪
Owner BEIJING UNIV OF CHEM TECH
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