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Method for preparing highly nitrogen-doped mesoporous carbon composites

A technology of composite materials and porous carbon, which is applied in the direction of hydrocarbons, hydrocarbons, carbon compound catalysts, etc., and can solve the problems of difficult materials handling in the scale-up process

Active Publication Date: 2017-12-08
UNIVERSITY OF STRASBOURG +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Despite their remarkable catalytic properties, these materials have various limitations: from high-temperature sensitivity (which makes them only well suited for low- or mesophilic catalytic processes) to severe synthetic limitations (i.e., intractable scale-up procedures and difficult material handling)

Method used

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  • Method for preparing highly nitrogen-doped mesoporous carbon composites
  • Method for preparing highly nitrogen-doped mesoporous carbon composites
  • Method for preparing highly nitrogen-doped mesoporous carbon composites

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0117] Example 1. General procedure for a highly N-rich active phase.

[0118] In a typical procedure, 2 g of dextrose and 3 g of citric acid were added to deionized water (10 mL) at room temperature (r.t.). Then, a fixed amount of ammonium carbonate (i.e., 1, 2 or 3 g) was added in a single portion to the mixture solution at room temperature and observed that due to CO 2 Instantaneous effervescence released. The suspension was stirred at room temperature until a clear solution was obtained, which was used as a source mixture for obtaining N-doped carbonaceous material deposited on a suitable support (after support soaking / impregnation). As for the latter, 2 g of different supports were used, i.e., SiC extrudates (30 m 2 g -1 ; SICAT), SiC powder (25m 2 g -1 ; SICAT), SiC foam (30m 2 g -1 ; SICAT), and α-Al 2 o 3 Beads (6m 2 g -1 ; Sasol). Slowly heat the wet solid in air: from room temperature to 130°C (10°C min -1 heating rate) and maintained at this temperature...

Embodiment 2

[0119] Example 2. Material Characterization.

[0120] With Bruker Avance DRX-400 spectrometer (400.13 and 100.61MHz, respectively for 1 H and 13 C) to obtain 1D ( 1 H and 13 C{ 1 H}) NMR spectrum. In ppm, relative to trimethylsilane (TMS), referenced to residual solvent resonance ( 1 H and 13 C) Chemical shifts, to report chemical shifts (δ).

[0121] With Setaram instrument, use 25mL min -1 Air flow rate and 10°C min from room temperature to 1000°C -1 The heating rate was used for thermogravimetric analysis (TGA). At liquid nitrogen temperature, by the BET method, using N 2 As an adsorbent (TriStar sorptometer), the specific surface area of ​​the different samples was measured. Before measurement, the samples were degassed overnight at 200°C to desorb moisture and impurities on their surfaces. XPS measurements of the supports were performed with a MULTILAB 2000 (THERMO VG) spectrometer equipped with an Al Ka ​​anode (hν = 1486.6 eV) using a 10 min acquisition. Pea...

Embodiment 3

[0122] Embodiment 3. catalytic reaction

[0123] 3.1 Oxygen Reduction Reaction (ORR).

[0124] In a three-electrode cell, in 0.1 M KOH supporting electrolyte, using a device equipped with a scan rate of 10 mV s -1 Electrochemical studies were performed on an Autolab PGSTAT30 (Eco Chemie, Netherlands) potentiostat with an analog linear sweep generator at 25°C. Mercury oxide (Hg / HgO) electrode and Pt wire electrode were used as reference electrode and counter electrode, respectively. Unless otherwise stated, in the following, all potentials are referred to as reversible hydrogen electrodes (RHE). Electrochemical impedance spectroscopy (EIS) was used to determine the electrolyte solution resistance.

[0125] 10.0 mg of catalyst sample, 5 mL of isopropanol, and 50 μL of Nafion solution (5 wt %) were ultrasonically mixed to form a homogeneous catalyst ink. For defined RRDE tests, 50 μL of catalyst ink was loaded onto a preconditioned glassy carbon (GC) electrode (5.5 mm diamete...

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Abstract

The present invention deals with a new methodology aimed at preparing highly N-doped mesoporous carbon macroscopic composites, and their use as highly efficient heterogeneous metal-free catalysts in a number of industrially relevant catalytic transformations.

Description

[0001] priority [0002] This application claims priority to European Patent Application No. EP 15152038.4 and Provisional European Patent Application No. EP15152039.2, filed 21 January 2015, the entire contents of which are incorporated herein by reference. technical field [0003] The present invention relates to novel methods aimed at the preparation of highly nitrogen-doped mesoporous carbon macroscopic composites and their use as highly efficient heterogeneous metal-free Use of catalyst (highly efficient heterogeneous metal-free catalyst). [0004] In this document, numbers in italics and between brackets ( ) refer to the list of references given at the end of this document. Background technique [0005] Rethinking fundamental metal-based catalytic processes, inspired by the design and fabrication of custom metal-free catalytic structures from cheap and readily available building blocks, is a challenging matter for modern and truly sustainable catalysis. Over the past...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J32/00
CPCB01J27/24B01J21/04B01J21/18B01J27/20B01J27/224B01J37/0203H01M4/96C01B17/0465Y02E60/50B01J20/20B01J35/19B01J35/50B01J35/647B01J37/0217B01J37/0221B01J37/0236B01J37/0244B01J37/04C07C5/333C07C2521/04C07C2527/224C07C2527/24
Inventor 刚帕友朱利亚诺·詹巴斯蒂亚尼刘岳峰乌斯塞努·巴阮定兰简-马里奥·赫特刚东越
Owner UNIVERSITY OF STRASBOURG
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