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Hierarchical structure hybrid loaded atomic precision gold nanocluster catalyst and preparation method thereof

A technology of gold nanoclusters and hybrids, applied in the field of noble metal nanocatalysts, to achieve large specific surface area, obvious performance advantages, and the effect of improving specific surface area

Pending Publication Date: 2022-03-01
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there has been no report on atomically precise gold nanocluster catalysts supported by nanosheet array-like hierarchical structure hydrotalcite / reduced graphene oxide (LDH / rGO) hybrids

Method used

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  • Hierarchical structure hybrid loaded atomic precision gold nanocluster catalyst and preparation method thereof
  • Hierarchical structure hybrid loaded atomic precision gold nanocluster catalyst and preparation method thereof
  • Hierarchical structure hybrid loaded atomic precision gold nanocluster catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Au 25 Capt 18 Preparation of nanoclusters

[0028] Weigh 1.0g of HAuCl 4 4H 2 O into 100mL methanol, configure to obtain 10mg / mL chloroauric acid methanol solution, measure 24.69mL of the above solution and 0.3804g TOABr (0.69mmol) into a 100mL single-necked flask filled with 20.31mL methanol, at 25±1°C in a water bath at 1200rpm With magnetic stirring, the mixture turned from orange yellow to deep red. After 15 minutes, 0.3912g captopril (0.60mmol) was added in the reaction solution, and the color of the solution turned white rapidly. After reacting for 30 minutes, the stirring rate was adjusted to 600rpm, and then 15mL NaBH 4 The ice solution was quickly added to the above reaction solution, and the color of the solution immediately changed to brown-green. After the above reaction solution was continuously reacted in a water bath at 25°C for 48 hours, it was centrifuged (4800r / min, 20min) to remove unreacted and insoluble Au(I):Capt polymer. The supernatant...

Embodiment 2

[0035] (1) Au 25 Capt 18 The preparation of nanoclusters is the same as in Example 1.

[0036] (2)Ni 3 The preparation of the Al-LDH / rGO hybrid carrier is the same as in Example 1.

[0037] (3) Au 25 / Ni 3 Preparation of Al-LDH / rGO catalyst

[0038] 25mg Au 25 Capt 18 Nanoclusters were dissolved in 100mL deionized water to obtain 0.25mg / mL Au 25 Capt 18 aqueous solution. 1.0g of Ni 3 The Al-LDH / rGO hybrid carrier was placed in a 150 mL beaker, 50 mL of deionized water and an appropriate amount of 0.1 mol / L sodium carbonate solution were added and ultrasonicated for 15 minutes to obtain a hybrid carrier dispersion with pH ~ 10.0. Measure 20mL0.25mg / mL Au 25 Capt 18 Aqueous solution, add an appropriate amount of 0.1mol / L sodium carbonate solution to adjust the pH to 8.0 in advance, add it to the above carrier dispersion under vigorous stirring, the theoretical loading of gold nanoclusters is 0.5wt%, and stir at 1000rpm for 4 hours. The mixture was collected by cent...

Embodiment 3

[0040] (1) Au 25 Capt 18 The preparation of nanoclusters is the same as in Example 1.

[0041] (2)Ni 3 The preparation of the Al-LDH / rGO hybrid carrier is the same as in Example 1.

[0042] (3) Au 25 / Ni 3 Preparation of Al-LDH / rGO catalyst

[0043] 25mg Au 25 Capt 18 Nanoclusters were dissolved in 100mL deionized water to obtain 0.25mg / mL Au 25 Capt 18 aqueous solution. 1.0g of Ni 3 The Al-LDH / rGO hybrid carrier was placed in a 150 mL beaker, 50 mL of deionized water and an appropriate amount of 0.1 mol / L sodium carbonate solution were added and ultrasonicated for 10 minutes to obtain a hybrid carrier dispersion with pH ~ 8.0. Measure 20mL0.25mg / mL Au 25 Capt 18 Aqueous solution, add an appropriate amount of 0.1mol / L sodium carbonate solution to adjust the pH to 8.0 in advance, add it to the above carrier dispersion under vigorous stirring, the theoretical loading of gold nanoclusters is 0.5wt%, and stir at 1000rpm for 4 hours. The mixture was collected by centr...

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Abstract

The invention relates to a multi-stage structure hybrid loaded atomic precision gold nano-cluster catalyst and a preparation method thereof. Belongs to the technical field of noble metal nano-catalysts. The expression of the catalyst is Au < n > / (M < 2 + >) Al-LDH / rGO-T, LDH nanosheets in a carrier of the catalyst vertically grow on two sides of rGO in a staggered manner, and M < 2 + > is any one or two of Mg < 2 + >, Ni < 2 + > and Co < 2 + > ions; the Au is a gold nanocluster, n is equal to 25, 38 and 127, and the Au is highly dispersed at the edge position of the LDH nanosheet and the junction of the LDH and the rGO; t represents the calcination temperature and is 260-300 DEG C. A captopril-protected Au nano-cluster is loaded on a hybrid carrier through a pH double-control electrostatic adsorption method, and a ligand is removed through moderate calcination, so that the catalyst is obtained. The method has the advantages that the obtained catalyst has a large specific surface area and more active sites, and shows high activity and high selectivity in the process of preparing benzaldehyde through solvent-free aerobic oxidation of benzyl alcohol under the condition of no additional alkali.

Description

technical field [0001] The invention belongs to the technical field of noble metal nano-catalysts, and in particular relates to a nanosheet array-like multi-level structure LDH / rGO hybrid supported atomic precision gold nano-cluster catalyst and a preparation method thereof. Background technique [0002] Selective oxidation of alcohols has become an important organic synthesis process because the corresponding aldehydes and ketones are important intermediates and precursors of medicines, pesticides, vitamins and fine chemicals. The catalysts commonly used to catalyze the selective oxidation of alcohols can be divided into homogeneous catalysts and heterogeneous catalysts. Homogeneous catalysts mainly include 2,2,6,6-tetramethylpiperidine-N-oxyl radical (TEMPO), complexes of Ru and Pd, etc., which have uniform active centers and are easy to contact with reactants. , thus showing high catalytic activity. However, due to its difficulty in separating from the product and causi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J23/66B01J37/34B01J37/03C07C45/38C07C47/54
CPCB01J23/892B01J23/8946B01J23/66B01J23/8913B01J37/348B01J37/342B01J37/03C07C45/38B01J35/40C07C47/54
Inventor 张慧于淑娣李进郭佳伟汪青琳魏卓君
Owner BEIJING UNIV OF CHEM TECH
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