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Preparation method and application of high hydrogenation selectivity Au-Pd monatomic alloy catalyst

An alloy catalyst, selective technology, applied in catalyst activation/preparation, reductive alkylation preparation, organic compound/hydride/coordination complex catalyst, etc., can solve the problem of low hydrogenation selectivity, low hydrogen activation capacity, etc. problem, to achieve the effect of high selectivity, simple preparation method and high catalytic activity

Active Publication Date: 2017-12-22
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The prepared Au-Pd single-atom alloy catalyst can overcome the problem of low hydrogen activation ability of Au and the low hydrogenation selectivity of Pd

Method used

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  • Preparation method and application of high hydrogenation selectivity Au-Pd monatomic alloy catalyst
  • Preparation method and application of high hydrogenation selectivity Au-Pd monatomic alloy catalyst
  • Preparation method and application of high hydrogenation selectivity Au-Pd monatomic alloy catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1: UiO-66-NH 2 preparation of

[0024] Preparation of UiO-66-NH by Hydrothermal Synthesis 2 . Weigh 0.23gZrCl 4 , 0.18g of 2-aminoterephthalic acid was dissolved in a mixed solution of 50ml of N, N-dimethylformamide and 0.15ml of water, and the mixed system was stirred at room temperature for 0.5h and then transferred to a polytetrafluoro-lined autoclave , placed in an oven at 120°C for 48h. After the removed reactor was cooled to room temperature, the solid product obtained by centrifugation was washed twice with N,N-dimethylformamide, and then stirred and washed with anhydrous methanol at room temperature for 12 hours. Dry in vacuum at 80°C for 12 hours before use.

Embodiment 2

[0025] Example 2: Au-Pd 0.03 @UiO-66-NH 2 preparation of

[0026] Weigh 0.2g dry UiO-66-NH 2 Solid, dispersed in a mixed system of 10ml water and 10ml ethanol, sonicated for 0.5h until uniformly dispersed. The configuration contains 1.33×10 -3 mol / LHAuCl 4 and 0.37×10 -4 mol / LH 2 PdCl 4 15ml of the solution, under the condition of ice bath, this solution was added drop by drop to UiO-66-NH through peristaltic pump within 40min 2 in the dispersed system. After the dropwise addition was completed, the mixture was further stirred under ice bath for 4 h. Then 5 ml of newly configured 0.08 mol / L sodium borohydride solution was added dropwise to the mixed system. After further stirring for 0.5 h, the obtained Au-Pd 0.03 @UiO-66-NH 2 Then wash with water three times, and vacuum-dry at 80°C until use. Example 3: Au-Pd 0.06 @UiO-66-NH 2 preparation of

Embodiment 3

[0027] Repeat the step in embodiment 3, difference is: the H 2 PdCl 4 The concentration of the solution was changed to 0.74×10 -4 mol / L.

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Abstract

The invention provides a preparation method and application of a high hydrogenation selectivity Au-Pd monatomic alloy catalyst, which belongs to the technical field of organic synthesis. The catalyst adopts MOF with an organic ligand being linked with an amino group as a carrier and adopts chloroauric acid and chloropalladic acid as metal precursors, the addition amount of Au and Pd is adjusted, when the Au loading amount is 1.93 weight percent, and the Pd loading amount is 0.02 to 0.11 weight percent, the monatomic alloy catalyst can be obtained, and the amino group has a decisive effect on the synthesis of the monatomic alloy. When nitrobenzene and benzaldehyde are used as raw materials, and when the raw materials of the prepared Au-Pd0.03@UiO-66-NH2 are completely converted under a mild condition, and 98 percent of N-benzyl aniline target product selectivity can be obtained. A coordination unsaturated metal locus of the MOF carrier can present certain L acidity, and the L acidity and a cyclohexane solvent used in the invention have apparent effect for promoting the condensation of aniline and benzyl alcohol.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to an amino immobilized metal precursor. Au-Pd single-atom alloy catalysts are prepared by a liquid-phase in-situ reduction method. In the reductive amination reaction of nitro compounds and aldehydes, they can be highly active and highly selective. Sexually catalyzed to generate secondary amines. Background technique [0002] Amines widely exist in natural products and synthetic substances, usually exhibit important biological activities, and can also serve as important linking structural units of substance molecules. According to the number of substituted hydrogen atoms in the amine molecule, amines can be divided into primary amines, secondary amines, and tertiary amines. Among them, secondary amines play an important role in practical industrial applications and are key intermediates for the synthesis of many substances such as dyes, additives, and drugs. For example, ...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J23/52B01J37/16C07C209/26C07C211/45
CPCB01J23/52B01J31/1691B01J31/2217B01J37/16C07C209/26C07C211/45
Inventor 梁长海殷冬冬李闯刘进轩
Owner DALIAN UNIV OF TECH
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