Preparation and application of loaded Pd3Cl cluster catalyst

A catalyst, supported technology, applied in the preparation of organic compounds, physical/chemical process catalysts, carbon-based compounds and other directions, can solve the problems of high reaction temperature, complex catalyst preparation, low yield, etc., to achieve a wide range of applications, Excellent cycle performance, high catalytic activity effect

Active Publication Date: 2017-11-10
ANHUI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] To sum up, there are still many problems in the existing catalytic system, such as complex catalyst preparation and large dosage, poor reaction selectivity, low yield, high reaction temperature, high oxygen pressure, and the need to add additives , needs light and other disadvantages
Therefore, there are still very limited systems that can really achieve high efficiency (high activity and high selectivity), environmental protection (no addition of alkaline additives), and stability (recycling of catalysts).

Method used

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  • Preparation and application of loaded Pd3Cl cluster catalyst
  • Preparation and application of loaded Pd3Cl cluster catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1: Pd 3 Oxidation of Benzyl Alcohol Catalyzed by Cl@TNT in n-Hexane Solution

[0031] Add 0.5mmol benzyl alcohol and 30mg catalyst Pd to a 10mL Schlenk reaction flask 3 Cl@TNT (Pd load is 1.5wt%) and 1mL n-hexane, and the reaction bottle is sealed, vacuumed and connected to an oxygen balloon to make it at 1atm O 2 atmosphere, and reacted at room temperature for 26 hours; after the reaction, the reaction solution was detected by gas chromatography, and the conversion rate of the target product benzaldehyde was 83.8%, and the selectivity was 85.4%.

Embodiment 2

[0032] Example 2: Pd 3 Oxidation of Benzyl Alcohol Catalyzed by Cl@TNT in Ethanol Solution

[0033] Add 0.5mmol benzyl alcohol and 30mg catalyst Pd to a 10mL Schlenk reaction flask 3 Cl@TNT (Pd load is 1.5wt%) and 1mL ethanol, and the reaction bottle is sealed, vacuumed and connected to an oxygen balloon to make it at 1atm O 2 After the reaction, the reaction solution was detected by gas chromatography, and the conversion rate of the target product benzaldehyde was 95.7%, and the selectivity was 98.5%.

Embodiment 3

[0034] Example 3: Pd 3 Oxidation of Benzyl Alcohol Catalyzed by Cl@TNT in Toluene Solution

[0035] Into a 10mL Schlenk reaction flask, add 0.5mmol benzyl alcohol, catalyst 30mg Pd 3 Cl@TNT (Pd load is 1.5wt%) and 1mL ethanol, and the reaction bottle is sealed, vacuumed and connected to an oxygen balloon to make it at 1atm O 2 atmosphere, and reacted at room temperature for 26 hours; after the reaction, the reaction solution was detected by gas chromatography, and the conversion rate of the target product benzaldehyde was 99.3%, and the selectivity was 100%.

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Abstract

The invention discloses a preparation and application of a loaded Pd3Cl cluster catalyst. The molecular formula of a Pd3Cl cluster is: [Pd3Cl(PPh2)2(PPh3)3]<+>, and the catalyst is recorded briefly as Pd3Cl@TNT. The loaded Pd3Cl cluster catalyst is prepared by loading the Pd3Cl cluster on a TNT (Trinitrotoluol) carrier. The catalyst Pd3Cl@TNT disclosed by the invention is capable of catalyzing primary (secondary) alcohol oxidation with high activity under an oxygen (normal pressure) condition, and corresponding aldehyde (ketone) can be correspondingly prepared with high selectivity. Reaction conditions are gentle, no catalyst or additive is needed, a small amount of the catalyst is used, a substrate application range is relatively wide, and meanwhile the catalyst can be recycled and reused for more than five times and has very good practicability.

Description

technical field [0001] The present invention relates to a heterogeneous catalyst, specifically a supported Pd 3 Preparation and application of Cl cluster catalysts. Background technique [0002] Oxidation of alcohols has always attracted much attention, because the corresponding oxidation products such as aldehydes, ketones or carboxylic acids are important raw materials for the production of high value-added products such as pharmaceuticals, vitamins and fragrances. The selective oxidation reaction from alcohols to aldehydes and ketones is one of the important reactions in organic reactions. The traditional oxidizing agents required for this type of reaction are chromates or dimethyl sulfoxide, which lead to the generation of a large number of toxic by-products while oxidizing alcohols. However, using air or oxygen as the oxidant, the by-product of oxidizing alcohol is only water, is considered to be an environmentally friendly and atom-economical process, which can reduc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/135B01J27/13C07C45/38C07C47/54C07C47/55C07C47/542C07C47/232C07C47/228C07C49/786C07C47/575C07C201/12C07C205/44C07D307/48
CPCB01J27/13B01J27/135C07C45/38C07C47/228C07C47/232C07C47/54C07C47/542C07C47/55C07C47/575C07C49/786C07C201/12C07C205/44C07D307/48Y02P20/584
Inventor 盛鸿婷貟亚培包琳泉朱满洲
Owner ANHUI UNIVERSITY
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