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Application of metal nanocluster catalyst in one-step preparation of acetal from alcohol

A technology of metal nano-clusters and catalysts, applied in the direction of metal/metal oxide/metal hydroxide catalysts, preparation of organic compounds, physical/chemical process catalysts, etc. The effect of less product and simple preparation method

Active Publication Date: 2021-06-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, the application of metal nanoclusters in the one-step preparation of acetals from alcohols has not been reported

Method used

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  • Application of metal nanocluster catalyst in one-step preparation of acetal from alcohol
  • Application of metal nanocluster catalyst in one-step preparation of acetal from alcohol
  • Application of metal nanocluster catalyst in one-step preparation of acetal from alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 50mg of HAuCl 4 . 4H 2 O mix K 2 PtCl 4 Dissolved in 20 mL of dichloromethane (HAuCl 4 . 4H 2 O and K 2 PtCl 4 The molar ratio of sodium borohydride is 0.125:1), add the thiol ligand in the ratio of 5:1 and stir at room temperature for 30 minutes, then dissolve 10 mg of sodium borohydride in 1 mL of 4 ℃ water, add the above solution to reduce, and precipitate slowly. Slowly turned brown, indicating the formation of AuPt alloy nanoparticles. After the reaction was carried out for 1-5 days, the absorption peak of the product was characterized by UV-Vis absorption spectrum, which proved that AuPt nanoclusters were formed. Finally, the alloy nanoclusters were purified, and the product dissolved in dichloromethane was spin-dried, then washed with methanol three times, extracted with methylene chloride, and finally spin-dried. 50 mg of alloy nanoclusters were dissolved in 20 mL of dichloromethane, and 500 mg of Al was added 2 O 3 The carrier was centrifuged to dry...

Embodiment 2～4

[0027] The experimental method and procedure are the same as in Example 1, and methylal is prepared by catalytic oxidation of methanol with different catalysts. The substrate was 10 mL of methanol, put into the reaction kettle, and then filled with oxygen, the reaction pressure was reduced to 1.5 MPa, and the reaction temperature was 80 °C, and the reaction started. The reaction was stopped after stirring for a period of time. After the temperature dropped to room temperature, the product was taken out, and the results were analyzed by GC-MS after centrifugal filtration. The specific results are shown in Table 1. Then select the AuPt / Al with the best catalytic activity 2 O 3 Alloy nanoclusters as catalysts to catalyze the oxidation of methanol to methylal. The selectivity and conversion of methanol catalytic oxidation to methylal at different temperatures and different reaction times were investigated. For specific results, see figure 1 .

Embodiment 5

[0029] 50mg of HAuCl 4 . 4H 2 O mixed AgNO 3 Dissolved in 20 mL of dichloromethane (HAuCl 4 . 4H 2 O and AgNO 3 The molar ratio of sodium borohydride is 0.125:1), add the thiol ligand in the ratio of 5:1 and stir at room temperature for 30 minutes, then dissolve 10 mg of sodium borohydride in 1 mL of 4 ℃ water, add the above solution to reduce, and precipitate slowly. Slowly turned brown, indicating the formation of AuAg alloy nanoparticles. After the reaction was carried out for 1-5 days, the absorption peak of the product was characterized by UV-Vis absorption spectrum, which proved that AuAg nanoclusters were formed. Finally, the alloy nanoclusters were purified, and the product dissolved in dichloromethane was spin-dried, then washed three times with methanol, extracted with dichloromethane, and finally spin-dried. 50 mg of alloy nanoclusters were dissolved in 20 mL of dichloromethane, and 500 mg of TiO was added 2The carrier was centrifuged to dry after 4 hours o...

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Abstract

The invention provides application of a metal nanocluster catalyst in one-step preparation of acetal from alcohol. The method comprises the following steps: under a solvent-free condition, selecting a M (M = Cu, Au, Pt, Pd and Ag) metal nanocluster catalyst with accurate atomic number, smaller size (< 0.05) and high dispersity (M = 2nm) as a catalytic oxidation active center, loading the metal nanocluster on a carrier to serve as a catalyst, taking oxygen or air as an oxidizing agent, and oxidizing alcohol by a one-step method to prepare the acetal, wherein the mass ratio of the loaded metal element to the catalyst is 0.05-5.00%. The method is simple and convenient in reaction operation, high in catalyst conversion rate and good in selectivity, does not need to add organic solvents and acid-base additives, is environment-friendly, and has high practicability and economy.

Description

technical field [0001] The invention belongs to the field of metal nano-cluster synthesis, in particular to the application of a metal nano-cluster catalyst in the preparation of acetal by an alcohol one-step method. Background technique [0002] As an important part of organic reaction, alcohol oxidation reaction has attracted people's attention. The product acetal produced by it is widely used in many fields. Acetal is an important chemical product with a wide range of uses and can be used as fuel additive , food additives and perfume cosmetics raw materials, etc., as diesel additives can increase the cetane number of diesel. Therefore, it is very important to seek a simple and environmentally friendly method to prepare acetal by one-step catalytic oxidative dehydrogenation, and it has important basic research significance and practical value. [0003] At present, there are usually two methods for the preparation of acetals by oxidative dehydrogenation of alcohols. The fi...

Claims

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Application Information

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IPC IPC(8): B01J23/52B01J23/89B01J35/00C07C41/50C07C43/303
CPCB01J23/52B01J23/8926C07C41/50B01J35/391B01J35/394C07C43/303
Inventor 黄家辉刘超任秀清杨洋
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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