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High-activity hydrotalcite loaded gold nanocluster catalyst and preparation method thereof

A gold nanocluster and hydrotalcite technology, applied in the field of highly active hydrotalcite-supported gold nanocluster catalyst and its preparation

Inactive Publication Date: 2015-04-15
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there has been no report on hydrotalcite as a carrier supporting Au nanocatalysts with a particle size of less than 2 nm for the selective oxidation of alcohols

Method used

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  • High-activity hydrotalcite loaded gold nanocluster catalyst and preparation method thereof
  • High-activity hydrotalcite loaded gold nanocluster catalyst and preparation method thereof
  • High-activity hydrotalcite loaded gold nanocluster catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of AuNCs-SG

[0028] Weigh 1.0g of HAuCl 4 4H 2 0 into 50 mL tetrahydrofuran, configure to obtain 20 mg / mL chloroauric acid tetrahydrofuran solution, measure the above solution 3.1 ml to a 25 ml three-necked flask, cool to 0 o C for 30 minutes. Slowly add 224 mg of glutathione (HSG) with 5 times the molar amount of Au into the three-necked flask; the stirring speed is 100 rpm. The solution turned from yellow to orange after one hour. After 10 hours, the stirring rate was adjusted to 1200 rpm, NaBH 4 Aqueous solution (10 times the molar amount of Au, 54 mg NaBH 4 dissolved in 3.0 mL of ice water) added quickly. At this time, the solution turned black, and a large amount of bubbles came out. After the reaction was carried out for 3 hours, the solution returned to room temperature. The solution was aged for 24 hours. Remove the THF in the upper layer, the volume ratio V of methanol and water is used for precipitation 甲醇 / V 水 =5 wash five times. t...

Embodiment 2

[0036] (1) Preparation of AuNCs-Capt

[0037] Weigh 1.0g of HAuCl 4 4H 2 0 into 50 mL tetrahydrofuran, configure to obtain 20 mg / mL chloroauric acid tetrahydrofuran solution, measure the above solution 3.1 ml to a 25 ml three-necked flask, cool to 0 o C for 30 minutes. 158 mg of captopril (Capt) with 5 times the molar amount of Au was slowly added into the three-neck flask; the stirring speed was 100 rpm. The solution turned from yellow to orange after one hour. After 10 hours, the stirring rate was adjusted to 1200 rpm, NaBH 4 Aqueous solution (10 times the molar amount of Au, 54 mg NaBH 4 dissolved in 3.0 mL of ice water) added quickly. At this time, the solution turned black, and a large amount of bubbles came out. After the reaction was carried out for 3 hours, the solution returned to room temperature. The solution was aged for 24 h. Remove the tetrahydrofuran in the upper layer, and the precipitation uses methanol and water volume ratio V 甲醇 / V 水 =5 wash five t...

Embodiment 3

[0045] (1) Preparation of AuNCs-SG

[0046] Weigh 1.0g of HAuCl 4 4H 2 0 into 50 mL tetrahydrofuran, configure to obtain 20 mg / mL chloroauric acid tetrahydrofuran solution, measure the above solution 3.1 ml to a 25 ml three-necked flask, cool to 0 o C for 30 minutes. Slowly add 224 mg of glutathione (HSG) with 5 times the molar amount of Au into the three-necked flask; the stirring speed is 100 rpm. The solution turned from yellow to orange after one hour. After 10 hours, the stirring rate was adjusted to 1200 rpm, NaBH 4 Aqueous solution (10 times the molar amount of Au, 54 mg NaBH 4 dissolved in 3.0 mL of ice water) added quickly. At this time, the solution turned black, and a large amount of bubbles emerged. After the reaction was carried out for 3 hours, the ice bath was removed, and the solution returned to room temperature. The solution was aged for 24 h. Remove the tetrahydrofuran in the upper layer, and the precipitation uses methanol and water volume ratio V ...

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Abstract

The invention relates to a high-activity hydrotalcite loaded gold nanocluster catalyst and a preparation method thereof, and belongs to the technical field of catalysts. The catalyst has a chemical formula: AuNCs / (M<2+>)(M<3+>)-LDH, wherein the AuNCs is a gold nanocluster, and the (M<2+>)(M<3+>)-LDH is hydrotalcite. The hydrotalcite has the structural formula: [(M<2+>)1-x(M<3+>)x(OH)<2>]<x+>(A<n->)x / n.mH2O), wherein the M<2+> is any one or two of Mg<2+>, Ni<2+> and Cu<2+> which are divalent metal ions, M<3+> is any one of Fe<3+>, Cr<3+> and Al<3+> which are trivalent metal ions, x ranges between 0.2 and 0.33, A<n-> is one of CO3<2->, NO<3->, Cl<-> and SO4<2-> which are anions, and m is the number of carried interlayer water. The AuNCs-SR serves as a precursor, the carboxyl on the AuNCs-SR as a ligand interacts with a laminate with positive charges on the (M<2+>)(M<3+>)-LDHm, AuNCs-SR is connected to the (M<2+>)(M<3+>)-LDHm in an anchoring way, and the ligand is removed by calcinating to obtain the catalyst with the chemical formula of AuNCs / (M<2+>)(M<3+>)-LDH. The catalyst has intrinsic alkalinity and hereby has excellent activity in the selective catalytic oxidation reaction of alcohol by selective catalysis under the alkaline-additive free condition.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular provides a highly active hydrotalcite-supported gold nano-cluster catalyst and a preparation method thereof. technical background [0002] In synthetic chemistry, the selective oxidation of alcohols is a very important catalytic conversion process because the corresponding aldehydes and ketones produced are of particular importance in the production of flavors, perfumes and bioactive substances. Traditionally, alcohols have been oxidized to the corresponding aldehydes and ketones with a large amount of toxic and expensive oxidants such as permanganate and hypochlorite. Therefore, using oxygen as a green oxidant to catalyze the oxidation of alcohols using reusable heterogeneous catalysts has become a desirable method. [0003] Recently, since supported Au catalysts in NaOH or K 2 CO 3 The unprecedented catalytic activity in the liquid phase aerobic selective oxidation of alc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/232C07C49/78C07C45/39
Inventor 张慧李论
Owner BEIJING UNIV OF CHEM TECH
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