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Composite AuAgPd catalyst for hydrolysis and oxidation of alkynol and its preparation method

A technology of oxidation reaction and catalyst, applied in the direction of catalyst activation/preparation, preparation of organic compounds, metal/metal oxide/metal hydroxide catalyst, etc.

Active Publication Date: 2018-02-09
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The supported catalyst AuAgPd@HT has not been reported yet

Method used

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  • Composite AuAgPd catalyst for hydrolysis and oxidation of alkynol and its preparation method

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Embodiment 1

[0011] Embodiment one: a kind of composite AuAgPd catalyst and preparation method for acetylenic alcohol hydrolysis and oxidation reaction comprise the following process steps: (1) AuPPh 2 Preparation of MeCl: Add appropriate amount of HAuCl to a 50 mL round bottom flask 4 (412mg, 1.0mmol), followed by an appropriate amount of EtOH (6mL). Subsequent PPh 2 Me (400 mg, 2.0 mmol) was dissolved in 20 mL of EtOH at 60 °C, and slowly added to the above mixture. It was stirred at room temperature for 24 h, and a color change was observed. The crude product was filtered under reduced pressure. Finally, the solid was dissolved and diluted with 20 mL of dichloromethane, and recrystallized with 100 mL of petroleum ether to obtain a pure solid. (2) Preparation of Au nanoparticles: AuPPh 2 MeCl (432 mg, 1.0 mmol) and dodecanethiol (10 mL) were mixed in 100 mL of toluene and a clear solution was formed. t-BuOH (741 mg, 10 mmol) was added to the above solution. The mixture was stirred...

Embodiment 2

[0012] Example 2: Apply the obtained catalyst AuAgPd@HT in the synthesis of bisphenol F: add phenol (5mmol) and AuAgPd@HT (50mg) into the reaction vessel, add 20mL tetrahydrofuran, stir at room temperature, and slowly add 37% formaldehyde solution, stir evenly, then add a certain amount of 10% hydrochloric acid solution, and heat to 50°C. The reaction time was 12 hours. After the reaction, the obtained reaction solution was separated into layers, and the oil layer was the crude reaction product. At the same time, the composite catalyst AuAgPd@HT can be recovered by filtration. The obtained crude product is rotary evaporated to recover the solvent, and the remaining phenol is recovered by vacuum distillation to obtain 4,4 dihydroxydiphenylmethane.

Embodiment 3

[0013]Example 3: Apply the obtained catalyst AuAgPd@HT in the hydrolysis of acetylenic alcohol: add phenylalkynol (1 mmol) and AuAgPd@HT (50 mg) into the reaction vessel, add 10 mL of tetrahydrofuran, stir at room temperature for 10 minutes, and then add 1mL of water, then heated to react at 60°C. The reaction time was 12 hours. After the reaction, the product was obtained with a yield of 98%.

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Abstract

The invention discloses a novel supported multi-metal nano-catalyst AuAgPd@HT and application of the same to a synthesis process of bisphenol F and hydrolysis of alkynol. According to the invention, Au nanoparticles, Au@HT, AuAg@HT and AuAgPd@HT are separately prepared in steps. The novel supported multi-metal nano-catalyst provided by the invention has the advantages of high activity, recyclability and long service life. Therefore, the design and synthesis of the supported multi-metal nano-catalyst have good industrial application prospects.

Description

technical field [0001] The invention discloses a composite AuAgPd catalyst for hydrolysis and oxidation of acetylenic alcohols and a preparation method. Traditional single-metal catalysts have problems such as low catalytic performance, easy aggregation of metal particles, and difficulty in recycling. This problem can be solved by reducing metals to nanoparticles and loading them on carriers. This patent describes the reduction of multiple precious metals into nanoparticles and successfully supports them on hydrotalcite, and successfully prepares a new type of supported multi-metal catalyst with high efficiency, simple and easy recovery, and long service life. It belongs to the field of chemical materials and medicines. Background technique [0002] Metal catalysts mainly refer to solid catalysts with metals as the main active components. According to whether the active components of the catalyst are supported on the carrier, the catalyst can be divided into supported meta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/52C07C37/20C07C39/16C07C45/26C07C49/82
CPCC07C37/20C07C45/26B01J23/52B01J37/0248B01J37/16B01J35/393B01J35/23C07C39/16C07C49/82Y02P20/584
Inventor 王大伟叶冬冬夏晓峰冷炎黄荣辉
Owner JIANGNAN UNIV
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