Supported nano Pd/MgO catalyst and method of preparing biphenyl compound from catalyst

A catalyst and supported technology, applied in the direction of physical/chemical process catalysts, hydrocarbons, hydrocarbons, etc., can solve the problems of difficult product separation, air and water sensitivity, etc., and achieve low price, reduced reaction time, and environmental friendliness Effect

Pending Publication Date: 2019-10-15
WUHAN UNIV OF TECH
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Problems solved by technology

For a long time, the catalyst of the Suzuki coupling reaction is mainly homogeneous palladium catalyst, but the homogeneous palladi

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  • Supported nano Pd/MgO catalyst and method of preparing biphenyl compound from catalyst

Examples

Experimental program
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Example Embodiment

[0016] Example 1

[0017] This embodiment provides a Pd / MgO catalyst (hereinafter referred to as Pd / MgO catalyst) used in the Suzuki coupling reaction. The catalyst is composed of a nano-magnesium oxide carrier and an active component supported on the nano-magnesium oxide carrier. It is divided into palladium; the mass percentage of palladium in the catalyst is 3%; the preparation method of the catalyst in this embodiment includes the following steps:

[0018] Step 1: Weigh 0.06g of palladium chloride and place it in a round bottom flask, then weigh 0.04g of sodium chloride and place it in the flask, and add 5ml of distilled water. Stir continuously at room temperature for 5 hours, and dissolve palladium chloride to prepare sodium chloropalladate solution.

[0019] Step 2: Weigh 1g of nano-magnesium oxide (specific surface area is 600m 2 / g) Add the sodium chloropalladate solution described in step 1. Stir at room temperature for 1 h until mixed.

[0020] Step 3: Measure 0.15 g of t...

Example Embodiment

[0023] Example 2

[0024] In the three-necked flask connected with the condenser, 1mmol bromobenzene, 1.1mmol phenylboronic acid, 2mmol potassium carbonate, 0.0003mmol Pd / MgO catalyst based on palladium element, and 3ml water were added. The reaction was carried out at a reaction temperature of 85°C for 25 minutes. After the reaction, samples were taken for HPLC analysis. The bromobenzene conversion rate was 84%, and the product biphenyl was obtained.

Example Embodiment

[0025] Example 3

[0026] In a three-necked flask connected to the condenser, 1mmol bromobenzene, 1.1mmol phenylboronic acid, 2mmol potassium carbonate, 0.5mmol tetrabutylammonium bromide, 0.0003mmol Pd / MgO catalyst based on palladium element, 3ml water were added. The reaction temperature was 85° C. for 25 min. After the reaction, samples were taken for HPLC analysis. The bromobenzene conversion rate was 99%, and the product biphenyl was obtained.

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Abstract

The invention discloses a supported nano Pd/MgO catalyst which comprises nano magnesium oxide as a carrier and palladium as an active component loaded on the carrier, wherein the content of the palladium is 3-10% of total mass of the catalyst. A preparation method of the catalyst comprises the following steps: step I: preparing a palladium-containing aqueous solution, step II: adding nano magnesium oxide into the palladium-containing aqueous solution prepared in the step I, and performing continuous stirring for 1-5h at room temperature, and step III: adding a reducer into a solution preparedin the step II for reduction treatment, reducing divalent palladium in soluble palladium salt to zero-valent palladium, performing filtration to form a filter cake and performing water washing to formthe supported nano Pd/MgO catalyst. The invention provides a method of preparing a biphenyl compound by applying the nano Pd/MgO catalyst into a Suzuki coupling reaction at the same time. The catalyst has the advantages of low possibility of losing metal Pd in the catalyst, recyclability, high catalytic reaction activity, short reaction time and the like.

Description

technical field [0001] The invention relates to a Pd / MgO catalyst, in particular to a supported nanometer Pd / MgO catalyst and a method for preparing biphenyl compounds using the catalyst. Background technique [0002] Since Miyaura et al. reported in 1979 that under the catalysis of palladium, the coupling reaction of organoboron compounds and halogenated hydrocarbons under mild conditions to prepare asymmetric biaryls, the Suzuki coupling reaction has formed a new era in the selective construction of carbon-carbon bonds. a new field of research. The basic principle of Suzuki coupling reaction is that carbon-carbon bond coupling can transform simple molecules into complex molecules. Taking the reaction of bromobenzene and phenylboronic acid as an example, the reaction formula is as follows: [0003] [0004] Suzuki coupling reaction occupies an extremely important position in chemical synthesis. This key step is involved in the synthesis of many organic chemicals such a...

Claims

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Application Information

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IPC IPC(8): B01J23/58C07C1/32C07C15/14
CPCB01J23/58C07C1/321C07C15/14Y02P20/584
Inventor 陈建张茂生庞冲朱梦惊项扶委
Owner WUHAN UNIV OF TECH
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