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Ag/UiO-66-NH2 composite material, and preparation method and application thereof

A uio-66-nh2, composite material technology, applied in catalyst activation/preparation, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of low conversion rate and inability to exhibit catalytic performance , the precious metal is not stable enough, etc., to achieve the effect of simple synthesis method and good reuse ability

Active Publication Date: 2018-05-18
芜湖数字信息产业园有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the conversion rate of olefin epoxidation reaction is extremely low under the condition of no catalyst
[0003] In recent years, noble metal nanomaterials have become a research hotspot in the field of catalysis. Noble metals have a high catalytic effect for catalyzing the epoxidation of olefins, but the noble metals in the single state are not stable enough in the air state, and are very easy to agglomerate. In the catalytic reaction Does not exhibit very good catalytic performance

Method used

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  • Ag/UiO-66-NH2 composite material, and preparation method and application thereof
  • Ag/UiO-66-NH2 composite material, and preparation method and application thereof
  • Ag/UiO-66-NH2 composite material, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1Ag / UiO-66-NH 2 composite material

[0018] (1) Preparation method

[0019] 1. UiO-66-NH 2 Preparation of crystals: 298.4mg of zirconium chloride and 232mg of 2-aminoterephthalic acid were placed in a hydrothermal synthesis reactor, and 30.0mL of acetic acid and 120mL of N,N-dimethylformamide (DMF) were added at the same time, and ultrasonic treatment 20 minutes, then put the hydrothermal synthesis reactor into an oven, and react at 120°C for 24 hours. After the reaction, remove the liquid in the solution and wash it with N,N-dimethylformamide. Put the solid into a methanol solution, let it stand overnight at room temperature, filter, put the solid particles into a vacuum drying oven at 80°C and dry under vacuum.

[0020] 2. UiO-66-NH 2 Crystal activation: UiO-66-NH 2 Put the crystal into a vacuum drying oven at 120°C for 24 hours in vacuum to obtain activated UiO-66-NH 2 Crystals, stored under nitrogen.

[0021] 3. Weigh 300 mg of silver nitrate solid pa...

Embodiment 2

[0026] Example 2Ag / UiO-66-NH 2 Selective Catalysis of Composite Materials for Styrene Reaction

[0027] The method is as follows: 10mmol (1.14ml) styrene and 30mmol (2.873ml) tert-butyl hydroperoxide are dissolved in 5ml of acetonitrile solution to obtain a mixed solution; the 50mg Ag / UiO- prepared in Example 1 is added to the mixed solution respectively 66-NH 2 Put the composite material in a 20mL eggplant-shaped reaction bottle, connect the condensing device, fix the reaction device, first insert the long needle below the liquid surface, pass nitrogen gas for 10 minutes, and remove the oxygen contained in the solution, then pull out the needle to use The whole reactor is sealed. React at a temperature of 80°C. After reacting for 18 hours, take the reaction solution and monitor it by gas chromatography. The results are as follows: Figure 4 shown.

[0028] Figure 4 Ag / UiO-66-NH synthesized for the present invention 2 In the gas phase diagram of the product after 0h and...

Embodiment 3

[0030] Example 3Ag / UiO-66-NH 2 Composite material repeatability test

[0031] After the reaction of Example 2 is finished, the Ag / UiO-66-NH 2 Composite material, repeat the experiment of embodiment 2 4 times. Figure 5 Ag / UiO-66-NH synthesized for the present invention 2The gas phase diagram of the product after 0h and 18h ​​in the fifth catalyzed styrene oxidation reaction, through repeated experiments, Ag / UiO-66-NH reacted five times 2 The conversion rate of styrene in the composite material is 34.6%, and the selectivity of styrene oxide is 76.9%, which means that the material still has good catalytic activity and selectivity. Prove that the Ag / UiO-66-NH synthesized by the present invention 2 Composite materials have good recyclability.

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Abstract

The invention relates to an Ag / UiO-66-NH2 composite material, and a preparation method and an application thereof. According to a technical scheme of the invention, the preparation method comprises the following steps: slowly dropwise adding an acetonitrile solution of silver nitrate into a UiO-66-NH2 crystal so as to obtain Ag+ / UiO-66-NH2; and adding a saturated ethanol solution of sodium borohydride into the Ag+ / UiO-66-NH2 so as to obtain the Ag / UiO-66-NH2 composite material. The Ag / UiO-66-NH2 composite material synthesized by using the preparation method provided by the invention has highly-efficient catalytic activity to styrene in an epoxidation reaction.

Description

technical field [0001] The invention belongs to the field of precious metal catalyzed organic compound synthesis, and a novel metal-organic framework material (UiO-66-NH 2 ) as a carrier to load silver nanoparticles into it to form a new Ag / UiO-66-NH 2 Composite material capable of selectively generating styrene oxide. Background technique [0002] Epoxides contain a three-membered ring structure consisting of one oxygen atom and two carbon atoms. It is an important class of organic synthesis intermediates and chemical raw materials, which can generate a series of valuable compounds through selective ring opening or functional group transformation, and are widely used in fine chemicals, petrochemicals, pharmaceuticals, surfactants, high Molecular materials and electronics industry and other fields. However, the conversion rate of olefin epoxidation is extremely low under the condition of no catalyst. [0003] In recent years, noble metal nanomaterials have become a resea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J37/10B01J37/06C07D301/19C07D303/04
Inventor 韩正波李跃香
Owner 芜湖数字信息产业园有限公司
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