MOFs-rGO supported Pd nano-catalyst as well as preparation and application thereof

A nano-catalyst, catalyst technology, applied in the field of catalysis, to achieve the effect of small particle size, good dispersion and stability, and simple preparation method

Active Publication Date: 2017-12-08
SHANTOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is a kind of Pd nano-catalyst supported by MOFs-rGO and preparation thereof, to solve existing problems

Method used

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  • MOFs-rGO supported Pd nano-catalyst as well as preparation and application thereof
  • MOFs-rGO supported Pd nano-catalyst as well as preparation and application thereof
  • MOFs-rGO supported Pd nano-catalyst as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] NH 2 - Preparation of MIL-101 (Cr): Weigh 800mg of chromium nitrate nonahydrate (2mmol), 360mg of 2-aminoterephthalic acid (2mmol) and 200mg of sodium hydroxide (5mmol), and add to 15mL of deionized water. Ultrasonic treatment at room temperature to make it evenly mixed, then transferred to a 50mL polytetrafluoro reactor, reacted at 160°C for 16h, cooled to room temperature, and filtered with a water-based filter membrane with a pore size of 0.22μm to obtain a grass-green solid . Finally, reflux the grass-green solid in 95% ethanol for 12 hours to wash away unreacted 2-aminoterephthalic acid to obtain NH 2 -MIL-101(Cr). The obtained solid powder was dried and activated in a vacuum oven at 100° C. for 12 hours before use.

[0029] NH 2 -MIL-101(Cr)-rGO-1, NH 2 -MIL-101(Cr)-rGO-2, NH 2 -The synthesis method of MIL-101(Cr)-rGO-3 and NH 2 - The synthesis method of MIL-101 (Cr) is the same. The difference is that 1%, 2% or 5% GO is added to the solution by mass rati...

Embodiment 2

[0031] Four kinds of carriers NH prepared in Example 1 2 -MIL-101(Cr), NH 2 -MIL-101(Cr)-rGO-1, NH 2 -MIL-101(Cr)-rGO-2, NH 2 -MIL-101(Cr)-rGO-3 prepared Pd nanoparticle-supported catalyst carrier, with Pd / NH 2 - The preparation of MIL-101 (Cr) is an example, the specific steps are as follows: Weigh 200 mg of activated solid powder NH 2 - MIL-101 (Cr), ultrasonically dispersed in 20 mL of water. During stirring, 1M HCl solution was added dropwise to the solution to acidify the NH 2 -MIL-101(Cr). After 10 min, 13 mL of 10 mmol of chloropalladium acid solution was added dropwise to the solution, and stirred at room temperature for 6 h. Then use a 0.22 μm pore size water-based filter membrane to carry out suction filtration, wash with 100ml of water and ethanol twice to neutrality, and obtain Pd 2+ / NH 2 - MIL-101 (Cr) solid. Pd 2+ / NH 2 - Disperse MIL-101(Cr) in 20mL water and stir evenly under ice bath. When the temperature of the solution dropped to 2-3° C., an exc...

Embodiment 3

[0033]

[0034] The catalyst prepared in Example 2 was used for the hydrodechlorination reaction of p-chlorophenol and o-chlorophenol. The specific steps are: use a pipette to measure p-chlorophenol or o-chlorophenol solution (18.36mg / mL, 1mmol) into a three-neck flask, dilute to 10mL, add 23mg of catalyst, ultrasonically disperse it, and stir for 10min. After that, 15 mmol of organic base was added to the reaction liquid, and the reaction was stirred under the condition of 30° C. water bath after ultrasonication for 1 min. The mixture was filtered with a needle filter with a pore size of 0.22 μm, and the filtrate was analyzed for its yield by liquid chromatography. The reaction substrates used and the corresponding yields are listed in Table 1. Under the same conditions, Pd / NH 2 -MIL-101(Cr)-rGO-2 and Pd / NH 2 -MIL-101(Cr)-rGO-3 has the best catalytic effect. To further explore the stability of the catalyst, after the reaction, Pd / NH 2 - The loss of Pd in ​​MIL-101(Cr)-...

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Abstract

The invention relates to a MOFs-rGO supported Pd nano-catalyst as well as preparation and application thereof. NH2-MIL-101(Cr)-rGO serves as a carrier, an active ingredient nano-Pd of the catalyst is encapsulated into a cage formed by the carrier, the weight percent of GO in the NH2-MIL-101(Cr)-rGO is 1-5%, and the capacity of the nano-Pd is 4-5wt%. By utilizing the structural characteristics of the MOFs cage, Pd<2+> supported MOFs-rGO is prepared by taking tetrachloroplatinate as a palladium source by utilizing an ion exchange method, and the MOFs-rGO supported Pd nano heterogeneous catalyst is prepared under the action of a NaBH4 reducing agent. Palladium nano-particles are mainly encapsulated in the MOFs-rGO cage, the adsorption performance and stability of the NH2-MIL-101(Cr)-rGO are improved by atomically closely packed rGO, the catalyst has small particle size and excellent dispersity and stability, and the catalytic performance is greatly improved. The catalyst is applied to a dechlorination reaction of parachlorophenol and o-chlorophenol and has high catalytic activity. Moreover, the preparation method of the catalyst disclosed by the invention is simple and easy to operate.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a MOFs-rGO supported Pd nanometer catalyst and its preparation and application. Background technique [0002] Metal organic frameworks or porous coordination polymers, or MOFs for short, are a new class of microporous crystal materials formed by the interaction of inorganic metal cations and organic bridging ligands through coordination bonds. The diversity of coordination modes between organic bridging ligands and metal ions or metal clusters determines the diversity of MOFs structures. More importantly, suitable metal ions and ligands can be selected according to needs to design and synthesize MOFs with specific structures and functions. MOFs have many excellent properties, such as ultra-high porosity (greater than 90%) and high specific surface area (the Langmuir area of ​​some MOFs is as high as 104m2g-1). MOFs have applications in the fields of gas adsorption ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28B01J37/03B01J37/30B01J37/16C07C39/04C07C37/00
CPCB01J31/28B01J35/0013B01J35/006B01J37/031B01J37/035B01J37/16B01J37/30B01J2531/0216B01J2531/62C07C37/00C07C39/04Y02P20/52
Inventor 鲁福身王海龙孟园胡全钦付钦瑞方子林
Owner SHANTOU UNIV
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