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Pd/UiO-66-NH2 material having high stability as well as preparation method and application of Pd/UiO-66-NH2 material

A uio-66-nh2 high-stability technology, applied in the direction of separation methods, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., can solve the problems of noble metal nanoparticles that are prone to agglomeration, expensive, Inhibit development and other problems, achieve good catalytic effect, long service life, good thermal stability and chemical stability

Inactive Publication Date: 2016-02-03
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Noble metals such as Pt, Pd, and Au have good catalytic effects, but noble metal nanoparticles are prone to agglomeration, and there are disadvantages such as high price and difficult separation, which inhibit their further development.

Method used

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  • Pd/UiO-66-NH2 material having high stability as well as preparation method and application of Pd/UiO-66-NH2 material
  • Pd/UiO-66-NH2 material having high stability as well as preparation method and application of Pd/UiO-66-NH2 material
  • Pd/UiO-66-NH2 material having high stability as well as preparation method and application of Pd/UiO-66-NH2 material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 10

[0033] Embodiment 10.3%Pd / UiO-66-NH 2 preparation of

[0034] 1) UiO-66-NH 2 Preparation: Weigh 0.0706g of 5-aminoterephthalic acid and 0.0261g of zirconium chloride, dissolve them in 5ml of N, N dimethylformamide, conduct a hydrothermal reaction at 120°C for 2880min, filter, wash, and vacuum-dry to obtain UiO- 66-NH 2 ;

[0035] 2) 0.3%Pd / UiO-66-NH 2 Preparation Weigh 0.1g of the UiO-66-NH obtained in Example 1 2 Ultrasonic dissolved in 8ml DMF solution, at the same time, measure 1.12mg of Pd(acac) 2 DMF solution was added dropwise to the above solution, at room temperature, ultrasonicated for 1h, then transferred to a 25ml round bottom flask and stirred for 4h, so that Pd ions could be fully adsorbed and evenly dispersed in UiO-66-NH 2 Carrier surface, freshly prepared NaBH 4 The solution was slowly added dropwise to the above mixed solution, and the Pd 2+ It is reduced to Pd atoms. In this process, it can be seen that the color of the solution changes from yellow to...

Embodiment 20

[0040] Embodiment 20.5%Pd / UiO-66-NH 2 preparation of

[0041] Weigh 0.1gUiO-66-NH 2 Ultrasonic dissolved in 8ml DMF solution, at the same time, measure 1.88mg of Pd(acac) 2 DMF solution was added dropwise to the above solution, and at room temperature, ultrasonicated for 1 hour, then transferred to a 25ml round bottom flask and stirred for 4 hours, so that Pd ions could be fully adsorbed and evenly dispersed on the surface of the carrier. Freshly prepared NaBH 4 The solution was slowly added dropwise to the above mixed solution, and the Pd 2+ It is reduced to Pd atoms. In this process, it can be seen that the color of the solution changes from yellow to black. After half an hour of aging, the Pd 2+ After complete reduction, filter in a sand core funnel, wash the filter cake three times with DMF, and then wash three times with ether to replace the DMF molecules in the MOF pores, dry the filter cake under vacuum at 80°C for 4 hours, 0.5%Pd / UiO-66-NH to get the powder 2 . ...

Embodiment 31

[0043] Example 31.0%Pd / UiO-66-NH 2 preparation of

[0044] Weigh 0.1gUiO-66-NH 2 Ultrasonic dissolved in 8ml DMF solution, at the same time, measure 3.77mg of Pd(acac) 2 DMF solution was added dropwise to the above solution, and at room temperature, ultrasonicated for 1 hour, then transferred to a 25ml round bottom flask and stirred for 4 hours, so that Pd ions could be fully adsorbed and evenly dispersed on the surface of the carrier. Freshly prepared NaBH 4 The solution was slowly added dropwise to the above mixed solution, and the Pd 2+ It is reduced to Pd atoms. In this process, it can be seen that the color of the solution changes from yellow to black. After half an hour of aging, the Pd 2+ After complete reduction, filter in a sand core funnel, wash the filter cake three times with DMF, and then wash three times with ether to replace the DMF molecules in the MOF pores, dry the filter cake under vacuum at 80°C for 4 hours, 1.0%Pd / UiO-66-NH to get the powder 2 .

[...

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Abstract

The invention relates to a Pd / UiO-66-NH2 material having the high stability as well as a preparation method and application of the Pd / UiO-66-NH2 material. According to the Pd / UiO-66-NH2 material, a carrier is a Zr6O32 secondary structure unit and has a carrier molecular formula being [Zr6O4(OH)4(O2C-C6NH3-CO2)6], and loaded noble metal is Pd. The preparation method is as follows: weighing UiO-66-NH2 and Pd(acac), performing ultrasonic dissolving on UiO-66-NH2 and Pd(acac) in a DMF solution, simultaneously dropwise adding a Pd(acac)2DMF solution in a UiO-66-NH2 solution, mixing, performing ultrasound operation to obtain a mixed solution, transferring the mixed solution into a round-bottom flask for stirring, dropwise adding NaBH4 solution for reducing, stirring, filtering, washing, and drying to obtain powder Pd / UiO-66-NH2. Pd / UiO-66-NH2 particles related in the invention are uniform in distribution, have the sizes of about 4nm, have a high-stability carbon monoxide oxidation performance, are high in stability and are reusable.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to a Pd / UiO-66-NH2 material with high stability, a preparation method and application thereof. Background technique [0002] In the past two decades, MOFs materials have attracted everyone's attention because of their special structures and potential applications in adsorption, separation, catalysis, luminescence, magnetism, and nonlinear optics. He also has a wide range of applications in homogeneous catalysis. Noble metals such as Pt, Pd, and Au have good catalytic effects, but noble metal nanoparticles are prone to agglomeration, and have disadvantages such as high price and difficult separation, which inhibit their further development. The microcrystalline and nanocrystalline structures of MOFs are very good carriers for immobilizing noble metal particles. [0003] XuQ reported that ZIF-8 supported Au nanoparticles catalyzed CO oxidation reaction, whic...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01D53/86B01D53/62
CPCY02A50/20
Inventor 王建国柏家奇庄桂林
Owner ZHEJIANG UNIV OF TECH
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