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Pd/UiO-66 catalyst having morphology-controllable Pd metal nanocrystal core and preparation method thereof

A technology of metal nanocrystals and catalysts, applied in the field of nanomaterials, can solve problems such as limiting the application of catalysts, and achieve significant research significance and value

Active Publication Date: 2018-03-13
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are few reports on the synthesis and preparation of metal / MOFs catalysts with metal nanoparticles with controllable morphology, which greatly limits the application of catalysts.

Method used

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  • Pd/UiO-66 catalyst having morphology-controllable Pd metal nanocrystal core and preparation method thereof
  • Pd/UiO-66 catalyst having morphology-controllable Pd metal nanocrystal core and preparation method thereof
  • Pd/UiO-66 catalyst having morphology-controllable Pd metal nanocrystal core and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1 A Pd / UiO-66 catalyst with spherical morphology Pd metal nanocrystal core I

[0035] A Pd / UiO-66 catalyst with a Pd metal nanocrystal core with spherical morphology, the preparation method of the Pd / UiO-66 catalyst is as follows:

[0036] (1) Weigh 37 mg of terephthalic acid (H 2 BDC), mixed with ultrasonic at room temperature and dissolved in 4 mL of N,N-dimethylformamide (DMF) to form solution A; weigh 10 mg of sodium chloropalladate (Na 2 PdCl 4 ), dissolved in 2 mL of N,N-dimethylformamide (DMF) at room temperature by ultrasonic mixing to form solution B; weigh 52 mg of zirconium tetrachloride (ZrCl 4 ), dissolved in 4 mL of N,N-dimethylformamide (DMF) by ultrasonic mixing at room temperature to form solution C;

[0037] (2) Mix solution B and solution A, stir for 5 min, add solution C to the above mixed solution at room temperature, and then add 1.2 mL of acetic acid to the mixed solution.

[0038] (3) The above mixed solution was sealed and stirred in...

Embodiment 2

[0039] Example 2 A Pd / UiO-66 catalyst with spherical morphology Pd metal nanocrystal core II

[0040] The preparation method of the catalyst provided in this example is the same as that in Example 1, except that in this example, in step (1), the amount of zirconium tetrachloride is 52 mg, and the amount of terephthalic acid is 37 mg. The amount of sodium chloropalladate was 10 mg; the temperature of the oil bath in step (3) was 115° C., and the stirring time was 22 hours.

Embodiment 3

[0041] Example 3 A Pd / UiO-66 Catalyst I with Tetrahedral Morphology and Pd Metal Nanocrystal Core

[0042] A Pd / UiO-66 catalyst with a Pd metal nanocrystal core with tetrahedral morphology, the preparation method of the Pd / UiO-66 catalyst is as follows:

[0043] (1) Weigh 37 mg of terephthalic acid (H 2 BDC), ultrasonically mixed and dissolved in 4 mL of N,N-dimethylformamide (DMF) at room temperature to form solution A; weigh 10 mg of palladium acetylacetonate (Pd(acac) 2 ), dissolved in 2 mL of N,N-dimethylformamide (DMF) at room temperature by ultrasonic mixing to form solution B; weigh 52 mg of zirconium tetrachloride (ZrCl 4 ), dissolved in 4 mL of N,N-dimethylformamide (DMF) by ultrasonic mixing at room temperature to form solution C;

[0044](2) Mix solution B and solution A, stir for 5 min, add solution C to the above mixed solution at room temperature, and then add 1.2 mL of acetic acid to the mixed solution.

[0045] (3) The above mixed solution was sealed and sti...

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Abstract

The invention relates to a Pd / UiO-66 catalyst having a morphology-controllable Pd metal nanocrystal core and a preparation method and application thereof. The preparation method of the Pd / UiO-66 catalyst comprises S1: dissolving terephthalic acid in dimethyl formamide to obtain a solution A, dissolving a palladium salt in dimethyl formamide to obtain a solution B and dissolving zirconium tetrachloride in dimethyl formamide to obtain a solution C for next use, S2: mixing the solutions A and B, carrying out stirring, mixing the mixture and the solution C and adding a small molecule acid into themixed solution, S3: sealing the mixed solution obtained by the step S2, carrying out heating along with stirring for 20-26h, after the reaction, carrying out centrifugation on the mixed solution andwashing and drying the centrifugal product to obtain the Pd / UiO-66 catalyst having a morphology-controllable Pd metal nanocrystal core. The Pd / UiO-66 catalyst obtained by the one step method has controllable Pd nanocrystal morphology and the morphology-controllable Pd nanoparticle is spherical or tetrahedral. The Pd / UiO-66 catalyst has a good UiO-66 crystalline state and a high specific surface area.

Description

technical field [0001] The invention relates to the field of nanomaterials, in particular, to a Pd / UiO-66 catalyst with a Pd metal nanocrystal core with a controllable morphology, and a preparation method and application thereof. Background technique [0002] Noble metal nanoparticles are widely used as catalysts due to their relatively small particle size, large specific surface area, and abundant coordinative unsaturated points and high surface activity. The unique chemical stability of noble metal materials makes it have unique catalytic stability, activity and regeneration after being made into nano-scale catalysts. The catalytic activity and selectivity of noble metal nanocrystal catalysts are largely affected by factors such as nanoparticle size, surface atomic species, and arrangement. Among them, the change of atomic arrangement is often characterized by the different morphology of nanocrystals. Therefore, in the process of synthesizing and preparing metal nanocrys...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07B31/00
CPCC07B31/00B01J31/1691B01J2231/641B01J2231/645B01J2531/48B01J35/391B01J35/396B01J35/393
Inventor 李光琴包士雄李满荣赵德鹏
Owner SUN YAT SEN UNIV
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