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Preparation method of polydopamine ball anchored Pd nanoparticle catalyst

A technology of polydopamine spheres and nanoparticles, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve problems such as complex preparation process, low reactivity, and poor catalyst stability, and achieve simplified preparation Process, improve catalytic performance, reduce the effect of preparation cost

Pending Publication Date: 2021-04-20
SOUTHWEST UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a simple and efficient preparation method of polydopamine sphere-anchored Pd nanoparticle catalyst, which mainly solves the problems of poor stability, low reactivity and complicated preparation process of traditional catalysts in the Heck reaction

Method used

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  • Preparation method of polydopamine ball anchored Pd nanoparticle catalyst
  • Preparation method of polydopamine ball anchored Pd nanoparticle catalyst
  • Preparation method of polydopamine ball anchored Pd nanoparticle catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The preparation of 1wt%-Pd / PDA-0h catalyst:

[0036] Measure 38mL absolute ethanol, 190mL 10mmol / L Tris solution, weigh 291mg DA and 0.4mL0.07035mol / L H 8 Cl 4 N 2 Pd solution was added into a 250mL beaker, stirred at 25°C for 24h, filtered with suction to obtain a black solid, and dried under vacuum at 60°C for 12h. sample at 200°C in H 2 / N 2 (1:1) mixed atmosphere reduction 1h, H 2 with N 2 The flow rate is 20mL / min. Named 1wt%-Pd / PDA-Oh.

Embodiment 2

[0038] The preparation of 3wt%-Pd / PDA-0h catalyst:

[0039] Measure 38mL absolute ethanol, 190mL 10mmol / L Tris solution, weigh 291mg DA and 1.2mL0.07035mol / L H 8 Cl 4 N 2 Pd solution was added into a 250mL beaker, stirred at 25°C for 24h, filtered with suction to obtain a black solid, and dried under vacuum at 60°C for 12h. sample at 200°C in H 2 / N 2 (1:1) mixed atmosphere reduction 1h, H 2 with N 2 The flow rate is 20mL / min. Named 3wt%-Pd / PDA-Oh.

Embodiment 3

[0041] The preparation of 5wt%-Pd / PDA-0h catalyst:

[0042] Measure 38mL absolute ethanol, 190mL 10mmol / L Tris solution, weigh 291mg DA and 2mL0.07035mol / L H 8 Cl4 N 2 Pd solution was added into a 250mL beaker, stirred at 25°C for 24h, filtered with suction to obtain a black solid, and dried under vacuum at 60°C for 12h. sample at 200°C in H 2 / N 2 (1:1) mixed atmosphere reduction 1h, H 2 with N 2 The flow rate is 20mL / min. Named 5wt%-Pd / PDA-Oh.

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Abstract

The invention discloses a polydopamine ball anchored Pd nanoparticle catalyst. Unsaturated nitrogen-containing functional group coordination bonds are formed by regulating the polymerization reaction time of DA, the interaction between a carrier and active center Pd nanoparticles is enhanced, and rich chemical groups on the surface of polydopamine provide stable adsorption sites for Pd. Polymerization of polydopamine and loading of Pd are carried out in one process, so that more sites are found in the dynamic deposition process of Pd nanoparticles, better dispersity and stability are achieved, the catalytic performance of the catalyst is improved, the stability of the catalyst is enhanced, a large number of nitrogen-containing and oxygen-containing functional groups in the synthesized catalyst and Pd form stable coordination bonds, and thus the loss and agglomeration of Pd nanoparticles are effectively inhibited, so that the cost of the catalyst is reduced, the problems of poor stability, low reaction activity and complex preparation process of the traditional catalyst in the Heck reaction are mainly solved, the catalyst is synthesized by a one-pot method, the preparation process is simplified, and the preparation cost is reduced.

Description

technical field [0001] The invention relates to the technical field of catalyst synthesis, in particular to a preparation method of a catalyst in which polydopamine spheres anchor Pd nanoparticles and its application in Heck reaction. Background technique [0002] The Heck reaction is one of the important synthetic reactions to form carbon-carbon double bonds. Since Heck and Morizoki independently discovered this reaction in the late 1960s, researchers have made it more and more widely used through continuous improvement of catalysts and reaction conditions. Such as synthetic pharmaceutical intermediates, spices, dyes and other fields. At present, noble metal Pd is the most efficient active center for catalyzing the Heck reaction. Traditionally, the Pd-based catalysts used in the Heck reaction are homogeneous catalysts containing phosphine ligands. Although this type of homogeneous Pd catalyst can promote the reaction, it is difficult to recover the catalyst after the reac...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J31/22B01J35/00C07B37/04C07C67/343C07C69/618
Inventor 冉茂飞罗正秀孙文晶代弢
Owner SOUTHWEST UNIVERSITY FOR NATIONALITIES
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