Synthesis and characterization of Ni0 NPs immobilized on acid activated montmorillonite (Ni{\deg}-Mont) as an efficient and reusable heterogeneous catalyst for one-pot synthesis of biscoumarins under microwave irradiation

TL;DR

This study reports the synthesis of Ni nanoparticles immobilized on acid-activated montmorillonite, serving as an efficient, reusable catalyst for one-pot biscoumarin synthesis under microwave irradiation, with high yields and multiple reuses.

Contribution

It introduces a novel Ni nanoparticle-immobilized montmorillonite catalyst for efficient microwave-assisted biscoumarin synthesis, demonstrating high activity and reusability.

Findings

Ni nanoparticles were successfully immobilized with an average size of 10-20 nm.

The catalyst achieved 85-95% yields in biscoumarin synthesis.

The catalyst was reusable at least seven times without significant activity loss.

Abstract

The present paper describes in situ preparation of Ni{\deg} nanoparticles immobilized on acid activated montmorillonite K10 (Ni{\deg}-Mont) by impregnation of Ni(OAc)2 into nanopores of acid activated montmorillonite K10 followed by polyol reduction. Ni{\deg} NPs was highly dispersed into the initiated mesopores on the surface or inside swelled-interlayers of the examined clay with average size of 10-20 nm. Acid treatment of montmorillonite was carried out with HCl (4 M) under controlled conditions for generation of the desired pore sizes as a host of Ni{\deg} NPs. The prepared Ni{\deg}-Mont was used as a highly efficient heterogeneous catalyst for one-pot synthesis of biscoumarins in 85-95% yields. The reactions were carried out via Knoevenagel condensation of aromatic aldehydes with 4-hydroxycoumarin under microwave irradiation. The Ni{\deg}-Mont catalyst was reused at least for seven times without significant loss of its catalytic activity.