Palladium nanoparticles (Pd‐NPs) were synthesized under green conditions in water by chemical reduction of PdCl2 with NaOH and supported by Fe3O4‐Lignin. Fe3O4‐Lignin is an organic–inorganic hybrid core‐shell was synthesized by sonication of a mixture of Fe3O4‐NPs (20 nm) and alkali lignin. The new materials Fe3O4‐Lignin and Fe3O4‐Lignin@Pd‐NPs were characterized by PXRD, SEM and FT‐IR spectroscopy. The Fe3O4‐Lignin@Pd‐NPs was further confirmed by UV–Visible spectroscopy, TEM, EDX, HRICP‐AES and TGA/DTA. The average size of Pd‐NPs determined from PXRD was 5–10 nm. The amount of palladium loaded on Fe3O4‐Lignin obtained from EDX analysis was 26.63% by mass. The amount of Fe and Pd present in the catalyst obtained from HRICP‐AES was 11.88 (wt. %) and 10.90 (wt. %) respectively per gram of lignin. The catalytic potential of Fe3O4‐Lignin@Pd‐NPs was evaluated in Mizoroki‐Heck C‐C coupling reaction. During the optimization studies of reaction between iodobenzene and n‐butyl acrylate in various solvents and under solvent‐free but aerobic conditions using various inorganic and organic bases, the product n‐butyl 3‐phenylprop‐2‐enoate (1a) obtained was as high as 95% in highly polar solvents as short as in 10 min and 99% under solvent‐free conditions in 3 min at 140 °C using n‐Pr3N as base. The scope of the above catalyst was investigated in the Mizoroki‐Heck reaction of various aryl/heterocyclic halides and n‐butyl acrylate/styrene under optimized solvent‐less conditions. The corresponding products were obtained in high yields (73–99%). The catalyst recovered by magnetic decantation was reused for five times in the C‐C coupling reaction between iodobenzene and n‐butyl acrylate which yielded 90–95% of the desired product, 1a.

Nickel nanoparticles were synthesized readily by sonication of a mixture of nickel(II) chloride hexahydrate, hydrazine hydrate, lignin and water at 60 °C. This lignin supported nickel nanoparticles (Lignin@Ni‐NPs) have been characterized by UV‐Visible, PXRD, EDX, SEM and TEM techniques. The average size of Ni‐NPs was found in the range of 15‐20 nm as revealed by TEM micrographs. The amount of nickel(0) loaded in Lignin@Ni‐NPs determined by EDX was 36.6 %. The catalytic activity of Lignin@Ni‐NPs have been evaluated in the transfer hydrogenation of carbonyl compounds into the corresponding alcohols. The catalyst have been found efficient for hydrogen‐transfer reduction of functionalised and non‐fuctionalised including heteroaromatic carbonyl compounds as the desired alcohols were obtained in high yields of about 90‐95 % at room temperature, under base‐free conditions and in short reaction times. The catalyst was recovered by simple filtration and it has an advantage of being reuable more than six times without significant loss in its catalytic activity.