6533b7d0fe1ef96bd125a414

RESEARCH PRODUCT

Design of PNIPAAM covalently grafted on halloysite nanotubes as a support for metal-based catalysts

Stefana MiliotoFilippo ParisiVincenzo CampiscianoV. SchembriGiuseppe LazzaraMarina MassaroGiuseppe CavallaroSerena RielaRenato Noto

subject

inorganic chemicalsMaterials scienceGeneral Chemical Engineeringchemistry.chemical_element02 engineering and technologyengineering.material010402 general chemistry01 natural sciencesHalloysiteLower critical solution temperatureNanomaterialsCatalysischemistry.chemical_compoundSuzuki reactionhalloysite PNIPAAM; microwave Suzuki reaction waterPolymer chemistryhalloysite PNIPAAMPhenylboronic acidSettore CHIM/02 - Chimica Fisicachemistry.chemical_classificationmicrowave Suzuki reaction waterSettore CHIM/06 - Chimica OrganicaGeneral ChemistryPolymer021001 nanoscience & nanotechnology0104 chemical scienceschemistryengineering0210 nano-technologyPalladiumNuclear chemistry

description

A thermo-responsive polymer such as poly(N-isopropylacrylamide) (PNIPAAM) was covalently grafted on the external surface of halloysite nanotubes (HNTs) by means of microwave irradiation. This nanomaterial was used as a support and stabilizer for palladium nanoparticles. The obtained HNT–PNIPAAM/PdNPs was characterized by means of TGA, SEM, EDS and TEM analyses. The palladium content of the catalyst was estimated to be 0.4 wt%. The stability of the catalytic material at different temperatures (below and above the PNIPAAM lower critical solution temperature) was tested in the Suzuki reaction under microwave irradiation. In addition, TEM analysis after five consecutive runs was performed. The catalyst showed a good catalytic activity toward the Suzuki cross-coupling reaction between phenylboronic acid and several aryl halides in aqueous media under microwave irradiation and low palladium loading (0.016 mol%, 8 mg of Pd). Turnover numbers (TONs) and frequencies (TOFs) up to 6250 and 37 500 h1, respectively, were reached. The catalyst was easily separated from the reaction mixture by centrifugation and reused for five consecutive cycles with a small drop in its catalytic activity.

https://doi.org/10.1039/c6ra06337c