In situ preparation of highly dispersed Pd supported on exfoliated layered double hydroxides via nitrogen plasma for 4-nitrophenol reduction.

Abstract

In this work, a simple and environmental-friendly nitrogen glow discharge plasma reduction method has been developed for synthesizing palladium nanoparticles (PdNPs) supported on exfoliated Mg-Al-layered double hydroxide (Pd/LDH) catalysts. The as-prepared catalysts were characterized by means of characterizations methods, which contain X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectrometry (XPS), and Fourier transform infrared (FT-IR). Highly dispersed ultrafine PdNPs were supported on exfoliated, defect-induced LDHs uniformly without agglomeration. The effects of treatment time of nitrogen plasma and Pd loading amount on structure, morphology, and catalytic performance of Pd/LDHs were investigated. The comparisons of structure and morphology between LDHs and Pd/LDHs were also discussed. The average particle size of as-synthesized PdNPs with face-centered cubic structure is 2.01 nm, which ranges from 1.18 to 3.01 nm. Nitrogen plasma cannot only reduce Pd2+, but also exfoliate LDHs, introduce defects, and even destroy the structure of LDHs. The Pd/LDH catalyst with 1 wt% Pd loading under nitrogen plasma treatment for 60 min showed the best catalytic performance in 4-nitrophenol reduction. The turnover frequency (TOF) of as-prepared catalyst is 20-fold higher than that of commercial Pd/C catalyst.