Mixed bio-based surfactant-templated mesoporous silica for supporting palladium catalyst

Abstract

The study aimed on the synthesis of bio-based surfactant-templated mesoporous silica for supporting palladium catalyst using mixed bio-based templating agents namely cashew nut shell liquid (CNSL) and castor oil for pore direction purposes. The materials prepared through co-condensation of 3-aminopropyltriethoxysilane (APTS) and tetraethyl orthosilicate (TEOS) in a 1:4 M ratio using 1:1, 4:1 and 9:1 ratio of CNSL and castor oil. The resulting porous materials were utilized to support the palladium(II) chloride catalyst, resulting in a heterogeneous catalyst-a better and more environmentally friendly catalyst than a homogeneous one. Different instruments were used to characterize the prepared materials such as nitrogen porosimeter, Powder X-ray Diffraction, Diffuse Reflectance Infrared Fourier Transform Spectroscopy and Inductively coupled plasma optical emission spectroscopy. Physisorption studies of the prepared materials indicated that the largest pore diameter of 43.84 nm could be obtained by using a 1:1 M ratio of CNSL and castor oil. On the other hand, the largest surface area of 209 m²/g was obtained from a 9:1 whereas the largest pore volume was 1.55 cm³/g from a 4:1. Diffuse Reflectance Infrared Fourier Transform Spectroscopy analysis confirmed the presence of N-H group, the bending vibration bands at around 1640 and 1543 cm^-1 indicating that the reaction of organoaminesilanes and tetraethyl orthosilicate had occurred. The palladium content of the supported catalyst was determined by ICP-OES which confirmed the attachment of palladium to the synthesized materials. The highest palladium loading was obtained from the adsorbent prepared by using 1:1 ratio of surfactants mixture which gave the adsorption value of 2.16 mmol/g. Powder X-ray Diffraction indicated that the synthesized organosilica materials are amorphous with improved crystallinity upon attachment of palladium catalyst. The incorporation of palladium in the synthesized materials using the mixed bio-based surfactant was successful.