Single-step fabrication of Na-TUD-1 novel heterogeneous base nano-catalyst for Knoevenagel condensation reaction

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ORIGINAL RESEARCH

Single‑step fabrication of Na‑TUD‑1 novel heterogeneous base nano‑catalyst for Knoevenagel condensation reaction Badria M. Al‑Shehri1,2 · Mohamed R. Shabaan2 · Mohd. Shkir3   · Ajeet Kaushik4   · Mohamed S. Hamdy1  Received: 18 July 2020 / Accepted: 27 October 2020 © Islamic Azad University 2020

Abstract This research, for the first time, reports the design and development of a heterogeneous nano-catalyst based on sodium ions ­(Na+) incorporation in Technical University of Delft (TUD-1) mesoporous silica for Knoevenagel condensation reaction. Facile one-step fabrication of Na-TUD-1 nano-catalysts (varying Si/Na ratio as 100–5) was demonstrated using the sol–gel route. The catalytic performance of Na-TUD-1 was evaluated as a base heterogeneous catalyst in Knoevenagel condensation reaction, which took place under conventional and microwave irradiations conditions using ethanol as a solvent. Na-TUD-1 exhibited superior catalytic activity in comparison to available homogeneous base catalysts such as sodium ethoxide. The Na-TUD-1 nano-catalyst demonstrated identical performance till the fourth run along with high stability and negligible leaching of Na. Moreover, the use of microwave heating reduced the reaction time from 240 to 20 min only with a TOF of 0.58 min−1. Such excellent performance of Na-TUD-1 heterogeneous nano-catalysts will certainly increase its industrial acceptability to achieve affordable and efficient waste-effluent treatments. Keywords  Na-TUD-1 · Knoevenagel condensation · Microwave · Conventional heating · Base catalyst

Introduction Knoevenagel condensation is one of the most important organic reactions for C–C bond formation [1–3]. This type of reaction is normally performed in the company of a base catalyst at elevated temperature [4–6]. Highly-efficient homogeneous base catalysts [1–6] have been used to catalyze

* Ajeet Kaushik [email protected] * Mohamed S. Hamdy [email protected] 1



Catalysis Research Group (CRG), Department of Chemistry, College of Science, King Khalid University, P.O. Box 9004, Abha 61413, Saudi Arabia

2



Chemistry Department, College of Science, Umm Al-Qura University, Makkah, Saudi Arabia

3

Advanced Functional Materials and Optoelectronics Laboratory (AFMOL), Department of Physics, College of Science, King Khalid University, Abha 61413, Saudi Arabia

4

NanoBioTech Laboratory, Department of Natural Sciences, Division of Sciences, Art and Mathematics, Florida Polytechnic University, Lakeland, FL 33805, USA





Knoevenagel reaction either in existence of common organic solvents or solvent-free environments [3, 4]. However, the use of homogeneous catalysts is always associate with some problems such as the difficulties in separation, recycling, products contaminations, and more seriously possible corrosion in the reactor vessel and the other environmental problems [7, 8]. Therefore, the replacement of homogeneous catalyst with an active and stable heterogeneous catalyst can overcome above-mentioned difficulties. Functionalized zeolit