Revisiting hydrotalcite synthesis: Efficient combined mechanochemical/coprecipitation synthesis to design advanced tunable basic catalysts

Author:

Nope Eliana12,Sathicq Ángel G.2,Martínez José J.3,ALOthman Zeid A.4,Romanelli Gustavo P.25,Nares Elena Montejano16,Ivars-Barceló Francisco6,Zuazo Juan Rubio78,Luque Rafael910,Balu Alina M.1

Affiliation:

1. Department of Organic Chemistry, University of Cordoba, Rabanales Campus, Marie Curie Building (C-3) , Ctra Nnal IV-A, Km 396, E14014 , Córdoba , Spain

2. Center for Research and Development in Applied Sciences “Dr. Jorge J. Ronco” CINDECA, Faculty of Exact Sciences, National University of La Plata , 47 N_ 257 , La Plata , 1900 , Argentina

3. School of Chemical Sciences, Faculty of Sciences, Pedagogical and Technological University of Colombia UPTC, Avenida Central del Norte , Tunja , Boyacá, 150003 , Colombia

4. Chemistry Department, College of Science, King Saud University , P.O. Box 2455 , Riyadh , 11451 , Saudi Arabia

5. CISAV, Department of Organic Chemistry, Faculty of Agricultural and Forestry Sciences, National University of La Plata, La Plata, Argentina; Forestry, National University of La Plata , Calles 60 y 119 s/n , La Plata , B1904AAN , Argentina

6. Department of Inorganic Chemistry and Technical Chemistry, Faculty of Sciences, UNED ; Av. España s/n , Las Rozas , 28232, Madrid , Spain

7. SpLine CRG BM25 Beamline, The European Synchrotron , 71, Avenue des Martys, 38000 , Grenoble , France

8. Instituto de Ciencia de Materiales de Madrid, Consejo Superior de Investigaciones Científicas (ICMM-CSIC) , 28049 , Madrid , Spain

9. Peoples Friendship University of Russia (RUDN University) , 6 Miklukho Maklaya str., 117198 , Moscow , Russian Federation

10. Universidad ECOTEC , Km. 13.5 Samborondón , Samborondón , EC092302 , Ecuador

Abstract

Abstract Hydrotalcite materials (HTs) were synthesized by a facile and swift combined mechanochemistry/coprecipitation approach, and their catalytic activity was evaluated and compared with conventionally synthesized hydrotalcites (co-precipitation method) in the Knoevenagel condensation between furfural and ethyl cyanoacetate/malononitrile. Characterization and catalytic activity results clearly demonstrate that the proposed combined mechanochemical/coprecipitation approach provides an improvement in crystallinity, morphology, tunable basicity, and textural properties (higher surface area and enhanced surface properties) as compared to HTs obtained via conventional coprecipitation methods. In addition, mechanochemically synthesized HTs largely improve catalytic activities, including conversion and product selectivity to Knoevenagel condensation products under solventless conditions, short reaction times, or reaction at room temperature as compared to conventional counterparts (e.g., 30–40 vs > 99% product yields).

Publisher

Walter de Gruyter GmbH

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