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Thermokinetic evaluation of zircon oxide green synthesis mediated by plant extract of Abelmoschus esculentus L. Moench

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Abstract

The Abelmoschus esculentus L. Moench (okra) is much appreciated in the Brazilian regional cuisine, however, the selection of these vegetables for human consumption leads to a large accumulation of biomass, since the pre-selection of this aims to choose only unripe vegetables, and the others are discarded. In this sense, the present work aims to reuse this biomass, using it as a capping/stabilizing agent in the green synthesis of zirconium oxide. For the synthesis, two aqueous extracts of Abelmoschus esculentus L. Moench from the peel and pulp were used together (AEP) and another obtained from the seeds (AES). The syntheses were carried out in a microwave reactor, following the time-power program (5 min/300 W). In this step, a mixture of Zr4+ complexes, phenolic compounds and precursors are obtained, which after lyophilization is coded AEP-Zr and AES-Zr. These materials were characterized by XRD, FTIR and thermoanalytical techniques. In order to evaluate the thermokinetic behavior of these materials, a DTG 60-H (Shimadzu) was used, and in synthetic air atmosphere, the TG-DTG-DTA analyses were performed at rates of (5/10/15/20) °C min−1, with the kinetic parameters being obtained by the Ozawa method. From the analysis of the DTG and DTA curves, it is observed that the complexes obtained are distinct, culminating in different processes for the formation of ZrO2. The AEP-Zr sample presents six main stages of mass loss, while the AES-Zr sample presents five main stages of mass loss. From the kinetic study, it is observed that between 200 and 300 °C are the processes with the highest activation energy (189.27 and 191.54 kJ), associated with the hydroxide transformation phenomena and the crystallization of ZrO2. For the AEP-Zr sample, the event with the highest activation energy (148.27 kJ) is found between 500 and 600 °C and is associated with the possible phase conversion and crystallization of ZrO2, and the energy in this process is lower than in the AES-Zr synthesis. According to master plot method, both samples thermodecomplexation occurs in a sequence of different models, reaffirming the physicochemical and compositional differences of the samples.

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Acknowledgements

The authors thank the funding agencies FAPESB and CAPES for granting the scholarships and the post-graduation programs PGQA (UNEB) and PPEQ (UFBA) and IFBaiano- Catu for the infrastructure provided.

Funding

Partial financial support was received from CAPES, via Master’s Scholarship between 2018 and 2019, for João Daniel S. Castro. A scholarship was received from FAPESB, via IC program, between 2018 and 2020 for Edinilson Ramos Camelo. All authors declare that they have no affiliations or involvement in any organization or entity with any financial or non-financial interest in the subject matter or materials discussed in this manuscript.

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Authors and Affiliations

  1. Departamento de Ciências Exatas e da Terra, Curso de Licenciatura em Química, Universidade do Estado da Bahia, Salvador, BA, CEP 41195-001, Brazil

    Edinilson Ramos Camelo & Cesário F. das Virgens

  2. Institute of Thermal Power Engineering, Zhejiang University, Zheda Road, 38, Hangzhou, 310027, People’s Republic of China

    João Daniel S. Castro

  3. Programa de Pós-Graduação em Química Aplicada, Departamento de Ciências Exatas e da Terra, Universidade do Estado da Bahia, Salvador, BA, CEP 41195-001, Brazil

    João Daniel S. Castro & Cesário F. das Virgens

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  1. Edinilson Ramos Camelo
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  3. Cesário F. das Virgens
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All authors contributed to the study conception and design. Material preparation, data collection and analysis were performed by JDSC, ERC and CFdV. The first draft of the manuscript was written by JDSC and ERC; and all authors commented on previous versions of the manuscript. All authors read and approved the final manuscript.

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Correspondence to Cesário F. das Virgens.

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Camelo, E.R., Castro, J.D.S. & das Virgens, C.F. Thermokinetic evaluation of zircon oxide green synthesis mediated by plant extract of Abelmoschus esculentus L. Moench. J Therm Anal Calorim 148, 49–62 (2023). https://doi.org/10.1007/s10973-022-11586-z

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