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Effect of pretreatment temperature on the surface modification of diatomite with trimethylchlorosilane

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Abstract

Diatomite samples from Costa Rica were purified using acidic treatments with hydrochloric acid, thermally treated (400–1000 °C) and then silylated with trimethylchlorosilane in toluene under inert atmosphere. The purification process allows to decrease the concentration of metals presented in the crude diatomite, as is confirmed by X-ray Fluorescence (XRF) Analysis. The silylated materials were analyzed by using Hyperpolarized 129Xe Nuclear Magnetic Resonance Spectroscopy (HP 129Xe NMR), Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Thermogravimetric Analysis (TGA), rehydration tests, and contact angle measurements. XRD measurements indicate that diatomite is mainly amorphous, but presents several crystalline phases (kaolinite, cristobalite, and quartz). Pretreatments at high temperatures cause changes in those crystalline phases, resulting in more amorphous materials. However, there is no difference in the overall structure of purified and thermally treated diatomite samples with respect to the silylation products. In addition, SEM measurements show no effect over the pore structure of the materials. On the other hand, TGA measurements and rehydration tests show lower losses of water for silylated materials prepared using higher pretreatment temperatures. Moreover, HP 129Xe NMR, FTIR, and contact angle measurements evidence a modification due to covalent attachment of Si(CH3)3-groups to the surface, which increases for higher pretreatment temperatures. The results provide valuable information about external factors that influence the surface modification of diatomite. This can be useful to control modifications that can be achieved in a similar way.

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Acknowledgments

The authors thank the Vicerrectoría de Investigación (Grant: 115-A9-062) and the Sistema de Estudios de Posgrado of the Universidad de Costa Rica for supporting the research reported in this article. Thanks are also given to Claudia Chaves for her support with the SEM analyses, to Jorge Salazar for performing the TGA analyses, to Dr. Matthias Findeisen for technical support during the NMR experiments, and to Prof. W. D. Einicke for the BET analyses. Prof. Stefan Berger is acknowledged for helpful discussions. Thanks are also given for the valuable comments made by the reviewers.

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  1. Allen Puente-Urbina & Isaac F. Céspedes-Camacho

    Present address: Escuela de Química, Tecnológico de Costa Rica, Cartago, 159-7050, Costa Rica

Authors and Affiliations

  1. Laboratorio de Investigación en Química Inorgánica, Escuela de Química, Universidad de Costa Rica, San Pedro, 11501-2060, Costa Rica

    Allen Puente-Urbina & Grettel Valle-Bourrouet

  2. Institut für Analytische Chemie, Universität Leipzig, Linnéstr. 3, 04104, Leipzig, Germany

    Julia Hollenbach, Isaac F. Céspedes-Camacho & Jörg Matysik

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  1. Allen Puente-Urbina
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Correspondence to Grettel Valle-Bourrouet.

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Puente-Urbina, A., Hollenbach, J., Céspedes-Camacho, I.F. et al. Effect of pretreatment temperature on the surface modification of diatomite with trimethylchlorosilane. J Porous Mater 23, 1439–1449 (2016). https://doi.org/10.1007/s10934-016-0204-1

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