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Article

Understanding the Working Mechanism of the Novel [email protected] Composite Materials as Stationary Phases for Liquid Chromatography

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A.N. Frumkin Institute of Physical Chemistry and Electrochemistry, Russian Academy of Sciences, Building 4, 31 Leninsky Prospect, 119071 Moscow, Russia
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Department of Chemistry, M.V. Lomonosov Moscow State University, Building 3, 1 Leninskie Gory, 119991 Moscow, Russia
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N.D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, 47 Leninsky Prospect, 119991 Moscow, Russia
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A.N. Nesmeyanov Institute of Organoelement Compounds, Russian Academy of Sciences, 28 Vavilov Street, 119991 Moscow, Russia
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Institute of Ecotechnology, National University of Science and Technology MISiS, 4 Leninsky Prospect, 119991 Moscow, Russia
*
Authors to whom correspondence should be addressed.
Academic Editor: George Z. Kyzas
Polymers 2022, 14(7), 1373; https://doi.org/10.3390/polym14071373
Received: 1 March 2022 / Revised: 21 March 2022 / Accepted: 25 March 2022 / Published: 28 March 2022
(This article belongs to the Collection Polymer Materials for Adsorption Applications)
Composite materials have been used based on coordination polymers or microporous metal-organic frameworks (MOFs) combined with mesoporous matrices for adsorption-related techniques, which enable outflanking some adverse phenomena manifested during pristine components operation and enhance the performance and selectivity of the resulting materials. In this work, for the first time, the novel [email protected] composites synthesized by the microwave-assisted (MW) technique starting from microporous HKUST-1 (Cu3(btc)2) MOF and biporous silica matrix (BPS) with bimodal mesopore size distribution were comparatively studied as materials for liquid-phase adsorption techniques utilizing the high-performance liquid chromatography (HPLC) method and benzene as a model adsorbate. It was established that the studied [email protected] composites can function as stationary phases for HPLC, unlike the pristine HKUST-1 and bare BPS materials, due to the synergetic effect of both components based on the preliminary enhanced adsorbate mass transfer throughout the silica mesopores and, subsequently, its penetrating into HKUST-1 micropores. The suggested mechanism involves the initial deactivation of open metal Cu2+ sites in the HKUST-1 framework structure by isopropanol molecules upon adding this polar component into the mobile phase in the region of the isopropanol concentration of 0.0 to 0.2 vol.%. Thereafter, at the medium range of varying the isopropanol concentration in the eluent of 0.2 to 0.3 vol.%, there is an expansion of the previously inaccessible adsorption centers in the [email protected] composites. Subsequently, while further increasing the isopropanol volume fraction in the eluent in the region of 0.3 to 5.0 vol.%, the observed behavior of the studied chromatographic systems is similar to the quasi-normal-phase HPLC pattern. According to the obtained thermodynamic data, benzene adsorption into HKUST-1 micropores from solutions with a vol.% of isopropanol in the range of 0.4 to 5.0 follows the unique entropy-driven mechanism previously described for the MIL-53(Al) framework. It was found that HKUST-1 loading in the composites and their preparation conditions have pronounced effects on their physicochemical properties and adsorption performance, including the adsorption mechanism. View Full-Text
Keywords: coordination polymers; HKUST-1 metal-organic framework (MOF); biporous silica (BPS); composite materials; adsorption; high-performance liquid chromatography (HPLC) coordination polymers; HKUST-1 metal-organic framework (MOF); biporous silica (BPS); composite materials; adsorption; high-performance liquid chromatography (HPLC)
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MDPI and ACS Style

Saifutdinov, B.R.; Isaeva, V.I.; Chernyshev, V.V.; Vergun, V.V.; Kapustin, G.I.; Ivanova, Y.P.; Ilyin, M.M.; Tkachenko, O.P.; Buryak, A.K.; Kustov, L.M. Understanding the Working Mechanism of the Novel [email protected] Composite Materials as Stationary Phases for Liquid Chromatography. Polymers 2022, 14, 1373. https://doi.org/10.3390/polym14071373

AMA Style

Saifutdinov BR, Isaeva VI, Chernyshev VV, Vergun VV, Kapustin GI, Ivanova YP, Ilyin MM, Tkachenko OP, Buryak AK, Kustov LM. Understanding the Working Mechanism of the Novel [email protected] Composite Materials as Stationary Phases for Liquid Chromatography. Polymers. 2022; 14(7):1373. https://doi.org/10.3390/polym14071373

Chicago/Turabian Style

Saifutdinov, Bulat R., Vera I. Isaeva, Vladimir V. Chernyshev, Vadim V. Vergun, Gennady I. Kapustin, Yulia P. Ivanova, Mikhail M. Ilyin, Olga P. Tkachenko, Aleksey K. Buryak, and Leonid M. Kustov. 2022. "Understanding the Working Mechanism of the Novel [email protected] Composite Materials as Stationary Phases for Liquid Chromatography" Polymers 14, no. 7: 1373. https://doi.org/10.3390/polym14071373

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