Impact of the Preparation Procedure on the Performance of the Microporous HKUST-1 Metal-Organic Framework in the Liquid-Phase Separation of Aromatic Compounds

Исаева, В. И.; Saifutdinov, B. R.; Чернышев, Владимир В.; Vergun, Vadim V.; Капустин, Г. И.; Kurnysheva, Yulia P; Ilyin, M. M.; Кustov, Leonid М.

doi:10.3390/molecules25112648

Cited by 15 publications

(15 citation statements)

References 66 publications

(68 reference statements)

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“…It can be seen from Figure 6 that the HKUST-1 reference sample has micropores with a narrow size distribution in the 0.6 to 0.9 nm region. It is in a good accordance with the micropore diameter reported for the pristine HKUST-1 metal-organic framework [ 56 ].…”

Section: Resultssupporting

confidence: 89%

“…Probably, the observed pattern is induced because of the abundant presence of micropores in the HKUST-1 structure ( Table 1 ) and, consequently, by diffusion difficulties during the adsorbate mass transfer in these pores upon the dynamic process of HPLC. Recently [ 56 ], we suggested that the adsorbate molecules cannot penetrate into HKUST-1 micropores under the high mobile phase flow rates because of diffusion limitations, while they can do under the low mobile phase flow rates. Therefore, no adsorption equilibrium during the pristine HKUST-1 powder exploitation as a stationary phase in HPLC, in our opinion, signifies the necessity of improving the surface chemistry and, especially, chromatographic properties of this matrix through enhancing its porous structure.…”

Section: Resultsmentioning

confidence: 99%

“…Recently [ 56 ], we have studied the peculiarities of the mechanism of the liquid-phase adsorption of aromatic compounds on the HKUST-1 material. The microporous HKUST-1 (Cu 3 (btc) 2 , btc = benzene-1,3,5-tricarboxylate) matrix is one of the best studied MOF materials.…”

Section: Introductionmentioning

confidence: 99%

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Understanding the Working Mechanism of the Novel HKUST-1@BPS Composite Materials as Stationary Phases for Liquid Chromatography

et al. 2022

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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 HKUST-1@BPS 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 HKUST-1@BPS 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 HKUST-1@BPS 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.

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Section: Resultssupporting

confidence: 89%

Section: Resultsmentioning

confidence: 99%

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Understanding the Working Mechanism of the Novel HKUST-1@BPS Composite Materials as Stationary Phases for Liquid Chromatography

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“…On the other hand, in the context of the efficient control of the morphology of MOF crystallites, MW-assisted synthesis shows particular potential. This technique is recognized as a promising strategy to efficiently manipulate the key physico-chemical characteristics of produced MOF materials [31][32][33].…”

Section: Introductionmentioning

confidence: 99%

“…Recently, we reported the impact of MW-assisted synthesis in the H 2 O-DMF system at an atmospheric pressure using a household MW oven on the structural, compositional, morphological and textural characteristics of the produced HKUST-1 material and thereby on its performance in liquid phase adsorption [32].…”

Section: Introductionmentioning

confidence: 99%

Modifying HKUST-1 Crystals for Selective Ethane Adsorption Using Ionic Liquids as Synthesis Media

et al. 2022

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Novel adsorbents for methane and ethane based on HKUST-1 metal-organic framework were synthesized by microwave (MW) assisted technique using ionic liquids (ILs) as synthesis media. It was found that the MW synthesis time remarkably impacts both the product yield and the physico-chemical characteristics of the produced HKUST-1 material. The crystalline phase purity, crystallite size/dispersion and textural properties of the synthesized HKUST-1 matrices determine their performance in methane and ethane adsorption. Therefore, the HKUST-1 material produced in MW fields for 3 min only shows the highest phase purity and the largest surface area (BET) and porosity, along with a rather small crystallite size (below ~300 nm), demonstrating high methane and ethane adsorption capacity in the pressure range 1–30 atm.

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Observation of a Reversible Order‐Order Transition in a Metal‐Organic Framework – Ionic Liquid Nanocomposite Phase‐Change Material

Nozari,

Azar,

Sajzew

et al. 2024

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Metal‐organic framework (MOF) composite materials containing ionic liquids (ILs) have been proposed for a range of potential applications, including gas separation, ion conduction, and hybrid glass formation. Here, an order transition in an IL@MOF composite is discovered using CuBTC (copper benzene‐1,3,5‐tricarboxylate) and [EMIM][TFSI] (1‐ethyl‐3‐methylimidazolium bis(trifluoromethanesulfonyl)imide). This transition – absent for the bare MOF or IL – provides an extended super‐cooling range and latent heat at a capacity similar to that of soft paraffins, in the temperature range of ≈220 °C. Structural analysis and in situ monitoring indicate an electrostatic interaction between the IL molecules and the Cu paddle‐wheels, leading to a decrease in pore symmetry at low temperature. These interactions are reversibly released above the transition temperature, which reflects in a volume expansion of the MOF‐IL composite.

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Impact of the Preparation Procedure on the Performance of the Microporous HKUST-1 Metal-Organic Framework in the Liquid-Phase Separation of Aromatic Compounds

Cited by 15 publications

References 66 publications

Understanding the Working Mechanism of the Novel HKUST-1@BPS Composite Materials as Stationary Phases for Liquid Chromatography

Understanding the Working Mechanism of the Novel HKUST-1@BPS Composite Materials as Stationary Phases for Liquid Chromatography

Modifying HKUST-1 Crystals for Selective Ethane Adsorption Using Ionic Liquids as Synthesis Media

Observation of a Reversible Order‐Order Transition in a Metal‐Organic Framework – Ionic Liquid Nanocomposite Phase‐Change Material

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