• Applied Chemistry for Engineering
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• v.33 no.4
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• pp.402-407
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• 2022

Statistical design of experiments was used to optimize the MOF-5 synthesis process. A mixture design was employed to optimize precursor concentration. The optimal composition of three chemical materials, terephthalic acid, zinc acetate dihydrate, and N,N-dimethylformamide for MOF-5 synthesis was determined by extreme vertices design methods as follows; 1 mol : 2.7 mol : 40 mol. A multilevel factorial design was selected to screen the significance of synthesis reaction conditions such as temperature, time, and stirring speed. Statistical analysis results suggested excluding stirring speed from further investigation. Using a central composition design, the synthesis time and temperature were optimized. The quadratic model equation was derived from 13 synthesis experiments. The model predicted that MOF-5 synthesized at 119 ℃ for 10.4 h had the highest crystallinity.

• Carbon letters
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• v.10 no.1
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• pp.19-22
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• 2009

In this work, the hydrogen storage behaviors of carbon nanotubes (CNTs)/metal-organic frameworks-5 (MOF-5) hybrid composites (CNTs/MOF-5) were studied. Hydrothermal synthesis of MOF-5 was conducted by conventional convection heating using 1-methyl-2-pyrrolidone (NMP) as a solvent. Morphological characteristics and average size of the CNTs/MOF-5 were also obtained using a scanning electron microscopy (SEM). The pore structure and specific surface area of the CNTs/MOF-5 were analyzed by N2/77 K adsorption isotherms. The capacity of hydrogen storage of the CNTs/MOF-5 was investigated at 298 K/100 bar. As a result, the CNTs/MOF-5 had crystalline structures which were formed by hybrid synthesis process. It was noted that the CNTs/MOF-5 can be potentially encouraging materials for hydrogen adsorption and storage applications at room temperature.

• Korean Chemical Engineering Research
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• v.61 no.2
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• pp.322-327
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• 2023

A design of experiments was evaluated in optimizing MOF-5 synthesis for acetylene adsorption. At first, mixture design was used to optimize precursor concentration, terephthalic acid, zinc acetate dihydrate and N,N-dimethylformamide. More specifically, 13 conditions with various molar ratios were designed by extreme vertices design method. After preparing the samples, XRD, N₂ physisorption and SEM analysis were performed for their characterization. Moreover, acetylene adsorption experiments were carried out over the samples under identical conditions. The optimal precursor composition for MOF-5 synthesis was predicted on a molar basis as follows: terephthalic acid : acetate dihydrate : dimethylformamide = 0.1 : 0.4 : 0.5. Thereafter, multi-level factorial design was designated to investigate the effect of synthesis reaction conditions such as temperature, time and stirring speed. By the statistical analysis of 18 samples designed, 4 reaction parameters were determined for additional adsorption experiments. Therefore, MOF-5 prepared under the synthesis time and temperature of 100 ℃ and 12 h, respectively, showed the maximum adsorption capacity of 15.1 mmol/g.

• Applied Chemistry for Engineering
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• v.30 no.5
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• pp.615-619
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• 2019

Statistical design of experiments was performed to optimize MOF-235 synthesis process. Concentrations of terephthalic acid (TPA), iron (III) chloride hexahydrate, N,N-dimethylformamide (DMF) and ethanol were important factors to develop the crystal structure of MOF-235. MOF-235 was synthesized with various concentrations of the listed chemicals above and the crystallinity was measured by XRD. The effect of the composition on the synthesis of MOF-235 was evaluated using a statistical analysis. For the variance analysis using F-test, the concentration of ethanol showed the greatest effect on the crystallinity and TPA the least influential. A regression model for predicting the crystallinity of MOF-235 was derived and the prediction results for two synthetic variables were presented using contour plots. Finally, the crystallinity was predicted by a mixture method with $FeCl_3$, ethanol and DMF.

• Bulletin of the Korean Chemical Society
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• v.27 no.10
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• pp.1523-1524
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• 2006

• Proceedings of the KAIS Fall Conference
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• 2011.12a
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• pp.357-360
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• 2011

A new copper adenine MOF (Bio-MOF) was synthesized by hydrothermal procedure and explored for its low temperature $CO_2$ adsorption. In this adenine a DNA nucleotide was used as a ligand for Cu in DMF solution at $130^{\circ}C$. The synthesized Bio MOF was characterized by XRD, SEM, EDS, TG and BE Tresults. The material possesses high surface area (716.08 $m^2g^{-1}$) with mono dispersed particles of about 2.126 nm. The maximum $CO_2$ adsorption capacity is 5wt% at $50^{\circ}C$, which is regenerable at $100^{\circ}C$ which is very low when compared to other metal organic frame work studied. This study proves that the synthesized material is also be a choice materials for low temperature $CO_2$adsorption.

• Applied Chemistry for Engineering
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• v.31 no.3
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• pp.258-266
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• 2020

The chemical fixation of CO₂ into cyclic carbonates is considered to be one of the most promising way to alleviate global warming and produce fine chemicals. In this work, the catalytic applicability of metal-organic frameworks (MOFs) as porous crystalline materials for the synthesis of five-membered cyclic carbonate from CO₂ and epoxides was reviewed. In addition, we have briefly classified the materials based on their different structural features and compositions. The studies revealed that MOFs exhibited good catalytic performance towards cyclic carbonate synthesis because of the synergistic effect between the acid sites of MOFs and nucleophile. Moreover, the effect of structure of designed MOFs and mechanism for the cycloaddition of CO₂ were suggested.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.32 no.6
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• pp.225-230
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• 2022

A new two-fold interpenetrating two-dimensional (2D) Tb(III) metal-organic framework (MOF), [Tb(p-XBP4)_2.5(H₂O)₂]·W(CN)₈ (1), was prepared using a p-XBP4 (N,N'-p-phenylenedimethylenbis(pyridin-4-one)), Cs₃[W(CN)₈], and Tb(NO₃)₃·6H₂O. The single crystal X-ray diffraction indicated that Tb-MOF exhibits a unique two-fold interpenetrating 2-D framework. It was also characterized through Fourier transform infrared spectroscopy (FTIR), and single and powder X-ray diffraction. To probe the molecular magnetic behavior, the magnetic properties of Tb-MOF were investigated by direct-current (DC) and alternating-current (AC) magnetic susceptibilities measurements and discussed.

• Bulletin of the Korean Chemical Society
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• v.30 no.12
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• pp.2921-2926
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• 2009

Cu-BTC[$Cu_3(BTC)_2(H_2O)_3$, BTC = 1,3,5-benzenetricarboxylate], one of the most well-known metal-organic framework materials (MOF), has been synthesized under atmospheric pressure and room temperature by using ultrasound. The Cu-BTC can be obtained in 1 min in the presence of DMF (N,N-dimethylformamide), suggesting the possibility of continuous production of Cu-BTC. Moreover, the surface area and pore volume show that the concentration of DMF is important for the synthesis of Cu-BTC having high porosity. The morphology and phase also depend on the concentration of DMF : Cu-BTC cannot be obtained at room temperature in the absence of DMF and aggregated Cu-BTC (with low surface area) is produced in the presence of high concentration of DMF. It seems that the deprotonation of benzenetricarboxylic acid by base (such as DMF) is inevitable for the room temperature syntheses.

• Membrane Journal
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• v.32 no.6
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• pp.367-382
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• 2022

Numerous metal-organic frameworks (MOFs) produced by periodic combinations of organic ligands and metal ions or metal-oxo clusters have led the way for the creation of energy-efficient membrane-based separations that may serve as viable replacements for traditional thermal counterparts. Although tremendous progress has been made over the past decade in the synthesis of polycrystalline MOF membranes, only a small number of MOFs have been exploited in the relevant research. Intercrystalline defects, or nonselective diffusion routes in polycrystalline membranes, are likely the reason behind the delay. Postsynthetic modifications (PSMs) are newly emerging strategies for providing polycrystalline MOF membrane diversity by leveraging advanced membranes as a platform and improving their separation capabilities via physical and/or chemical treatments; therefore, neither designing and developing MOFs nor tailoring membrane synthesis techniques for focused MOFs is necessary. In this minireview, seven subclasses of PSM techniques that have recently been adapted to polycrystalline MOF membranes are outlined, along with obstacles and future directions.