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Synthesis and Characterization of Metal–Organic Frameworks
Published in T. Grant Glover, Bin Mu, Gas Adsorption in Metal-Organic Frameworks, 2018
The second important parameter of MOF synthesis is the solvent because the solubility of the starting materials must be ensured and the selection of the solvent can influence the reaction rate. As a primary component of the reaction mixtures, polar aprotic solvents, such as N,N-dimethylformamide (DMF), N,N-diethylformamide (DEF), N,N-dimethylacetamide (DMA), and 1-methyl-2-pyrrolidinone (NMP), are commonly used. In addition to the high solubility of metal salts, it is known that these solvents are partially decomposed through the solvothermal reaction. The generated amine species (e.g., dimethylamine) can facilitate the deprotonation of organic linkers, leading to the formation of a strong bond between the metal ion and the deprotonated linker terminal (e.g., carboxylate and imidazolate). To facilitate the linker deprotonation, basic additives, such as triethylamine and sodium hydroxide, can also be used. Indeed, the addition of base enables the room temperature MOF synthesis.16 It is not always necessary to purify these solvents as long as the target materials are obtained with reasonable reproducibility. Similarly, regular solvents (not dried solvents) can be used when hydrated metal salts are used for the MOF synthesis. However, if the reproducibility and/or crystallinity of MOF materials are poor, the reasons could be related to the purity of the solvents and other starting materials.
Microporous and Mesoporous Solids
Published in Elaine A. Moore, Lesley E. Smart, Solid State Chemistry, 2020
Elaine A. Moore, Lesley E. Smart
Different synthesis types are also needed to produce crystals of particular sizes and/or morphology. Templating techniques can also be used to control the pore size and to give access to metal sites that are exposed when a templating solvent such as N,N-dimethylformamide or N,N-diethylformamide is removed; it is these metal sites that then provide sites for gases, particularly hydrogen, to adsorb. Ultrasound- and microwave-assisted syntheses have been used to produce MOFs, for example, for potential biomedical use. Such MOFs need to be nontoxic and nanocrystalline and have high loading capacities.
Fluid Properties
Published in W. M. Haynes, David R. Lide, Thomas J. Bruno, CRC Handbook of Chemistry and Physics, 2016
W. M. Haynes, David R. Lide, Thomas J. Bruno
Name Dibutyl sul de Dibutyl sulfone Dibutyl sulfoxide Dibutyl tartrate Dichloroacetic acid Dichloroacetic anhydride 1,1-Dichloroacetone o-Dichlorobenzene m-Dichlorobenzene p-Dichlorobenzene 1,2-Dichlorobutane 1,4-Dichlorobutane 1,10-Dichlorodecane Dichlorodi uoromethane 1,1-Dichloroethane 1,2-Dichloroethane 1,1-Dichloroethene cis-1,2-Dichloroethene trans-1,2-Dichloroethene 1,7-Dichloroheptane 1,6-Dichlorohexane Dichloromethane (Dichloromethyl)benzene 1,2-Dichloro-2-methylpropane 1,1-Dichloro-1-nitroethane 1,8-Dichlorooctane 1,2-Dichloropentane 1,5-Dichloropentane 1,2-Dichloropropane, ()1,3-Dichloropropane 2,2-Dichloropropane 2,5-Dichlorostyrene 1,2-Dichloro-1,1,2,2-tetra uoroethane 2,4-Dichlorotoluene 2,6-Dichlorotoluene 3,4-Dichlorotoluene Dicyclohexyl ether Dicyclohexyl hexanedioate Dicyclopentadiene Didecyl ether Diethanolamine Diethoxydimethylsilane 1,2-Diethoxyethane Diethoxymethane N,N-Diethylacetamide Diethylamine N,N-Diethylaniline o-Diethylbenzene m-Diethylbenzene p-Diethylbenzene Diethyl carbonate Diethylene glycol Diethylene glycol dimethyl ether Diethyl ether N,N-Diethylformamide Diethyl fumarate Diethyl glutarate Diethyl hexanedioate Diethyl maleate Diethyl malonate Mol. form. C8H18S C8H18O2S C8H18OS C12H22O6 C2H2Cl2O2 C4H2Cl4O3 C3H4Cl2O C6H4Cl2 C6H4Cl2 C6H4Cl2 C4H8Cl2 C4H8Cl2 C10H20Cl2 CCl2F2 C2H4Cl2 C2H4Cl2 C2H2Cl2 C2H2Cl2 C2H2Cl2 C7H14Cl2 C6H12Cl2 CH2Cl2 C7H6Cl2 C4H8Cl2 C2H3Cl2NO2 C8H16Cl2 C5H10Cl2 C5H10Cl2 C3H6Cl2 C3H6Cl2 C3H6Cl2 C8H6Cl2 C2Cl2F4 C7H6Cl2 C7H6Cl2 C7H6Cl2 C12H22O C18H30O4 C10H12 C20H42O C4H11NO2 C6H16O2Si C6H14O2 C5H12O2 C6H13NO C4H11N C10H15N C10H14 C10H14 C10H14 C5H10O3 C4H10O3 C6H14O3 C4H10O C5H11NO C8H12O4 C9H16O4 C10H18O4 C8H12O4 C7H12O4 4.2925 25.7250 24.7340 9.441 8.3320 15.825 14.620 10.1220 5.0220 2.394355 7.7420 9.3035 6.6835 3.500-150 10.1025 10.4220 4.6020 9.2025 2.1420 8.3425 8.6035 8.9325 6.920 7.1523 16.330 7.6425 6.8920 9.9225 8.3720 10.2730 11.3720 2.5825 2.48420 5.6828 3.3628 9.3928 3.4520 4.8435 2.4340 2.64420 25.7520 3.21625 3.9020 2.52720 32.120 3.68020 5.1530 2.59420 2.36920 2.25920 2.82024 31.8220 7.2325 4.266620 29.620 6.5623 6.65930 6.10920 7.56025 7.55031 a 0.66248E+02 0.67156E+02 0.11014E+02 b -0.16417E+00 -0.16448E+00 -0.10859E-01 c 0.12001E-03 0.92275E-04 0.49242E-05 d
The effect of solvents on photocatalytic activity of Fe-BTC metal organic framework obtained via sonochemical method
Published in Inorganic and Nano-Metal Chemistry, 2019
Mehri Hossein Zadeh, Narjes Keramati, Mohsen Mehdipour Ghazi
The organic liquids, such as N, N-dimethylformamide (DMF), N, N-diethylformamide (DEF), 1-methyl-2-pyrrolidone (NMP)[16] and the binary solvents with water or ethanol[16–18] are conventional solvents for synthesis of MOFs. The application of different solvents in the process of synthesizing MOFs leads to the production of products of varying size and morphology. Also, this parameter is effective on the synthesis time. In a study by Hao et al., the higher synthesis time, costly solvent and the less quality of produced crystals by the DEF solvent have been reported against NMP.[19] In another study, the effect of the H2O/EtOH volume ratio on the synthesis of Mg-based benzene tricarboxylate frameworks was investigated. The results indicated that this ratio is effective on the dimensions of the final structure. As the ethanol increased, the dimensions of the structure varied from zero to three dimensional.[15,20]