High-Throughput Assisted Rationalization of the Formation of Metal Organic Frameworks in the Iron(III) Aminoterephthalate Solvothermal System

Abstract

Through the use of high-throughput methods, solvothermal reactions of FeCl 3 and 2-aminoterephthalic acid in protic as well as aprotic reaction media were systematically studied. Thus, the fields of formation of the isoreticular structures of MIL-53, MIL-88, and MIL-101 based on Fe(III) and aminoterephthalate could be identified for the first time. The resulting 3D framework materials with amino-functionalized pores have been characterized using X-ray diffraction; IR spectroscopy; and thermogravimetric, elemental, and energy dispersive X-ray analysis. Due to the applied high-throughput method, a high density of information was obtained in a short period of time, which allows the extraction of important reaction trends and contributes to a better understanding of the role of compositional as well as process parameters in the synthesis of inorganic-organic hybrid materials. We have found that the nature of the reaction medium has the most profound impact on structure formation. Furthermore, the concentration of the starting mixture (i.e., the solvent content) and the temperature have also been identified as key parameters for the formation of the different hybrid phases.

An Amine‐Functionalized Iron(III) Metal–Organic Framework as Efficient Visible‐Light Photocatalyst for Cr(VI) Reduction

“…The formation of these MOFs have been confirmed by their XRD patterns (Figure S12, Supporting Information). Those XRD patterns were in good agreement with as‐synthesized iron(III)‐based MOFs that were previously reported 46, 47, 48. The photocatalytic reduction of Cr(VI) was also investigated over MIL‐53 (Fe), NH 2 –MIL‐53 (Fe), MIL‐101 (Fe), and NH 2 –MIL‐101 (Fe).…”

Structural and elemental influence from various MOFs on the performance of Fe@C catalysts for Fischer–Tropsch synthesis

“…N 2 physisorption at 77 K, TGA and XRD confirmed the presence of MIL-68 [21][22][23] , MIL-88A [24][25][26] , MIL-100 [27][28][29] , MIL-101 [30][31][32] , and MIL-127 [33][34][35] (see Table S1, Figure S1 and Figure S2) ‡. XRD of the F300 Fe-BTC MOF revealed a very low degree of crystallinity, but the MIL-100 topology was confirmed since the isotherm contained an additional step in the micropore regime corresponding to the large cages in the MTN-type framework [27][28] .…”

Synthesis and O2 Reactivity of a Titanium(III) Metal–Organic Framework

“…3k, 8,9 In several analogues of the M 3 OX(bdc) 3 (M-MIL-101; bdc 2− = 1,4-benzenedicarboxylate; X = F, Cl, OH; M = Cr, 10 Fe, 11 V, 12 Al 13 ) and M 3 OX(btc) 2 (M-MIL-100; btc 3− = 1,3,5-benzenetricarboxylate; M = Cr, 14 Fe, 15 V, 12b Al, 16 Sc 17 ) series of frameworks, however, metal-bound solvent molecules can be partially, or in some cases, fully removed by heating under vacuum to generate five-coordinate M 3+ cations. 8,9 The M-MIL-101 and M-MIL-100 compounds are composed of triangular M 3 O(COO) 6 clusters, wherein each metal is octahedrally coordinated and bound to bridging carboxylates at the equatorial positions, a μ 3 -O 2− anion at one axial position, and either a solvent molecule or a charge-balancing anion at the other axial position.…”