The porous spherical alumina (γ‐Al2O3) as catalyst support was prepared by sol‐gel method, and FeCl3/γ‐Al2O3 materials were prepared by impregnation method. The FeCl3/γ‐Al2O3 materials were used as catalyst in the Solketal production process by acetalization of acetone and glycerol, showing considerable catalytic performance. When the molar ratio of glycerol and acetone was 1 : 10, 0.2 mol% FeCl3/γ‐Al2O3 was used as the catalyst, and the reaction was carried out at 25 °C for 30 min, the conversion of glycerol was 99.89 %, the selectivity of Solketal was 98.36 %, and the yield of Solketal reached 98.25 %. The mechanism is due to the spherical γ‐Al2O3 support has high thermal stability, large specific surface area, and rich pore structure, encouraging abundant active sites and high catalytic activity of FeCl3 for the acetalization reaction. Thereafter, the experimental results prove that the prepared FeCl3/γ‐Al2O3 catalyst can be easily recovered and reused many times, indicating its great value for large‐scale research and application in the future.
The porous spherical alumina (γ-Al2O3) as catalyst support was prepared by sol-gel method, and FeCl3/γ-Al2O3 materials were prepared by impregnation method. The FeCl3/γ-Al2O3 materials were used as catalyst in the Solketal production process by acetalization of acetone and glycerol, showing considerable catalytic performance. When the molar ratio of glycerol and acetone was 1:10, 0.2 mol% FeCl3/γ-Al2O3 was used as the catalyst, and the reaction was carried out at 25°C for 30 min, the conversion of glycerol was 99.89%, the selectivity of Solketal was 98.36%, and the yield of Solketal reached 98.25%. The mechanism is due to the spherical γ-Al2O3 support has high thermal stability, large specific surface area, and rich pore structure, encouraging abundant active sites and high catalytic activity of FeCl3 for the acetalization reaction. Thereafter, the experimental results prove that the prepared FeCl3/γ-Al2O3 catalyst can be easily recovered and reused many times, indicating its great value for large-scale research and application in the future.
C 14 H 16 BrCuN 3 O 4 , monoclinic, P12 1 /c1 (no. 14), a = 7.1063(2) Å, b = 21.0421(7) Å, c = 11.0447(4) Å, b = 95.974(2)°, V = 1642.6 Å 3 , Z = 4, R gt (F) = 0.028, wRref(F 2 ) = 0.078, T = 273 K. Source of materialSynthesis of the title compound was carried out by stirring the solution of CuBr2 (0.225 g, 1 mmol), 1,10-phenanthroline hydrate (0.198 g, 1 mmol), and glycine (0.075 g, 1 mmol) in ethanol (20 ml) for 6 hours at room temperature. After filtration, the filtrate was allowed to stand at room temperature. Slow evaporation of the solvent yielded blue crystals. Experimental detailsWhile the H atoms bonded to O atoms and involved in hydrogen bonds were localized from Fourier difference maps and refined freely, the other H atoms were added geometrically and treated as riding rigid body approximations.Discussion 1,10-Phenanthroline and its substituted derivatives represent a widely investigated class of chelating agents [1]. Some intrinsic properties of phenanthroline such as the structural rigidity and luminescence make them attractive. The most fruitful field of exploitation of these ligands is coordination chemistry. In the structure of the title compound [Cu(gly)(phen)(H2O)]Br · H 2 O, the Cu(II) ion is five-coordinated with an oxygen atom from a water molecule and chelated by a gly ion and a phen molecule (gly = glycin monoanion, phen = 1,10-phenanthroline), both of which are bidentate ligands to form a distorted square-pyramid (figure, top). The gly and phen units are both asymmetrically coordinated to the copper atom (d(Cu1N1) = 1.998(2) Å,006(2) Å) in the plane of the square pyramid with a water molecule occupying the fifth position. The Cu1O3 distance (2.259(2) Å) is slightly longer than the four distances above, which is because of the weaker coordination ability of the water oxygen compared with the other four coordinated atoms of gly and phen [2]. One lattice water molecule and one non-coordinated bromine anion are also present in the unit cell. The title compound includes one chiral C atom (C14) and crystallizes as racemic mixture of the enantiomers. The [Cu(gly)(phen)(H2O)] + , Br ions and H 2 O molecules units are interconnected by six kinds of strong hydrogen bonds to form a one-dimensional infinite supramolecular chains, and then each one-dimensional chain is interlinked by p-p interactions to form a two-dimensional structure. The distance between the two adjacent phenanthroline planes is in the range 3.3 Å 3.7 Å (d(C1···C4¢) = Z. Kristallogr.
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