Binuclear vanadium complex, and preparation method and application thereof
A technology of complexes and solvates, applied in the field of binuclear vanadium complexes, can solve problems such as application limitations, and achieve the effects of narrow molecular weight distribution, high yield and wide application range
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Embodiment 1
[0038] Embodiment 1 Preparation and characterization of binuclear vanadium complexes of the present invention
[0039] 1, the preparation of binuclear vanadium complex of the present invention
[0040]
[0041] Compound (Ⅳ) 4.1g (4.44mmol) and compound (Ⅴ) VO(iPrO) 3 2.10mL (8.90mmol) was refluxed in 30mL of toluene for 12h. Cool and dry in vacuo to remove volatile components, and then extract the residue with 30 mL of dichloromethane. Standing at 0 ° C to obtain a brown solid compound, brown solid compound C 70 h 100 o 8 V 2 ·2CH 2 Cl 2 4.32g, yield 83%.
[0042] 2. Characterization of the binuclear vanadium complex of the present invention
[0043] 2.1 Elemental analysis
[0044] Elemental analysis was performed after vacuum drying for 12 h. Molecular formula C 70 h 98 V 2 o 8 ·2CH 2 Cl 2 , the measured value (theoretical value) is as follows:
[0045] C: 67.01% (67.55%); H: 7.86% (8.49%).
[0046] 2.2 Infrared Spectrum
[0047] IR: 1572w, 1408w, 1260s...
Embodiment 2
[0083] Embodiment 2 Binuclear vanadium complex of the present invention catalyzes the synthesis of polylactic acid
[0084] Gel Permeation Chromatography (GPC) analysis uses the following instruments:
[0085] Shimadzu GPC instrument equipped with LC-20A pump, DGU-20A3 degasser, CTO-20A column oven, RID-10A differential detector, 2 Shodex silica gel columns (KF-803 and KF-804) and 1 guard column (KF-G). At 40°C, tetrahydrofuran (HPLC grade) was used as the mobile phase at a flow rate of 1 mL / min. Calibrated with narrow molecular weight distribution polystyrene.
[0086] 1. Catalysis under different conditions
[0087] The ring-opening polymerization reaction is carried out using Schlenk technology, as follows:
[0088]Connect a two-necked flask equipped with a stirring magnet to a Schlenk line equipped with argon gas and a pump, bake and dry it by flame for three minutes, and after argon gas-vacuum operation at least 3 times, add 2gL-lactide, Appropriate amount of benzyl ...
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