A kind of binuclear vanadium complex and preparation method and use
A technology for complexes and compounds, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic compounds of Group 5/15 without C-metal bonds, etc., can solve problems such as application limitations, Achieving the effects of narrow molecular weight distribution, high yield and simple preparation method
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Embodiment 1
[0038] Example 1 Preparation and characterization of the binuclear vanadium complex 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 Spectroscopy
[0047] IR: 1572w, 1408w, 12...
Embodiment 2
[0083] Example 2 Synthesis of polylactic acid catalyzed by the binuclear vanadium complex of the present invention
[0084] Gel Permeation Chromatography (GPC) analysis uses the following instruments:
[0085]Shimadzu GPC instrument equipped with LC-20A pump, DGU-20A3 degassing unit, CTO-20A column thermostat, RID-10A differential detector, 2 Shodex silica gel columns (KF-803 and KF-804) and 1 protection 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-neck flask equipped with a stirring magnet to a Schlenk line equipped with argon and a pump, bake and dry it with a flame for three minutes, and then add 2 g of L-lactide after filling with argon-vacuum for at least 3 times , a...
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