A kind of mononuclear vanadium complex and its preparation method and application
A complex and mononuclear technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as application limitations, achieve narrow molecular weight distribution, simple preparation method, The effect of high catalytic activity
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Embodiment 1
[0033] Embodiment 1 Preparation and characterization of mononuclear vanadium complex of the present invention
[0034] 1, the preparation of mononuclear vanadium complex of the present invention
[0035]
[0036] Compound (Ⅲ) 2.0g (4.58mmol) and compound (Ⅳ) 1.32g (4.61mmol) were refluxed in toluene 30mL for 12h. Cool, vacuum dry to remove volatile components, and then extract with warm acetonitrile 30mL. After standing overnight at 0°C for 12h, 1.96g of reddish-brown crystal vanadium complex (II) was obtained, with a yield of 76%.
[0037]2. Characterization of the mononuclear vanadium complex of the present invention
[0038] 2.1 Elemental analysis
[0039] Molecular formula C 34 h 53 VO 4 , the measured value (theoretical value) is as follows
[0040] C: 70.69% (70.81%); H: 9.35% (9.26%).
[0041] 2.2 Infrared Spectrum
[0042] IR(cm-1):3487w, 1567w, 1417m, 1361s, 1292s, 1240w, 1229w, 1214w, 1199w, 1190w, 1155m, 1125m, 1108s, 1013s, 1003s, 978m, 876w, 845w, 799s...
Embodiment 2
[0073] Embodiment 2 Mononuclear vanadium complex of the present invention catalyzes the synthesis of polylactic acid
[0074] Gel Permeation Chromatography (GPC) analysis uses the following instruments:
[0075] 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.
[0076] 1. Catalysis under different conditions
[0077] The ring-opening polymerization reaction is carried out using Schlenk technology, as follows:
[0078] 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 with a flame for three minutes, and after argon gas-vacuum operation at least 3 times, add 2g of L-lactide , ...
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