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

Active Publication Date: 2017-11-17
ASTATECH CHENGDU BIOPHARM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these vanadium complexes, especially when the ligand includes three or four phenolic structures, have very limited applications in ring-opening polymerization (Thermodynamics, Kinetics, and Mechanisms of Cyclic Esters Polymerization, ACS Symposium Series, Vol.764, Chapter 13, pp 160–198; A journey into the electrochemistry of vanadium compounds, Coord.Chem.Rev., in press, doi:10.1016 / j.ccr.2015.02.022)

Method used

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  • A kind of mononuclear vanadium complex and its preparation method and application
  • A kind of mononuclear vanadium complex and its preparation method and application
  • A kind of mononuclear vanadium complex and its preparation method and application

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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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Abstract

The present invention provides a mononuclear vanadium complex shown as formula I, and also provides a preparation method and application of the complex. The mononuclear vanadium complex has the advantages of simple preparation method, low toxicity, high catalytic activity and narrow molecular weight distribution; and the method can effectively control the molecular weight of the polymer according to the needs, and has a broad market prospect.

Description

technical field [0001] The invention relates to a mononuclear vanadium complex and its application. Background technique [0002] In recent years, the market demand for biodegradable polymers such as polylactic acid, polyglycolic acid, and lactic acid amino acid copolymers has grown dramatically due to their biological safety. Especially polylactic acid, it has received people's great attention (Chemical Routes for the Transformation of Biomass into Chemicals, Chem.Rev.2007,107,2411; Polymers from renewable resources: A perspective for a special issue of polymer reviews, Polym.Rev ., 2008, 48, 1; Synthetic polymer scaffolds for tissue engineering, Chem. Soc. Rev., 2009, 38, 1139). [0003] Industrially, these biodegradable polymers can be prepared by ring-opening polymerization of corresponding monomers, which requires the use of catalysts. Currently, stannous isooctanoate (Sn(Oct) 2 ) is a catalyst commonly used in industry at present. [0004] However, studies in recen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/00C08G63/08C08G63/85C08F4/685C08F10/00
Inventor 杨佑喆卡尔·瑞德肖孙秋郭鹏
Owner ASTATECH CHENGDU BIOPHARM CORP
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