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

Active Publication Date: 2017-03-29
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 binuclear vanadium complex and preparation method and use
  • A kind of binuclear vanadium complex and preparation method and use
  • A kind of binuclear vanadium complex and preparation method and use

Examples

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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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Abstract

The present invention provides a binuclear vanadium complex shown as formula I, and also provides a preparation method and application of the complex. The binuclear 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 binuclear 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. However, studies in recent years hav...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/00C08G63/85C08G63/08
CPCC07C39/235C07C31/28C07F9/005
Inventor 杨佑喆卡尔·瑞德肖孙秋郭鹏
Owner ASTATECH CHENGDU BIOPHARM CORP
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