Utilize dinuclear amine imine magnesium complex to catalyze the method of caprolactone polymerization

A technology of binuclear amine imine magnesium and complexes, which is applied in the direction of magnesium organic compounds, can solve the problems of metal residues, etc., and achieve the effects of low cost, fast reaction rate, and various catalyst structures

Active Publication Date: 2021-09-24
TAISHAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, one problem that still needs to be solved is that there will inevitably be metal residues in the products made by metal complex catalysts, and it is almost impossible to completely remove these residues from the polymer, so low-toxicity magnesium complexes become More promising catalysts, especially when polymers are used in the field of biomedicine, such catalysts are even more important

Method used

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  • Utilize dinuclear amine imine magnesium complex to catalyze the method of caprolactone polymerization
  • Utilize dinuclear amine imine magnesium complex to catalyze the method of caprolactone polymerization
  • Utilize dinuclear amine imine magnesium complex to catalyze the method of caprolactone polymerization

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The structural formula of the ligand used is the above formula (A), where R is hydrogen, and the reaction process is as follows: under a nitrogen atmosphere, slowly add 5 mL of benzyl alcohol tetrahydrofuran solution (2.0 mol / L) to an equimolar amount of Mg ( n Bu) 2 Hexane solution (2.0 mol / L, 5 mL) was reacted for 1 hour, 2.09 g of the ligand was dissolved in 20 mL of dry toluene, and added to Mg( n Bu) 2 In the reaction mixture with benzyl alcohol, after adding, the reaction liquid was naturally raised to room temperature, and then heated to 60 ° C for 3 hours. After the reaction was completed, the solvent was vacuum-dried, and the residue was washed with dry n-hexane, filtered, and then the product was collected and dried. Weighed to obtain 2.75 g of solid, yield 81.2%.

Embodiment 2

[0037] The structural formula of the ligand used is the above formula (A), where R is methyl, and the reaction process is as follows: under a nitrogen atmosphere, slowly add 5 mL of benzyl alcohol tetrahydrofuran solution (2.0 mol / L) to an equimolar amount at -10°C Mg( n Bu) 2 Hexane solution (2.0 mol / L, 5 mL) was reacted for 1 hour, 2.37 g of the ligand was dissolved in 20 mL of dry toluene, and added to Mg( n Bu)2 and benzyl alcohol reaction mixture, after adding, the reaction liquid was naturally raised to room temperature, and then heated to 40 ° C for 12 hours, after the reaction was completed, the solvent was vacuum-dried, and the residue was washed with dry n-hexane, filtered, and then the product was collected and dried Weighed to obtain 3.27g solid, yield 89.1%.

Embodiment 3

[0039] The structural formula of the ligand used is the above formula (A), where R is ethyl, and the reaction process is as follows: under a nitrogen atmosphere, slowly add 5 mL of benzyl alcohol THF solution (2.0 mol / L) to an equimolar amount at -10°C Mg( n Bu) 2 Hexane solution (2.0 mol / L, 5 mL) was reacted for 1 hour, 2.65 g of the ligand was dissolved in 30 mL of dry toluene, and added to Mg( n Bu) 2 In the reaction mixture with benzyl alcohol, after adding, the reaction liquid was naturally raised to room temperature, and then heated to 50 ° C for 4 hours. After the reaction was completed, the solvent was vacuum-dried, and the residue was washed with dry n-hexane, filtered, and then the product was collected and dried. Weighed to obtain 3.17g solid, yield 80.3%.

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Abstract

The invention discloses a method for catalyzing the polymerization of caprolactone by using a binuclear amineimine magnesium complex, using the binuclear amineimine magnesium complex as a catalyst, and using ε ‑Caprolactone as raw material, catalyzed under anhydrous, oxygen-free and gas protection ε ‑Caprolactone is polymerized to obtain polycaprolactone. The present invention uses self-developed binuclear amineimine magnesium complexes as catalysts for the ring-opening polymerization of caprolactone. The preparation method of the binuclear amineimine magnesium complex catalysts is simple, low in cost, high in product yield, and has various catalyst structures. The central magnesium coordinates with the N and N atoms of the ligand, has high catalytic activity, does not require a co-catalyst, and has a fast reaction rate. The obtained polymer has narrow molecular weight distribution, controllable molecular weight and high yield.

Description

technical field [0001] The invention relates to a method for catalyzing the polymerization of caprolactone, in particular to a method for catalyzing the polymerization of caprolactone by using a dinuclear amine imine magnesium complex. Background technique [0002] With the enhancement of people's awareness of environmental protection, the development of degradable biomaterials that can reduce environmental pollution has become one of the important research fields of polymer materials. Polylactone is a biodegradable, green and environment-friendly polymer material, and it has attracted more and more attention as a substitute for petroleum products. In the natural living environment, waste polylactone materials can be completely decomposed into small molecules by microorganisms in the soil. Because polyester is non-toxic, non-irritating, and has good biocompatibility, it is widely used in medical and environmental protection fields, such as surgical sutures, packaging, drug ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/08C08G63/83C07F3/02
Inventor 于广福许凤华顿爱社孙丰刚张海东王洪宾姚伟游淇
Owner TAISHAN MEDICAL UNIV
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