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Equipartition type beta-diketone imidogen rareearth complexes-sec-propyl alcohol system and uses thereof

A diketimine-based, rare-earth complex technology is applied in the fields of compounds containing Group 3/13 elements of the periodic table, organic chemistry, chemical instruments and methods, etc., to achieve high activity, good application prospects, and easy synthesis.

Inactive Publication Date: 2009-01-14
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the use of β-diketoimino rare earth complex-alcohol system as a controllable catalytic system for the ring-opening polymerization of cyclic monomers of L-lactide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Ln[p-Cl-C 6 h 4 NC(Me)CHC(Me)NC 6 h 4 -p-Cl] 3 Synthesis of Complex-Isopropanol System Ln=Pr, La, Ce, Gd, Sm, Eu, Nd, Y

[0021] The in situ generated Li[p-Cl-C 6 h 4 NC(Me)CHC(Me)NC 6 h 4 -p-Cl] (9.00mmol) in toluene-hexane (30mL) was added to 25mL of THF in LnCl 3 (0.74g, 3.00mmol) in the turbid solution, reacted at room temperature for 24h, heated to 50°C for 48h, centrifuged, and discarded very little precipitate. The mother liquor was drained, added toluene for extraction, and centrifuged. The resulting clear liquid was concentrated and frozen overnight at 0° C. to obtain 2.46 g (2.24 mmol) of crystals, with a yield of 75%. Then isopropanol is added, and the desired homogeneous β-diketoimine-based rare earth complex-isopropanol system is obtained after sufficient reaction.

Embodiment 2

[0022] Example 2: La[p-Cl-C 6 h 4 NC(Me)CHC(Me)NC 6 h 4 -p-Cl] 3 -Isopropanol system catalyzes the controllable polymerization of L-lactide

[0023] In the reaction flask that has been dehydrated and deoxygenated, add 0.40 g (2.78 mmol) of L-lactide under the protection of argon, add 2.10 mL of tetrahydrofuran with a syringe, and add the catalyst-iso 0.69mL (1.00×10 -2 mmol·mL -1 ). Polymerize for 30 minutes, stop the reaction with alcohol containing 5% hydrochloric acid, precipitate the polymer with denatured alcohol, and vacuum dry to constant weight to obtain 0.40 g of polylactide with a yield of 100%.

[0024] The theoretical molecular weight of polymkeric substance is 57,600, and GPC measured number average molecular weight (M n ) is 50,100, the molecular weight distribution (M w / M n ) is 1.15.

[0025] The determination method of above-mentioned polymer molecular weight and molecular weight distribution is as follows: the polymer is made into the tetrahydrofu...

Embodiment 3

[0026] Example three: Nd[p-Cl-C 6 h 4 NC(Me)CHC(Me)NC 6 h 4 -p-Cl] 3 -Isopropanol system catalyzes the controllable polymerization of L-lactide

[0027] In the reaction flask that has been dehydrated and deoxygenated, add 0.50 g (3.47 mmol) of L-lactide under the protection of argon, add 2.31 mL of tetrahydrofuran with a syringe, and add the catalyst-iso 1.16mL (1.00×10 -2 mmol·mL -1 ). Polymerize for 15 minutes, terminate the reaction with alcohol containing 5% hydrochloric acid, precipitate the polymer with denatured alcohol, and vacuum-dry to constant weight to obtain 0.48 g of polylactide with a yield of 96%.

[0028] The theoretical molecular weight of polymkeric substance is 41,500, and GPC measured number average molecular weight (M n ) is 39,100, the molecular weight distribution (M w / M n ) is 1.14.

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PUM

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Abstract

The invention discloses a homoleptic Beta-Diketiminato rare earth complex-isopropyl alcohol system, the homoleptic Beta-Diketiminato rare earth complex has the following chemical formula: Ln[p-Cl-C6H4NC(Me)CHC(Me)NC6H4-p-Cl]3, wherein, Ln represents rare earth metal. Meanwhile, the invention discloses applications of the complex -isopropyl alcohol system in the controllable ring-opening polymerization reaction of L-lactide as a catalyst. The homoleptic Beta-Diketiminato rare earth complex-isopropyl alcohol system can controllably catalyze the ring-opening polymerization reaction of L-lactide under mild conditions, and can obtain poly-lactide acid that can predict the molecular weight and narrowness of molecular weight distribution, and has extreme high catalytic activity.

Description

technical field [0001] The invention relates to a rare earth complex-alcohol system, in particular to a homogeneous β-diketoimine-based rare earth complex-isopropanol system and its use in the controllable ring-opening polymerization of L-lactide Applications. Background technique [0002] Polylactic acid (also known as polylactide) is a class of biodegradable polymer materials, which can be degraded under physiological conditions, and the degradation products are non-toxic, so it is widely used in drug controlled release systems, orthopedic fixation and tissue engineering Scaffold materials, etc.; the polymer is mainly synthesized by ring-opening polymerization of cyclic monomers of L-lactide, and the use of controllable polymerization method can make the polymerization process controllable, and obtain a narrow molecular weight distribution and predictable molecular weight The polymers have better physical and mechanical properties, good biodegradability and biocompatibili...

Claims

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Application Information

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IPC IPC(8): C07F5/00C08G63/84C08G63/08
Inventor 薛明强沈琪
Owner SUZHOU UNIV
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