Alkoxy rare-earth potassium multi-metal cluster compound and use thereof

A technology of alkoxy rare earth and rare earth metal, which is applied in the application field of ring-opening polymerization reaction, can solve problems that have not been seen yet, and achieve the effect of long active life

Inactive Publication Date: 2007-03-14
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there have been no reports of multimetal clusters containing rare earth metals and alkali metal potassium as catalysts for ring-opening polymerization of lactones.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment one: Ln 4 K 20 [OCH 2 CH 2 N(CH 3 ) 2 ] 26 (OH) 6 Synthesis of complexes Ln=Yb SmNd Pr, etc.

[0021] In the reaction flask after dehydration and deoxygenation treatment (taking Ln=Yb as an example), add metal K and an appropriate amount of THF under the protection of argon, and add a certain amount of anhydrous N, N-dimethylaminoethanol with a syringe, The reaction proceeded rapidly, and when no obvious bubbles were generated, it was stirred at room temperature for 24 hours, and the tube was sealed for later use. Then weigh anhydrous YbCl 3 0.84g (3mmol) was placed in a reaction flask that had been dehydrated and deoxygenated, added 30mlTHF, stirred at room temperature for half an hour, and then added to KOCH 2 CH 2 N(CH 3 ) 2 (19.5mmol) of tetrahydrofuran solution, add 0.25g (4.5mmol) of KOH, cook in a pot, stir and react in an oil bath at 40°C for 24 hours, centrifuge to remove the precipitate, vacuum the clear liquid to remove the solvent THF...

Embodiment 2

[0022] Embodiment 2: Nd 4 K 20 [OCH 2 CH 2 N(CH 3 ) 2 ] 26 (OH) 6 Catalytic ring-opening polymerization of ε-caprolactone

[0023] Make catalyst into 5×10 -6 Toluene solution with molar concentration, in a round-bottomed flask filled with argon gas through strict dehydration and deoxygenation, add 1.00ml ε-caprolactone and 9.90ml toluene in turn, place at 20°C and stir at room temperature, add 0.09ml of catalyst with a syringe Toluene solution. After 1 min, terminate with 2N HCl-ethanol, and finally precipitate the polymer with a large amount of ethanol. The polymer was dried under vacuum, weighed 1.03 g, and the conversion was 100%. GPC analysis: number average molecular weight (Mn) = 58870, molecular weight distribution index (weight average molecular weight / number average molecular weight Mw / Mn) = 1.75.

Embodiment 3

[0024] Embodiment three: Yb 4 K 20 [OCH 2 CH 2 N(CH 3 ) 2 ] 26 (OH) 6 Catalytic ring-opening polymerization of ε-caprolactone

[0025] Make catalyst into 2.5×10 -6 Toluene solution with molar concentration, in a round-bottomed flask filled with argon gas through strict dehydration and deoxygenation, add 1.00ml ε-caprolactone and 9.76ml toluene in turn, place it at 20°C and stir at room temperature, add 0.24ml of catalyst with a syringe Toluene solution. After 1 min, stop with 2NHCl-ethanol, and finally precipitate the polymer with a large amount of ethanol. The polymer was dried under vacuum, weighing 0.60 g, and the conversion was 76%. GPC analysis: number average molecular weight (Mn) = 85712, molecular weight distribution index (weight average molecular weight / number average molecular weight Mw / Mn) = 1.66.

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PUM

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Abstract

The present invention discloses one kind of alkoxy RE-K polymetal cluster compound containing 24 kinds of metal in the chemical expression of Ln4K20[OCH2CH2N(CH3)2]26(OH)6, where, Ln expresses RE metal. The present invention also discloses the application of the alkoxy RE-K polymetal cluster compound as catalyst for lactone ring-opening polymerization. The alkoxy RE-K polymetal cluster compound has very high activity of catalyzing the ring polymerization and copolymerization of epsilon-caprolactone and cyclic carbonate in mild conditions, and may be used as catalyst for initiating the random copolymerization and block copolymerization of two kinds of cyclic lactone. As catalyst, it has very long active life.

Description

technical field [0001] The invention relates to a class of alkoxy rare earth polymetallic clusters, in particular to a class of alkoxy rare earth potassium polymetallic clusters and their application in ring-opening polymerization of lactones. Background technique [0002] Fatty polyester and polycarbonate are a class of biodegradable polymer materials with good biocompatibility and can be used for sustained release of drugs. The ring-opening polymerization of cyclic lactones and cyclic carbonates is a convenient way to synthesize aliphatic polyesters and polycarbonates. [0003] Many alkoxy metal compounds can catalyze the ring-opening polymerization of such cyclic lactones and cyclic carbonates. In 1991, U.S. Patent No. 5,028,667 announced that alkoxy yttrium and alkoxy rare earth compounds can catalyze ε-hexene Controlled ring-opening polymerization of esters, valerolactone. Later, it was also reported in the literature that some compounds co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00C07F5/00C08F4/46C08G63/84
Inventor 盛鸿婷沈琪孙宏枚姚英明
Owner SUZHOU UNIV
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