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First-class rare earth macrolide/valerolactone/caprolactone terpolymer and preparation method thereof

A caprolactone terpolymer and caprolactone ternary technology, applied in the field of rare earth macrolide/valerolactone/caprolactone terpolymer and its preparation, to improve mechanical properties and thermal stability , mild reaction conditions and excellent heat resistance

Active Publication Date: 2019-10-15
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is still little research on the application of rare earth metal catalysts to the ring-opening reaction of macrolides.

Method used

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  • First-class rare earth macrolide/valerolactone/caprolactone terpolymer and preparation method thereof
  • First-class rare earth macrolide/valerolactone/caprolactone terpolymer and preparation method thereof

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Embodiment 1

[0015] The preparation of embodiment 1 rare earth macrocyclic lactone / valerolactone / caprolactone terpolymer

[0016] Under nitrogen protection, 1.6 mmol of cycloethylene tridecanedioate, 1.2 mmol of δ-valerolactone and 1.2 mmol of ε-caprolactone were added to the reactor and mixed uniformly. Take 20μmol rare earth catalyst (C 6 h 5 NPPh 2 )Lu(CH 2 C 6 h 4 NMe 2 -o) 2 Dissolve in 1 mL of toluene and add to the mixture in the above reactor. The polymerization reaction temperature was 25°C, and the polymerization was carried out for 1000 minutes. Methanol was added to terminate the reaction, washed with methanol, and dried in vacuum to obtain a macrocyclic lactone / valerolactone / caprolactone terpolymer. The analysis results of polymer structure and properties are as follows: in mole percentage, the tridecanedioic acid cycloethylene ester content is 40%, the δ-valerolactone content is 30%, and the ε-caprolactone content is 30%. The number average molecular weight is 5.8×10...

Embodiment 2

[0017] Preparation of embodiment 2 rare earth macrocyclic lactone / valerolactone / caprolactone terpolymer

[0018] Under nitrogen protection, 2 mmol of cycloethylene tridecanedioate, 1.2 mmol of δ-valerolactone and 0.8 mmol of ε-caprolactone were added to the reactor and mixed uniformly. Take 20μmol rare earth catalyst (2-MeC 6 h 4 NPPh 2 )Sc(CH 2 C 6 h 4 NMe 2 -o) 2 Dissolve in 1 mL of toluene and add to the mixture in the above reactor. The polymerization reaction temperature was 25°C, and the polymerization was carried out for 1000 minutes. Methanol was added to terminate the reaction, washed with methanol, and dried in vacuum to obtain a macrocyclic lactone / valerolactone / caprolactone terpolymer. The polymer structure and property analysis results are as follows: in mole percentage, the tridecanedioic acid cycloethylene ester content is 50%, the δ-valerolactone content is 30%, and the ε-caprolactone content is 20%. The number average molecular weight is 7.2×10 4g / mo...

Embodiment 3

[0019] Preparation of embodiment 3 rare earth macrocyclic lactone / valerolactone / caprolactone terpolymer

[0020] Under nitrogen protection, 1.2 mmol of cycloethylene tridecanedioate, 1.2 mmol of δ-valerolactone and 1.6 mmol of ε-caprolactone were added to the reactor and mixed uniformly. Take 20μmol rare earth catalyst (4-MeC 6 h 4 NPPh 2 )Sc(CH 2 C 6 h 4 NMe 2 -o) 2 Dissolve in 1 mL of cyclohexane and add to the mixture in the above reactor. The polymerization reaction temperature was 25°C, and the polymerization was carried out for 1000 minutes. Methanol was added to terminate the reaction, washed with methanol, and dried in vacuum to obtain a macrocyclic lactone / valerolactone / caprolactone terpolymer. The polymer structure and property analysis results are as follows: in mole percentage, tridecanedioic acid cycloethylene ester content is 30%, δ-valerolactone content is 30%, ε-caprolactone content is 40%. The number average molecular weight is 5.9×10 4 g / mol, molecu...

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Abstract

The invention provides a first-class rare earth macrolide / valerolactone / caprolactone terpolymer and a preparation method thereof, and belongs to the technical filed of high polymer materials. The first-class rare earth macrolide / valerolactone / caprolactone terpolymer is prepared by catalyzing macrolide, delta-valerolactone and e-caprolactone to terpolymerize by using a rare earth catalyst under room temperature; the number-average molecular weight is 1*10<4> to 50*10<4> g / mol, and the molecular weight distribution is narrow; on the basis of mole percent, the sum of macrolide, delta-valerolactone and e-caprolactone is 100%; macrolide accounts for 10-70%, delta-valerolactone accounts for 10-80%, and e-caprolactone accounts for 10-80%; macrolide is selected from 14-16 macrolides; the rare earth catalyst is LnR2Xn; Ln is rare earth metal; R is alkyl connected to the rare earth metal; X is radical which is complexed with the rare earth; n is the number of Lewis acid. According to the first-class rare earth macrolide / valerolactone / caprolactone terpolymer, phosphine amine type non-cyclopentadienyl rare earth complex rare earth catalyst is treated as a main catalyst; the catalyzing activityis high; the reaction conditions are mild; the product structure is controllable; the terpolymer in which macrolide is introduced is capable of greatly improving the mechanical performance and the heat stability of polyester materials; a high-performance polyester material with outstanding heat resistance can be obtained.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a kind of rare earth macrolide / valerolactone / caprolactone terpolymer and a preparation method thereof. Background technique [0002] From the perspective of green and sustainable development, polymer materials need to switch from petroleum-based polymers to bio-based polymers. Among many polymer materials, aliphatic polyester is a typical bio-based polymer, which has many excellent properties, such as biodegradability, biocompatibility, etc. opened up broad prospects. Aliphatic polyesters can be prepared by polycondensation or ring-opening polymerization. In contrast, ring-opening polymerization is a chain growth reaction. Under the same conversion rate, polymers with higher molecular weights can be synthesized. At the same time, ring-opening polymerization also has the advantages of mild reaction conditions, less side reactions, etc., can control the chain end groups o...

Claims

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Application Information

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IPC IPC(8): C08G63/08C08G63/84
CPCC08G63/08C08G63/823
Inventor 冷雪菲李杨董婧晗牛慧王艳色
Owner DALIAN UNIV OF TECH
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