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Hyperbranched polyester rare earth complex containing nitrogen heterocyclic terminal group, and preparation method and use thereof

A technology of hyperbranched polyester and rare earth complexes, which is applied in the fields of compounds containing group 3/13 elements of the periodic table, chemical instruments and methods, and organic chemistry. problems, to achieve the effect of simple synthesis method, easy processing and molding, and long fluorescence lifetime

Active Publication Date: 2015-08-12
JIAXING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation route of this method is generally long, and the rare earth complexes with polymerization activity are generally vinyl monomers, and the types and range of monomers that can be selected are relatively narrow.

Method used

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  • Hyperbranched polyester rare earth complex containing nitrogen heterocyclic terminal group, and preparation method and use thereof
  • Hyperbranched polyester rare earth complex containing nitrogen heterocyclic terminal group, and preparation method and use thereof
  • Hyperbranched polyester rare earth complex containing nitrogen heterocyclic terminal group, and preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] (1) Add 0.3000g hydroxyl-terminated hyperbranched polyester I and 1.1351g acyl chloride-containing nitrogen heterocyclic compound I into a three-necked flask, add 25ml dimethyl sulfoxide, dissolve, stir and mix evenly, and under nitrogen protection, heat up to 60°C, add 0.64ml triethylamine, react for 24 hours, wait for the temperature in the reaction bottle to drop to room temperature, settle the reaction solution in deionized water, filter it with suction, and dry it under vacuum at 80°C for 12h to obtain a light yellow powder containing nitrogen. Ring-terminated hyperbranched polyester I. The structural formula of the above-mentioned terminal hydroxyl hyperbranched polyester I and the nitrogen heterocyclic compound I containing acid chloride group is as follows:

[0051]

[0052] attached figure 1 It is the proton nuclear magnetic resonance spectrum of the hyperbranched polyester I of the nitrogen-containing heterocyclic end group in embodiment 1. The peak at 2....

Embodiment 2

[0056] The hyperbranched polyester I of 0.5000g nitrogen-containing heterocyclic end group, 0.5224g terbium nitrate and 0.6857g 1,10-phenanthroline are added in the three-necked flask, add 10ml dimethyl sulfoxide, dissolve and stir to mix evenly, in Stir the reaction at 60°C for 4 hours, cool to room temperature, settle the reaction solution in a large amount of absolute ethanol, filter it with suction, and dry it in vacuum at 80°C for 12 hours to obtain a light yellow powder of hyperbranched polyester terbium with nitrogen-containing heterocyclic end groups Complex I.

[0057] attached Figure 4 It is the fluorescence emission spectrogram of the hyperbranched polyester terbium complex I of the nitrogen-containing heterocyclic end group in Example 2 excited at 320 nm. The hyperbranched polyester terbium complex I containing nitrogen heterocyclic end groups can emit the characteristic fluorescence of terbium ions under the excitation of 320nm, and the emission intensity is the...

Embodiment 3

[0059] (1) Add 0.3000g hydroxyl-terminated hyperbranched polyester II and 0.5764g acyl chloride-containing nitrogen heterocyclic compound II into a three-necked flask, add 20ml dimethyl sulfoxide, dissolve and mix evenly, and heat up to 70°C, add 0.55ml triethylamine, react for 36 hours, wait until the temperature in the reaction bottle drops to room temperature, settle the reaction solution in anhydrous ether, filter it with suction, and dry it under vacuum at 80°C for 12h to obtain a light yellow powder containing nitrogen Hyperbranched polyesters II with heterocyclic end groups. The structural formula of the above-mentioned hydroxyl-terminated hyperbranched polyester II and the nitrogen heterocyclic compound II containing acid chloride group is as follows:

[0060]

[0061] (2) Add 0.5000g of hyperbranched polyester II containing nitrogen-containing heterocyclic end groups, 0.7653g of terbium nitrate and 1.1261g of α-thienoyl trifluoroacetone into a three-necked flask, a...

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Abstract

The invention discloses a hyperbranched polyester rare earth complex containing a nitrogen heterocyclic terminal group, and a preparation method and a use thereof, wherein the hyperbranched polyester rare earth complex containing the nitrogen heterocyclic terminal group has the structural formula represented by the formula (I). The preparation method comprises the following steps: (1) hydroxyl-terminated hyperbranched polyester is modified by a modifier, the nitrogen heterocyclic terminal group is connected on a terminal hydroxyl, and thus hyperbranched polyester containing the nitrogen heterocyclic terminal group is obtained; and (2) the hyperbranched polyester containing the nitrogen heterocyclic terminal group, a second ligand and a rare earth soluble salt are dissolved in an organic solvent and undergo a reaction, and after the completion of the reaction, the hyperbranched polyester rare earth complex containing the nitrogen heterocyclic terminal group is obtained by separating from the reaction solution. With utilization of a coordination reaction of nitrogen atoms of the nitrogen heterocyclic group of the hyperbranched polyester with rare earth ions, the hyperbranched polyester rare earth complex containing the nitrogen heterocyclic terminal group is prepared; the rare earth complex is simple in synthesis method, is easy to process and mold, high in luminescent intensity and long in fluorescent lifetime, and can be used in the fields of display materials or luminous paints and the like.

Description

technical field [0001] The invention relates to a complex, in particular to a hyperbranched polyester rare earth complex containing a nitrogen-containing heterocyclic end group, a preparation method and application thereof. Background technique [0002] Bipyridine, 1,10-phenanthroline, terpyridine and their derivatives are a class of compounds with a heterocyclic conjugated structure, and the electron cloud density near the N atom that can coordinate with rare earth ions in the molecular structure is relatively high. High, it is beneficial to the effective energy transfer between rare earth ions, and at the same time, the co-coordination of N atoms and rare earth ions can form a stable five-membered ring structure, and rare earth complexes with strong fluorescence can be obtained. Therefore, this type of heterocycle Compounds have been widely used as organic ligands of rare earth ions. [0003] However, the small-molecule rare earth complexes prepared with the above-mention...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00C09K11/06
CPCC07F5/00C09K11/06C09K2211/1029C09K2211/145C09K2211/182
Inventor 刘丹周大鹏王红梅郑斌李城剑吴美霞
Owner JIAXING UNIV
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