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Terpyridine zinc benzoate complex and preparation condition thereof

A technology of zinc benzoate and terpyridine, which is applied in the direction of luminescent materials, organic chemistry, chemical instruments and methods, etc., can solve the problems that there is no logical theory, long-wave zinc organic coordination polymer fluorescent materials are rare, etc., and achieve crystallization The effect of high purity, high thermal stability and simple operation process

Active Publication Date: 2017-06-16
CHONGQING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far, there are many zinc organic coordination polymers that emit blue fluorescence, but long-wave zinc organic coordination polymer fluorescent materials that emit yellow or red fluorescence are rare, and due to the particularity of the supramolecular field, its The preparation conditions have always been a black box, and there is no logical theory at all. Therefore, the development of new long-wave zinc organic coordination complex fluorescent materials and their preparation conditions has important significance and good market application prospects in the technical fields of long-wave fluorescence anti-counterfeiting. , and provide the possibility to replace rare earth resources

Method used

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  • Terpyridine zinc benzoate complex and preparation condition thereof
  • Terpyridine zinc benzoate complex and preparation condition thereof
  • Terpyridine zinc benzoate complex and preparation condition thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1 Zinc complex of the present invention [Zn(tpb) 2 (Htpb) 2 ] preparation

[0030] a) Weigh the raw materials according to the following molar ratio, Htpb: Zn(NO 3 ) 2 :DMF:H 2 O: HNO 3 The molar ratio is 1:2:516:8888:18, and in a 50mL glass beaker, mix and stir for 0.5 hours;

[0031] b) Transfer the mixture obtained in step a) into a 25 mL reaction kettle, and react at 140° C. for 3 days;

[0032] c) Naturally cooled to room temperature, yellow crystals were observed, filtered, washed with DMF and water in turn, and naturally dried to obtain the target product.

[0033] Use Perkin-Elmer2400 elemental analyzer to carry out elemental analysis on C, H, N elements of the target product, calculated value (%): C, 71.93; H, 4.02; N, 11.18; Actual measurement (%): C, 71.87; H, 4.03; N, 11.21.

[0034] Using a Nicolet Impact 410FTIR spectrometer with KBr as substrate at 400-4000cm -1 Infrared analysis of the target product within the range, FT-IR (KBr, cm -1 ...

Embodiment 2

[0039] Example 2 The zinc complex of the present invention [Zn(tpb) 2 (Htpb) 2 ] preparation

[0040] a) Weigh the raw materials according to the following molar ratio, Htpb: Zn(NO 3 ) 2 :DMF:H 2 O: HNO 3 The molar ratio is 1:1:516:8888:12, placed in a 50mL glass beaker, mixed and stirred for 1 hour;

[0041] b) Transfer the mixture obtained in step a) into a 25 mL reaction kettle, and react at 130° C. for 3 days;

[0042] c) Naturally cooled to room temperature, light yellow crystals were observed, filtered, washed with DMF and water in turn, and naturally dried to obtain the target product.

[0043] The target product was characterized by elemental analysis, infrared, fluorescence, and X-ray powder diffraction under the same conditions as in Example 1. The results were similar to those in Example 1. The target product obtained in Example 2 was the same as that obtained in Example 1. The sample is of high purity, the results are shown in Figure 5 .

[0044] Repeatin...

Embodiment 3

[0045] Example 3 The zinc complex of the present invention [Zn(tpb) 2 (Htpb) 2 ] preparation

[0046] a) Weigh the raw materials according to the following molar ratio, Htpb: Zn(NO 3 ) 2 :DMF:H 2 O: HNO 3 The molar ratio is 1:1:774:7778:15, placed in a 50mL glass beaker, mixed and stirred for 0.5h;

[0047] b) Transfer the mixture obtained in step a) into a 25 mL reaction kettle, and react at 140° C. for 2 days;

[0048] c) Naturally cooled to room temperature, light yellow crystals were observed, filtered, washed with DMF and water in turn, and naturally dried to obtain the target product.

[0049] The target product was characterized by elemental analysis, infrared, fluorescence, and X-ray powder diffraction under the same conditions as in Example 1. The results were similar to those in Example 1. The target product obtained in Example 3 was the same as that obtained in Example 1. The sample is of high purity, the results are shown in Figure 5 .

[0050] Repeating ...

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Abstract

Belonging to the field of fluorescent solid materials, the invention in particular relates to a terpyridine zinc benzoate complex [Zn(tpb)2(Htpb)2] and its preparation condition. The terpyridine zinc benzoate complex prepared by the invention has a coordination structure shown as formula (1) in the specification, can emit yellow fluorescence under 365nm ultraviolet irradiation, and has high thermal stability, and the skeleton starts decomposition at a temperature above 300DEG C, so that the complex can be used as a zinc based fluorescent solid material in various fields, and specifically can be applied to ink anti-counterfeiting technology, like anti-counterfeiting of bills, currencies, securities and other high-end products. According to the preparation condition of the terpyridine zinc benzoate complex [Zn(tpb)2(Htpb)2] provided by the invention, the operation is simple, the crystallization purity is high, and the yield is up to 69%. (formula (1)).

Description

technical field [0001] The invention belongs to the field of fluorescent solid materials and relates to a transition metal complex, in particular to a zinc terpyridine benzoate complex [Zn(tpb) 2 (Htpb) 2 ] and its preparation conditions. Background technique [0002] In the commodity economy society, anti-counterfeiting is an important issue that people are generally concerned about. Chemical anti-counterfeiting is a method with wide application prospects because of its simple manufacture, convenient identification, low cost, good confidentiality and high reliability. The development of chemical anti-counterfeiting technology depends on the discovery of new chemical anti-counterfeiting materials. For a long time, the preparation of chemical anti-counterfeiting fluorescent materials mostly uses rare earth elements as the main raw materials, but on the one hand, rare earth elements are expensive, and their use and cost are limited. On the other hand, with the consumption of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/55C09K11/06
CPCC07D213/55C09K11/06C09K2211/188
Inventor 黄坤林于方舟傅雪莲虞哲张明星陈新冉红雨徐文娟
Owner CHONGQING NORMAL UNIVERSITY
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