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2,3',5,5'-cadmium diphenyltetracarboxylate complex and its preparation method

A technology of diphenyltetracarboxylic acid and cadmium complex, which is applied in the direction of cadmium organic compounds, chemical instruments and methods, luminescent materials, etc., and achieves the effect of good thermal stability

Inactive Publication Date: 2016-05-11
LUOYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, based on 2,3′,5,5′-diphenyltetracarboxylic acid as a bridging ligand and formed with cadmium metal, there is no cadmium complex fluorescent material see reports

Method used

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  • 2,3',5,5'-cadmium diphenyltetracarboxylate complex and its preparation method
  • 2,3',5,5'-cadmium diphenyltetracarboxylate complex and its preparation method
  • 2,3',5,5'-cadmium diphenyltetracarboxylate complex and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Mix 0.1mmol (33.0mg) of 2,3′,5,5′-dibenzenetetracarboxylic acid, 0.1mmol (5.6mg) of potassium hydroxide, 0.1mmol (21.8mg) of bih with 0.1mmol (26.6mg) of Cadmium acetate was dissolved in 12mL of water to make a mixed solution, and the mixed solution was added to a 25mL closed reaction kettle, heated to 120°C at a rate of 10°C per hour, maintained at this temperature for 3 days, and then naturally cooled to room temperature, A colorless blocky crystal can be obtained, which is separated, washed and dried in sequence, and finally the target product is obtained with a yield of about 52%. The main infrared absorption peaks are: 3124m, 2938m, 2360m, 2341s, 1601s, 1541s, 1428m, 1396m, 1274s, 1239s, 1111s, 1087s, 1063s, 1030m, 939s, 913s, 848s, 772s, 706s.

[0023] The cadmium complex of 2,3',5,5'-diphenyltetracarboxylate prepared in Example 1 was further characterized, and the process is as follows:

[0024] (1) Determination of the crystal structure of the complex

[0025]...

Embodiment 2

[0042] Mix 0.06mmol (19.8mg) of 2,3′,5,5′-dibenzenetetracarboxylic acid, 0.18mmol (10.08mg) of potassium hydroxide, 0.06mmol (13.1mg) of bih with 0.18mmol (43.9mg) of Cadmium acetate was dissolved in 12mL of water to make a mixed solution, and the mixed solution was added to a 25mL closed reaction kettle, heated to 130°C at a rate of 10°C per hour, maintained at this temperature for 3 days, and then cooled to room temperature naturally. A colorless blocky crystal can be obtained, which is separated, washed and dried in sequence to obtain the target product with a yield of about 51%.

Embodiment 3

[0044] Mix 0.18mmol (59.4mg) of 2,3′,5,5′-dibenzenetetracarboxylic acid, 0.06mmol (2.4mg) of sodium hydroxide, 0.18mmol (39.3mg) of bih with 0.06mmol (14.6mg) of Cadmium acetate was dissolved in 12mL of water to make a mixed solution, and the mixed solution was added to a 25mL closed reaction kettle, heated to 130°C at a rate of 10°C per hour, maintained at this temperature for 3 days, and then cooled to room temperature naturally. A colorless massive crystal can be obtained, which is separated, washed and dried in sequence to obtain the target product with a yield of about 47%.

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Abstract

The invention relates to a 2,3'5,5'-diphenyl tetracarboxylic acid cadmium complex and a preparation method thereof and relates to the field of cadmium complex fluorescent materials. A chemical formula of the 2,3'5,5'-diphenyl tetracarboxylic acid cadmium complex is {[Cd2(bptc)(bih)(H2O)2].H2O}n, wherein bptc is 2,3',5,5'-diphenyl tetra formic acid anion ligand, and bih is 1,6-di(imidazole-1-) hexane. The preparation method of the 2,3'5,5'-diphenyl tetracarboxylic acid cadmium complex comprises the following steps: under hydrothermal condition, dissolving 2,3',5,5'-diphenyl tetra formic acid, an inorganic base, 1,6-di(imidazole-1-) hexane and a cadmium salt in water, adding the obtained mixed solution into a closed reaction still, heating to 120-160 DEG C at a speed of 10 DEG C per hour, performing heat preservation for 3 days, then cooling to room temperature under natural conditions, so that colourless massive crystals are generated, and then washing and drying, so that the target product, namely the 2,3'5,5'-diphenyl tetracarboxylic acid cadmium complex, is obtained finally. The 2,3'5,5'-diphenyl tetracarboxylic acid cadmium complex has stable fluorescence property and high yield, and the preparation method is simple, and has good repeatability.

Description

technical field [0001] The present invention relates to d 10 The field of metal complex fluorescent materials specifically relates to a 2,3',5,5'-diphenyltetracarboxylate cadmium complex and a preparation method thereof. Background technique [0002] Fluorescent complexes with high luminescence performance have great application prospects in the fields of communication, satellite, radar, optical computer and biomolecular probes. Therefore, the molecular design, synthesis and property research of such functional complexes are of great significance. where d 10 Metal-organic coordination polymers have attracted extensive attention due to their good fluorescence properties. [0003] 2,3′,5,5′-Dibenzenetetracarboxylic acid and its derivatives are an important class of bridging ligands. Some molecular-based coordination polymer materials constructed by reacting such ligands with metal ions have been studied. reported and exhibited excellent potential performance. At present, b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F3/08C09K11/06
Inventor 常新红赵颖李飞飞马录芳李仕辉
Owner LUOYANG NORMAL UNIV
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