A kind of coumarin copper complex and its preparation method and application
A technology of copper complexes and coumarin, which is applied in the fields of copper organic compounds, material excitation analysis, fluorescence/phosphorescence, etc., can solve the problems of difficult material preparation, staying in the theoretical research stage, and poor detection performance.
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Embodiment 1
[0044] The preparation of embodiment 1 C1 copper ion complex
[0045] 1. Preparation of fluorescent coumarin compound C1: by synthesizing two kinds of fluorescent coumarin compound C1, and further constructing its copper ion complex, which is used for the detection of trace water in common organic solvents and actual commodities. The structural formula of the compound C1 used is as follows, which can be synthesized with reference to the literature method:
[0046]
[0047] For the synthesis method, please refer to: C1, Chem.Commun., 2017, 53, 1813-1816.
[0048] 2. Preparation of C1 copper ion complex
[0049] Preparation of stock solution 1: Weigh copper acetate monohydrate (7.4mg) and dissolve it in 7.4mL ultra-dry acetonitrile to obtain stock solution 1, Cu 2+ The concentration is 5mM.
[0050] Preparation of stock solution 2: Take C1 (2.9 mg, 0.014 mmol) and dissolve it in 7 mL of ultra-dry acetonitrile to obtain stock solution 2. The concentration of C1 is 2 mM.
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Embodiment 2
[0053] Example 2 Characterization and water detection application of C1 copper ion complex
[0054] The C1 copper ion complex prepared in Example 1 can be characterized by an ultraviolet-visible spectrophotometer or fluorescence spectrum, and the formation of the complex structure can be determined through the quenching of the fluorescence of the C1 solution.
[0055] Depend on figure 1 a It can be seen that in ultra-dry acetonitrile, with the Cu in the C1 probe solution 2+ As the content increases, the absorption of the solution at 423nm increases gradually, while the absorption intensity at 351nm decreases gradually, and an isoabsorptive point appears at 376nm. Depend on figure 1 b It can be seen that the fluorescence intensity of the C1 probe solution increases with the Cu 2+ The addition gradually decreases, indicating that in Cu 2+ A complex was formed with C1 during the titration. The addition of 9.6 μL of stock solution 1 quenched the fluorescence of C1, proving ...
experiment example 1
[0064] Experimental Example 1 Detection of Moisture in Common Solvents
[0065] Weigh copper acetate monohydrate (7.4mg) and dissolve in 7.4mL ultra-dry acetonitrile to obtain stock solution 1, Cu 2+ The concentration is 5mM. Take C1 (2.9mg, 0.014mmol) and dissolve it in 7mL ultra-dry acetonitrile to obtain stock solution 2, the concentration of C1 is 2mM.
[0066] Add 3 mL of ultra-dry acetonitrile solution to the cuvette, add 15 μL of stock solution 2 to obtain a C1 probe solution with a concentration of 10 μM, add 9.6 μL (1.6 equiv) of stock solution 1 to obtain C1-Cu 2+ complex solution. To the C1-Cu 2+ Add 90 μL of distilled water to the complex solution, and test the fluorescence spectrum of the obtained solution as follows: Figure 8 shown.
[0067] The fluorescence intensity at the maximum emission wavelength of the curve is 3674520, and this value is used as the Y value, which is substituted into the C1-Cu established by the present invention 2+ The working curv...
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