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A kind of fluorescent probe for identifying mercury ion and its preparation method and identification method

A fluorescent probe and identification method technology, applied in the field of fluorescent probes for identifying mercury ions and their preparation and identification, can solve the problems of inapplicability to real-time and on-site detection, complex sample processing, and high detection costs, and achieve visible structure and selection. The effect of good performance and low identification cost

Active Publication Date: 2022-05-17
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the sensitivity of these methods is relatively high, they all have the disadvantages of high detection cost, complicated sample processing, time-consuming, and are not suitable for real-time and on-site detection.

Method used

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  • A kind of fluorescent probe for identifying mercury ion and its preparation method and identification method
  • A kind of fluorescent probe for identifying mercury ion and its preparation method and identification method
  • A kind of fluorescent probe for identifying mercury ion and its preparation method and identification method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1: A kind of preparation method of the fluorescent probe of identifying mercury ion, the steps are as follows:

[0041] (1) Add 1g of 2,5-dibromoaniline, 1.2g of 4-vinylpyridine, 50mg of bistriphenylphosphine palladium dichloride and 1.2g of anhydrous potassium carbonate into 5ml of anhydrous reagent DMF and mix, and seal the mixture in N 2 In a high-pressure reaction bottle under atmosphere, react at 110°C for 25 hours to obtain product A;

[0042] (2) Product A was completely dissolved into a black suspension with dichloromethane to obtain Product B;

[0043] (3) Product B was washed with water and saturated saline for 3 times successively to obtain product C;

[0044] (4) The product C was left to stand and layered, and the bottom dichloromethane layer was separated, dried with anhydrous magnesium sulfate, spin-dried, and finally recrystallized with absolute ethanol to obtain a fluorescent probe.

Embodiment 2

[0045]Embodiment 2: a kind of preparation method of the fluorescent probe of identifying mercury ion, the steps are as follows:

[0046] (1) Add 0.5g of 2,5-dibromoaniline, 1g of 4-vinylpyridine, 40mg of bistriphenylphosphine palladium dichloride and 1g of anhydrous potassium carbonate into 5ml of anhydrous reagent DMF and mix, and seal the mixture in N 2 In a high-pressure reaction bottle under atmosphere, react at 100°C for 18 hours to obtain product A;

[0047] (2) Product A was completely dissolved into a black suspension with dichloromethane to obtain Product B;

[0048] (3) Product B was washed with water and saturated saline for 3 times successively to obtain product C;

[0049] (4) The product C was left to stand and layered, and the bottom dichloromethane layer was separated, dried with anhydrous magnesium sulfate, spin-dried, and finally recrystallized with absolute ethanol to obtain a fluorescent probe.

Embodiment 3

[0050] Embodiment 3: a kind of preparation method of the fluorescent probe of identifying mercury ion, the steps are as follows:

[0051] (1) Add 1.5g of 2,5-dibromoaniline, 1.5g of 4-vinylpyridine, 60mg of bistriphenylphosphine palladium dichloride and 1.5g of anhydrous potassium carbonate into 5ml of anhydrous reagent DMF and mix, and seal the mixture in N 2 In a high-pressure reaction bottle under the atmosphere, react at 120 ° C for 32 hours to obtain product A;

[0052] (2) Product A was completely dissolved into a black suspension with dichloromethane to obtain Product B;

[0053] (3) Product B was washed with water and saturated saline for 3 times successively to obtain product C;

[0054] (4) The product C was left to stand and layered, and the bottom dichloromethane layer was separated, dried with anhydrous magnesium sulfate, spin-dried, and finally recrystallized with absolute ethanol to obtain a fluorescent probe.

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Abstract

The invention discloses a fluorescent probe for identifying mercury ions, a preparation method and an identification method thereof. The chemical structure of the probe is shown in Figure 1. Its preparation method is to add 2,5-dibromoaniline, 4-vinylpyridine, bistriphenylphosphine palladium dichloride and anhydrous potassium carbonate into DMF and mix, and the mixture is sealed in N 2 In a high-pressure reaction bottle under atmosphere, react at 100-120°C for 18-32 hours to obtain product A; completely dissolve product A with dichloromethane into a black suspension to obtain product B; wash product B with water and saturated saline in sequence , to obtain product C; the product C was left to stand and layered, and the bottom dichloromethane layer was separated, dried with anhydrous magnesium sulfate, spin-dried, and finally recrystallized with ethanol to obtain a fluorescent probe. The identification method is to identify mercury ions in the DMF system. The invention is a novel fluorescent probe for identifying mercury ions, which has the characteristics of low identification cost, simple identification process, visible results, high sensitivity and good selectivity.

Description

technical field [0001] The invention relates to a reagent for identifying mercury ions and its preparation method and identification method, in particular to a fluorescent probe for identifying mercury ions and its preparation method and identification method. Background technique [0002] Mercury is one of the most dangerous metal pollutants. It is a typical heavy metal ion with strong toxicity and can cause permanent damage to the biological nervous system. Mercury in the environment is oxidized into water-soluble divalent mercury ions in the air. Once mercury ions enter the water environment, they will be converted into organic methylmercury by bacterial microorganisms, and quickly accumulate in organisms such as fish to enter food chain. Methylmercury damages the human nervous system, causing brain damage, cognitive and motor disorders, etc. The "Minamata disease" that shocked the world is a type of organic mercury poisoning. Therefore, the development of highly select...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/38C09K11/06G01N21/64
Inventor 张晓东王攀周桂林粟绍媛张胜李孟轩倪新龙
Owner GUIZHOU UNIV