Preparation method of reactive fluorescent probe for rapid hydrazine detection

A fluorescent probe and reactive technology, applied in the field of fluorescent probes, achieves the effect of cheap and easy-to-obtain raw materials, simple synthesis steps, and specificity

Pending Publication Date: 2021-11-05
LANZHOU UNIVERSITY +1
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  • Description
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However, probes that can efficiently det

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  • Preparation method of reactive fluorescent probe for rapid hydrazine detection
  • Preparation method of reactive fluorescent probe for rapid hydrazine detection
  • Preparation method of reactive fluorescent probe for rapid hydrazine detection

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[0031] First, at room temperature, to FeCl 3 · 6h 2 O (162.17 g, 0.6 mol, 0.0024 mol / L) was added to the aqueous solution of 2-naphthol (43.25 g, 0.3 mol), and the suspension was warmed to 50 ° C for 3 h. After cooling, filtrate, dissolve the solids obtained in CH 2 CL 2 Medium, income CH 2 CL 2 After washing three times with distilled water, the activated carbon decolorized, dried over magnesium sulfate, and then removing the solvent, the solvent was removed, and the crude product was vacuum dried under vacuum, and the purity of white needle is crystallized. 1,1'-2-naphthol.

[0032] Then, 1,1'-zonnate (1.0047 g, 3.5 mmol), K 2 CO 3 (0.9696 g, 7 mmol), Cucl (0.1054 g, 1.05 mmol) was added to the round bottom flask, and 20 ml of metalloylene, heated, stirred, thoroughly stirred, and slowly added methylimidazole (157 μL, 2.0 mmol), continued to heat it to 120 ° C, reactive 20 h, and the reaction was monitored by TLC. After the reaction, the coated solvent is a yellow solid. CHCL ...

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Abstract

The invention discloses a preparation method of a reactive fluorescent probe for rapid hydrazine detection, and relates to the field of fluorescent probes. The method comprises the steps: adding powdery 2-naphthol into an aqueous solution of FeCl3.6H2O to obtain a suspension, dissolving a solid obtained by separation into CH2Cl2, and recrystallizing to obtain 1,1'-bi-2-naphthol; mixing and heating 1,1'-binaphthol, K2CO3, CuCl and m-xylene, and adding methylimidazole to obtain a yellow solid; performing recrystallization to obtain yellow powdery solid PXX; and completely dissolving the synthesized PXX in DMF in an ice-water bath at 0 DEG C, slowly dropwise adding POCl3 into the solution, heating to room temperature after dropwise adding, reacting, heating again, continuing reacting, stopping heating after reacting is finished, cooling to room temperature, precipitating, filtering, drying and recrystallizing to obtain the target probe. The method has the advantages of naked eye recognition, rapidness, high efficiency, high selectivity, strong anti-interference performance, short detection time and low production cost.

Description

technical field [0001] The invention belongs to the field of fluorescent probes, and in particular relates to a preparation method of a reactive fluorescent probe for rapid detection of hydrazine. Background technique [0002] Hydrazine (N 2 h 4 ) are widely used in the pharmaceutical and agricultural industries due to their high activity. Because of its high enthalpy, combustion can produce a large amount of heat and gas. In the aerospace industry, it is usually used as a rocket propellant. At the same time, because of its strong nucleophilicity, it can also form a variety of derivatives. However, due to its high toxicity and good water solubility, it can be miscible with water in any volume ratio, and can easily be taken orally, percutaneously or inhaled by the human body, causing serious damage to the liver, lungs, kidneys and nerves. According to the US Environmental Protection Agency (EPA), purified hydrazine is listed as a potential carcinogen with a threshold limi...

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Application Information

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IPC IPC(8): C07F1/08C09K11/06G01N21/64
CPCC07F1/005C09K11/06G01N21/6428C09K2211/188C09K2211/1011C09K2211/1044
Inventor 刘相汪硕硕王蓓刘旭明于桂琴
Owner LANZHOU UNIVERSITY
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