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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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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, probes that can efficiently detect hydrazine still need to be developed.

Method used

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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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Embodiment Construction

[0031] First, at room temperature, to FeCl 3 ·6H 2 Powdered 2-naphthol (43.25 g, 0.3 mol) was added to O (162.17 g, 0.6 mol, 0.0024 mol / L) aqueous solution, and the suspension was heated to 50° C. and stirred for 3 h. After cooling and filtering, the isolated solid was dissolved in CH 2 Cl 2 , resulting in CH 2 Cl 2 After the solution was washed three times with distilled water, it was decolorized with activated carbon and dried with magnesium sulfate. After the magnesium sulfate was removed by filtration, the solvent was removed in vacuo to obtain a solid crude product. The crude product was vacuum-dried at room temperature and recrystallized with toluene to obtain white needle-like pure 1,1'-bi-2-naphthol.

[0032] Then, 1,1'-binaphthol (1.0047g, 3.5mmol), K 2 CO 3 (0.9696g, 7mmol), CuCl (0.1054g, 1.05mmol) were added to a round bottom flask, 20mL of m-xylene was added at room temperature, heated, stirred fully to dissolve, and after the solution became transparent, s...

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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...

Claims

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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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