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Fluorescent material for rapidly detecting explosives as well as preparation method and application of fluorescent material

A technology for fluorescent materials and explosives, applied in the field of explosives detection, can solve the problems of high price, not easy to carry, difficult to quickly detect online, etc., and achieve the effect of easy implementation and simple preparation method

Pending Publication Date: 2022-06-24
山东产研绿色与健康研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the equipment is not easy to carry, expensive, and requires professionals to operate, and it is difficult to realize online rapid detection in different places

Method used

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  • Fluorescent material for rapidly detecting explosives as well as preparation method and application of fluorescent material
  • Fluorescent material for rapidly detecting explosives as well as preparation method and application of fluorescent material
  • Fluorescent material for rapidly detecting explosives as well as preparation method and application of fluorescent material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Synthesis of Fluorescent Material A for Rapid Detection of Explosives:

[0037] (1) In a 500 mL round-bottomed flask, add a magnetic stirring bar, add 11 g (70 mmol) of 1,8-diaminonaphthalene, 7.8 g (20 mmol) of 1,3,5-tris(p-formylphenyl)benzene, add 1.9 g (10 mmol) of sodium metabisulfite, 150 mL of ethanol, after stirring and dissolving, heat under reflux at 100 °C for 2 hours, stop heating, add an appropriate amount of dilute hydrochloric acid, adjust the pH to neutrality, and then precipitate is formed, filter, dry, and recrystallize to obtain the precipitation. Product, the preform is yellow powder, 8.2g.

[0038] The structure of the preform was characterized by NMR and mass spectrometry, and the obtained 1 H NMR spectrum as figure 1 shown, 13 C NMR spectrum as figure 2 As shown, the mass spectrum is as image 3 The specific data are as follows:

[0039] 1 H NMR(600MHz,DMSO)δ7.07-7.03(m,6H),6.86(d,J=8.2Hz,6H),6.30(t,J=7.8Hz,6H),6.12(d,J=8.1Hz , 6H), 6.01(...

Embodiment 2

[0045] Explosive Detection:

[0046]10 mg of the fluorescent material A prepared in Example 1 was dissolved in 3 mL of tetrahydrofuran, and 200 μL of the solution was drawn with a pipette and evenly coated on the filter paper strip. After the solvent was volatilized, an explosives detection test paper was prepared.

[0047] The prepared test paper is pale yellow under white light and blue under 254nm ultraviolet lamp. Add 30uL (0.01mg / mL) TNT methanol solution dropwise to the filter paper strip, the filter paper strip turns blue under white light, after the solvent evaporates, the filter paper strip is still blue, under 254nm UV lamp, the color is better than before fade. It can be seen that the fluorescent material A prepared in Example 1 can realize rapid naked-eye detection of TNT.

[0048] Dissolve 10 mg of the fluorescent material A prepared in Example 1 in 3 mL of tetrahydrofuran and place it in a cuvette for UV detection. After adding 30 μL (0.01 mg / mL) of TNT methano...

Embodiment 3

[0052] Synthesis of Fluorescent Material B for Rapid Detection of Explosives:

[0053] Using the prefabricated product prepared in Example 1 as a raw material, in a 500 mL round-bottomed flask, a magnetic stirring bar was added, and 1,3,5-tris(1H-piperidin-2-yl)benzene 5.8g (10mmol), 1,3,5-tris(1H-piperidin-2-yl)benzene was added. 4.1 g (15 mmol) of 8-dibromooctane, 2.4 g (30 mmol) of 50% sodium hydroxide solution, 740 mg (2 mmol) of TBAI, 150 mL of acetone, stirred at room temperature for 24 hours, stopped stirring and washed with suction to obtain fluorescent material B , as a brown solid.

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Abstract

The invention discloses a fluorescent material for rapidly detecting explosives and a preparation method of the fluorescent material, and the preparation method comprises the following steps: S1, mixing 1, 8-diaminonaphthalene and derivatives thereof with 1, 3, 5-tri (p-formylphenyl) benzene and derivatives thereof or 1, 3, 5-tri (4-carboxyphenyl) benzene and derivatives thereof in a first solvent, adding sodium pyrosulfite, carrying out a reflux reaction, filtering, washing, and drying to obtain 1, 8-diaminonaphthalene-1, 8-diaminonaphthalene-1, 8-diaminonaphthalene-1, 8-diaminonaphthalene-1, 3, 5-tri (p-formylphenyl) benzene; after the reaction is finished, adding an acid solution to adjust the pH value of the reaction solution to be neutral, filtering, drying and recrystallizing to obtain a prefabricated product; and S2, mixing the prefabricated product with halogenated hydrocarbon in a second solvent, adding an alkali catalyst, stirring, filtering dry weight, and performing heavy crystallization to obtain the fluorescent material. The invention also discloses application of the fluorescent material in detection of explosives. The fluorescent material disclosed by the invention has a good spatial configuration and can be used for detecting various explosives, such as 2, 4, 6-trinitrotoluene, 2, 4-dinitrotoluene, mononitrotoluene, hexogen and plastic explosives.

Description

technical field [0001] The present invention relates to the technical field of explosive detection, in particular to a fluorescent material for rapid detection of explosives and a preparation method and application thereof. Background technique [0002] Explosives mainly include some nitroaromatic hydrocarbons, nitro aliphatics, ammonium nitrates, nitrates and peroxides. [0003] The ultra-trace detection technology of explosives is mainly to detect the vapor volatilized from the explosives and the ultra-trace explosives remaining on the surface of the explosive container and any object (including the human body) that has been in contact with the explosive. technology. At present, the technical methods for the detection of ultra-trace explosives mainly include gas chromatography-mass spectrometry, gas chromatography-electron capture mass spectrometry, surface-enhanced Raman spectroscopy, X-ray imaging, thermal neutron analysis, electrochemistry and ion mobility spectrometry...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/70C09K11/06G01N21/64
CPCC07D239/70C09K11/06G01N21/643C09K2211/1044C09K2211/1007
Inventor 蒋琼李新建张彤
Owner 山东产研绿色与健康研究院有限公司
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