Fluorescent material for detecting explosives with fluorescent lighting, preparation method and application

A technology of fluorescent materials and explosives, applied in the field of fluorescent sensors, can solve the problems of difficult detection work, sensitive to pollutants, and high instrument cost, and achieve the effects of simple preparation method, rapid fluorescence enhancement, and fast response speed.

Active Publication Date: 2017-10-27
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Due to the wide variety of explosives, it has brought many difficulties to the detection work
At present, methods such as ion mobility spectrometer and Raman spectroscopy are generally used to detect explosives. However, these methods are limited in their use due to the high cost of instruments, sensitivity to pollutants, or inconvenient detection in public places, such as colorimetry. Optical detection methods such as fluorescence method or fluorescence method have attracted widespread attention due to their fast response speed, simple and reliable instrument, and can be used for detection in public places. However, most of the methods for detecting explosives based on fluorescence are fluorescence quenching. The eyes are not sensitive to the gradual weakening or even quenching of the fluorescence intensity, so it is not easy to observe

Method used

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  • Fluorescent material for detecting explosives with fluorescent lighting, preparation method and application
  • Fluorescent material for detecting explosives with fluorescent lighting, preparation method and application
  • Fluorescent material for detecting explosives with fluorescent lighting, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] A fluorescent lighting-type fluorescent material M-TPP for detecting explosives, its preparation method and application:

[0059] (1) Preparation of M-TPP

[0060] Weigh 200mg (0.54mmol) of 1-p-bromophenyl-2,5-diphenylpyrrole (TPP), 87mg (0.64mmol) of p-tolylboronic acid, 32mg (0.027mmol) of tetrakis (triphenyl Phosphine) palladium, 229mg (2.16mmol) of anhydrous sodium carbonate in a 100mL two-necked bottle, vacuumize and fill with nitrogen to remove oxygen in the system, add 20mL of toluene and 5mL of methanol, react at 75°C for 24h, and the reaction is over Finally, toluene and methanol were removed by rotary evaporation to obtain solid 1; solid 1 was dissolved in dichloromethane, washed with water, and the organic phase was separated by column chromatography with petroleum ether / dichloromethane (1:1 by volume) as eluent, Rotary evaporation and recrystallization gave a white flocculent solid. Characterize the structure of the white flocculent solid by NMR and mass s...

Embodiment 2

[0068] A fluorescent lighting-type fluorescent material M-TPP for detecting explosives, its preparation method and application:

[0069] (1) Preparation of M-TPP

[0070] Weigh 200mg (0.54mmol) of 1-p-bromophenyl-2,5-diphenylpyrrole (TPP), 87mg (0.64mmol) of p-tolylboronic acid, 32mg (0.027mmol) of tetrakis (triphenyl Phosphine) palladium, 229mg (2.16mmol) of anhydrous sodium carbonate in a 100mL two-necked bottle, vacuumize and fill with nitrogen to remove oxygen in the system, add 20mL of toluene and 5mL of methanol, react at 90°C for 14h, and the reaction ends Finally, toluene and methanol were removed by rotary evaporation to obtain solid 1; solid 1 was dissolved in dichloromethane, washed with water, and the organic phase was separated by column chromatography with petroleum ether / dichloromethane (1:1 by volume) as eluent, Rotary evaporation, recrystallization, obtain white flocculent solid; Characterize the structure of described white flocculent solid by NMR and mass s...

Embodiment 3

[0078] A fluorescent lighting-type fluorescent material V-TPP for detecting explosives, its preparation method and application:

[0079] (1) Preparation of V-TPP

[0080] ① 200mg (0.54mmol) of 1-p-bromophenyl-2,5-diphenylpyrrole (TPP), 88mg (0.64mmol) of p-hydroxyphenylboronic acid, 32mg (0.027mmol) of four (triphenylphosphine) ) and palladium, 229mg (2.16mmol) of anhydrous sodium carbonate were placed in a 100mL two-neck bottle, vacuumed and filled with nitrogen to remove oxygen in the system, 20mL of toluene and 5mL of methanol were added, and the reaction was stirred at 75°C for 24h After the reaction, toluene and methanol were removed by rotary evaporation to obtain solid 6; solid 6 was dissolved in dichloromethane to obtain solution c; solution c was added to an excess volume fraction of 5% dilute hydrochloric acid solution, acidified, Wash and separate the liquid, take the organic phase and use ethyl acetate / petroleum ether (volume ratio 1:3) as the eluent for column ch...

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PUM

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Abstract

The invention discloses a fluorescence illuminating fluorescent material for detecting explosive, a preparing method and application, and belongs to the field of fluorescence sensors. A structural formula of the fluorescent material is as shown in formula I and formula II. When the structural formula is I, the fluorescent material is prepared by Suzuki coupling reaction of TPP and phenylboronic acid with different substituent groups at para-positions; a polymer is prepared by hydrosilylation of V-TPP and polymethylsiloxane; the fluorescent material is used for quantitative detection of the explosive and specific detecting steps comprise: dissolving the fluorescent material in a mixed solvent of tetrahydrofuran and water to obtain a fluorescent reagent; measuring the initial fluorescence intensity of the fluorescent reagent, then placing an explosive solution to be detected into the fluorescent reagent in sequence, uniformly stirring after adding every time, and instantly measuring the fluorescence intensity, wherein by comparing the change of the fluorescence intensity before and after the explosive solution is added, along with increment of the explosive, the fluorescence intensity of the fluorescent reagent is enhanced.

Description

technical field [0001] The invention relates to a fluorescent lighting-type fluorescent material for detecting explosives, a preparation method and an application thereof, and belongs to the field of fluorescent sensors. Background technique [0002] Since Nobel invented safe explosives in 1864, explosives have played an extremely important role in the development of modern society, especially in the military field, aerospace field, infrastructure construction field and some industrial fields. However, with the expansion of the application range of explosives With the emergence of new varieties of explosives and the invention of new explosives technology, the safety management of explosives has become more and more important. [0003] Especially after the "9.11" incident, a new situation has emerged in anti-terrorism. Worldwide, terrorist activities are rampant, and terrorist bombings are on the rise year by year, seriously threatening the safety of people's lives and proper...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D207/323C07D207/327C07D207/325C08G77/26C09K11/06G01N21/64
CPCC07D207/323C07D207/325C07D207/327C08G77/26C09K11/06C09K2211/1022C09K2211/1029C09K2211/1466G01N21/6428
Inventor 支俊格董立超梁开畅董宇平石建兵佟斌杨佩佩
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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