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A kind of fluorescent nanomaterial and application thereof for detecting pentaerythritol tetranitrate

A technology of pentaerythritol tetranitrate and fluorescent nanomaterials, which is applied in the field of fluorescent nanomaterials, can solve the problems of limited response rate and sensing performance, poor gas permeability of sensing films, fluorescence quenching of fluorescent molecules, etc., and achieves good application prospects , The preparation method is simple and fast, and the effect of easy separation

Active Publication Date: 2020-07-31
INST OF ANALYSIS GUANGDONG ACAD OF SCI (CHINA NAT ANALYTICAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the lack of benzene ring structure and generally low saturated vapor pressure of nitrate ester explosives, it is often difficult to achieve trace detection through simple gas phase contact, especially the saturated vapor pressure of PETN is only 0.12ppt. There are few reports on the gas phase detection technology
Traditional fluorescent sensing and detection methods are often realized by charge transfer between the electron-rich structure and the nitro group on the explosive, but the electron-rich structure usually leads to serious self-aggregation, which causes fluorescence quenching of fluorescent molecules.
In addition, the electron-rich structure usually contains polyphenylene ring system, and the gas permeability of the sensing film made of it is often poor, which limits the response rate and sensing performance.

Method used

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  • A kind of fluorescent nanomaterial and application thereof for detecting pentaerythritol tetranitrate
  • A kind of fluorescent nanomaterial and application thereof for detecting pentaerythritol tetranitrate
  • A kind of fluorescent nanomaterial and application thereof for detecting pentaerythritol tetranitrate

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Experimental program
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Embodiment 1

[0034] Embodiment 1: The present invention is used for the preparation method of the fluorescent nanomaterial of detecting pentaerythritol tetranitrate

[0035] (1) Synthesis of nano-silica microspheres

[0036] Take 50mL of ethanol, 5.6g of ammonia water (30%) and 4.5g of water in a 250mL flask, dissolve 2.5g of tetraethoxysilane in 5mL of ethanol, quickly add to the above solution, and stir vigorously at 40°C for 5 minutes. Dissolve 2.4 g of vinyltriethoxysilane (the molar ratio of tetraethoxysilane (TEOS) to vinyltriethoxysilane (VTEOS) is 1:1) in 5 mL of ethanol, and add it dropwise to the above solution . After the addition, continue to stir and heat vigorously for 30 minutes, then centrifuge the mixed solution at a rate of 3500 rpm, wash with ethanol and water several times, and dry to obtain 3.2 g of white powdery nano-silica microspheres with a particle size of 200- 300nm.

[0037] (2) Synthesis of fluorene-substituted nano-silica microspheres

[0038]Weigh 450mg o...

Embodiment 2

[0044] The sensing thin layer based on compound 1 was prepared on the quartz substrate by solid phase transfer technique. The preparation method of the sensing thin-layer device comprises the following steps: dispersing the fluorene-substituted nano-silicon oxide microspheres in ethanol at a concentration of 3 mg / mL, and slowly dropping the dispersion into distilled water drop by drop after ultrasonic oscillation, A thin layer of nano-microspheres is formed on the surface of the solution, and the quartz plate substrate is pulled out of the liquid surface from the ethanol-water dispersion at a fixed angle, so that the thin layer of nano-microspheres evenly covers the surface of the quartz plate to form a thin sensing layer. Place in a vacuum oven to drain the residual liquid.

[0045] The fluorescence spectrum and photostability of the sensing thin-layer device can be tested by an ultraviolet-visible fluorescence spectrometer. When testing the sensing performance, put a little...

Embodiment 3

[0051] A solid phase transfer technique similar to that of Example 2 was used to prepare a sensing thin layer based on Compound 1 on a quartz plate substrate. The dispersion concentration of the microspheres in ethanol was 3 mg / mL, which was dropped into distilled water to obtain a thin layer of nano-microspheres. Cover the surface by pulling the quartz sheet and allow to dry. When testing the sensing performance, place the blank, trinitrotoluene (TNT), RDX, and trinitrophenol (PA) samples at the bottom of four sealed quartz cuvettes, and cover them with absorbent cotton Sealed for several hours before use. Put the prepared sensing thin-layer device into the cuvette and seal it, and use the ultraviolet-visible fluorescence spectrometer to quickly measure the change of its fluorescence emission curve, and compare the influence of four analytes on the fluorescence emission peak intensity at 355nm. Such as Figure 4 As shown, after 10 minutes of exposure to different analytes, ...

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Abstract

The invention discloses a fluorescent nano material for detecting PETN (Pentaerythritol Nitrate), which is as shown in a structural formula I shown in the description. A radical group containing double bonds coats the peripheries of nano silica microspheres of which the particle size is 200 to 300 nm, and fluorene is introduced in the double bonds so as to use the double bonds as a sensing unit. The fluorescent nano material disclosed by the invention is simple in preparation method, high in yield, easy to separate and high in purity, is capable of quickly and accurately detecting free PETN molecules in a gas phase according to the change of the strength and the color of fluorescent light and has very high sensitivity and selectivity, gas-phase trace detection on the PETN is realized, andcontribution to personal safety of citizens and social stability is made.The formula is shown in the description.

Description

Technical field: [0001] The invention relates to the field of chemical sensor materials, in particular to a fluorescent nanometer material for detecting pentaerythritol tetranitrate and an application thereof. Background technique: [0002] Due to the constant changes in the world situation, the research and development of explosive detection technology has been paid more and more attention by research groups at home and abroad. Common detection techniques include gas chromatography-mass spectrometry, ion mobility spectrometry, surface-enhanced Raman spectroscopy, and biological detection methods. The development of these traditional detection technologies is relatively mature, but they often require the support of large instruments, which have defects such as high price, complicated operation, and inconvenient portability. Colorimetric and fluorometric methods have attracted widespread attention due to their fast response, visual recognition, and simple instrumentation. C...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64C09K11/06C09K11/02B82Y20/00B82Y30/00B82Y40/00
CPCB82Y20/00B82Y30/00B82Y40/00C07B2200/11C09K11/02C09K11/06G01N21/6402
Inventor 高宜逊
Owner INST OF ANALYSIS GUANGDONG ACAD OF SCI (CHINA NAT ANALYTICAL
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