A kind of detection method utilizing fluorescence sensing p-trinitrotoluene

A trinitrotoluene and detection method technology, which is applied in the field of explosive detection, can solve the problems of poor solubility, complex synthesis method, sensitivity and repeatability to be developed, and achieve high solubility and high fluorescence quenching efficiency Effect

Active Publication Date: 2021-01-29
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although many fluorescent detection materials have been reported in the past, such as metal complexes, dendrimers, MOF materials, etc., their sensitivity, repeatability and applicability have yet to be developed.
Traditional conjugated polymers have been well applied in fluorescence detection, but their synthesis methods are relatively complicated and their solubility is relatively poor

Method used

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  • A kind of detection method utilizing fluorescence sensing p-trinitrotoluene
  • A kind of detection method utilizing fluorescence sensing p-trinitrotoluene
  • A kind of detection method utilizing fluorescence sensing p-trinitrotoluene

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Experimental program
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Embodiment approach

[0024] A typical implementation of the present application provides an application of a silicon-containing alkynyl carbazole hyperbranched polymer in the fluorescence detection of trinitrotoluene. The chemical structural formula of the silicon-containing alkynyl carbazole hyperbranched polymer is :

[0025] The weight average molecular weight of the hyperbranched polymer is 4800-5100 g / mol.

[0026] Preferably, the polydispersity index (PDI) of the hyperbranched polymer is 1.5-1.6.

[0027] Another embodiment of the present application provides a method for detecting p-trinitrotoluene using fluorescence sensing, adding 2,4,6-trinitrotoluene to a silicon-containing alkynyl carbazole hyperbranched polymer The solution to be tested is obtained in the solution, and the fluorescence intensity of the solution to be tested is detected. The chemical structural formula of the alkynyl carbazole hyperbranched polymer containing silicon is:

[0028] The weight average molecular weig...

Embodiment 1

[0042] Add carbazole (3.09g, 18.6mmol) into the round bottom flask, pour 100mL of glacial acetic acid, stir at reflux temperature until the carbazole is completely dissolved, then add KI (4.98g, 10mmol), KIO 3 (3.9g, 18.0mmol), potassium iodate was added three times, stirred and refluxed for 6h. After the time is up, precipitates gather on the flat bottom, and the reaction solution is cooled to room temperature and then filtered. The resulting solid is washed with dichloromethane and then with methanol. After drying, it becomes a light pink solid powder, that is, 1,3,6- Triiodocarbazole. Yield 70%. 1 H-NMR:(DMSO,400MHz),δ(ppm):7.401-7.403(d,1H),7.689-7.713(m,1H),8.025(s,1H),8.566-8.509(d,2H),11.439 (s,1H).

[0043] Take 1,3,6-triiodocarbazole (2g, 4.55mmol) into a three-necked flask, add 20mL tetrahydrofuran, 10mL triethylamine, stir to dissolve, add trimethylsilylacetylene (3.57g, 36.36mmol), C 18 h 15 P (61mg, 0.56mmol), CuI (50mg, 0.27mmol), after bubbling argon for 2...

Embodiment 2

[0046] In a 100mL flask, add triacetylcarbazole (0.5g, 2.09mmol), 3,6-dibromo-9-hexylcarbazole (3g, 10mmol), triethanolamine (10mL), toluene (30mL), mix well, and argon Gas protection for 30min, then add [(C 6 h 5 ) 3 P] 2 PdCl 2 (58mg, 0.05mmol), CuI (10mg, 0.05mmol), under the protection of argon, stirred and refluxed for 48 hours. After the reaction stopped, it was cooled to room temperature, the solution was obtained by suction filtration, and the solvent was spin-dried to obtain a crude product. The crude product was extracted with ethyl acetate Soxhlet for 24 hours to remove unnecessary small molecules to obtain the final brown solid product, denoted as P 1 , Yield: 80%. 1 H NMR: (CDCl 3 ,400MHz),δ(ppm):0.27-0.92(s,12H),0.98-1.46(d,16H),1.50-1.71(s,8H),1.73-2.02(s,2H),7.31-8.63(m ,14H).

[0047] The chemical formula of its preparation process is as follows:

[0048]

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Abstract

The invention discloses a method for detecting p-trinitrotoluene by means of fluorescence sensing. 2,4,6-trinitrotoluene is added to a solution of alkynyl carbazole hyperbranched polymer containing silicon to obtain a solution to be tested , detecting the fluorescence intensity of the solution to be tested, the chemical structural formula of the alkynyl carbazole hyperbranched polymer containing silicon is: the weight average molecular weight of the hyperbranched polymer is 4800-5100 g / mol. The detection method provided by the invention adopts the hyperbranched polymer with higher solubility, and can detect TNT in more organic solvents.

Description

technical field [0001] The invention relates to the field of explosive detection, in particular to a detection method for p-trinitrotoluene by means of fluorescence sensing. Background technique [0002] 2,4,6-Trinitrotoluene (TNT) is white or amaranth light yellow needle crystal, odorless and hygroscopic. The compound is a relatively safe explosive, resistant to impact and friction, but sudden heating of any amount can cause an explosion. The compound has moderate toxicity and can penetrate through the skin, respiratory tract and digestive tract. Its main hazard is chronic poisoning. The compound can irritate the skin locally to produce dermatitis and yellowing. The chronic effects are mainly manifested as toxic gastritis, toxic hepatitis, aplastic anemia, anemia, and toxic cataract. [0003] Due to the low cost of raw materials for TNT preparation of explosives, and the advantages of saving time and labor in construction operations (such as blasting of abandoned buildi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00G01N21/64
CPCC08G83/005C08G83/006G01N21/643G01N2021/6432
Inventor 崔月芝任金瓶陶芙蓉
Owner QILU UNIV OF TECH
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