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A high-sensitivity fluorescent probe for detecting oxalyl chloride and its preparation method and application

A fluorescent probe and high-sensitivity technology, applied in fluorescence/phosphorescence, chemical instruments and methods, luminescent materials, etc., can solve the problems of poor selectivity, slow response speed, high detection limit, etc., achieve low detection limit, fast and sensitive response , the effect of simple steps

Active Publication Date: 2022-03-01
XUZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Due to its extremely high toxicity, fluorescent probes used in the detection of oxalyl chloride must overcome many problems such as slow response speed, high detection limit, and poor selectivity.

Method used

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  • A high-sensitivity fluorescent probe for detecting oxalyl chloride and its preparation method and application
  • A high-sensitivity fluorescent probe for detecting oxalyl chloride and its preparation method and application
  • A high-sensitivity fluorescent probe for detecting oxalyl chloride and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: the synthesis of fluorescent probe DATPA

[0027] A magnetic stirring bar was added to a 100 mL round bottom flask, and the compound of formula 2 (0.5 g, 0.7 mmol) was dissolved in acetic acid solution. Iron powder (0.47 g, 8.4 mmol) was added to the reaction flask. The reaction was stirred at 90°C for 2 hours. After that, the reaction mixture was cooled to room temperature and extracted with dichloromethane (100 mL×2). The organic layer was collected and washed with water (100 mL×3), dried over anhydrous sodium sulfate, and then evaporated under reduced pressure. The crude product was further purified using silica gel column chromatography (dichloromethane / petroleum ether, 2 / 1, V / V) to obtain the fluorescent probe DATPA as a yellow solid (0.24 g, 0.36 mmol). The yield was 51%.

[0028] The proton nuclear magnetic resonance spectrum of the prepared fluorescent probe DATPA: 1 H NMR (400MHz, CDCl 3 )δ: 7.43 (d, J = 8.3Hz, 4H), 7.32-7.26 (m, 8H), 7.21 (...

Embodiment 2

[0031] Embodiment 2: the synthesis of fluorescent probe DATPA

[0032] A magnetic stirring bar was added to a 100 mL round bottom flask, and the compound of formula 2 (0.5 g, 0.7 mmol) was dissolved in acetic acid solution. Iron powder (0.2 g, 3.5 mmol) was added to the reaction flask. The reaction was stirred at 90°C for 2 hours. After that, the reaction mixture was cooled to room temperature and extracted with dichloromethane (100 mL×2). The organic layer was collected and washed with water (100 mL×3), dried over anhydrous sodium sulfate, and then evaporated under reduced pressure. The crude product was further purified using silica gel column chromatography (dichloromethane / petroleum ether, 2 / 1, V / V) to obtain the fluorescent probe DATPA as a yellow solid (0.22 g, 0.33 mmol). The yield was 47%.

[0033] The yellow solid product prepared in this example is proved to be the fluorescent probe DATPA according to its H NMR spectrum, C NMR spectrum and high resolution mass sp...

Embodiment 3

[0034] Embodiment 3: the synthesis of fluorescent probe DATPA

[0035] A magnetic stirring bar was added to a 100 mL round bottom flask, and the compound of formula 2 (0.5 g, 0.7 mmol) was dissolved in acetic acid solution. Iron powder (0.47 g, 8.4 mmol) was added to the reaction flask. The reaction was stirred at 80°C for 2 hours. After that, the reaction mixture was cooled to room temperature and extracted with dichloromethane (100 mL×2). The organic layer was collected and washed with water (100 mL×3), dried over anhydrous sodium sulfate, and then evaporated under reduced pressure. The crude product was further purified using silica gel column chromatography (dichloromethane / petroleum ether, 2 / 1, V / V) to obtain the fluorescent probe DATPA as a yellow solid (0.23 g, 0.35 mmol). The yield was 50%.

[0036] The yellow solid product prepared in this example is proved to be the fluorescent probe DATPA according to its H NMR spectrum, C NMR spectrum and high resolution mass s...

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Abstract

The invention discloses a high-sensitivity fluorescent probe for detecting oxalyl chloride and its preparation method and application. The probe compound is 4,7-bis(4-(diphenylamino)phenyl)benzothiadiazole ‑5,6‑diamine, named as DATPA, its structural formula is shown in Formula 1, it uses o-phenylenediamino group as the reaction site of oxalyl chloride, benzothiadiazole and bis(4‑(diphenylamino)phenyl ) is a fluorescent chromophore; its preparation method is a reduction reaction in which o-dinitrobenzene units are reduced to o-phenylenediamino groups. The probe DAPTA of the present invention can be solidified and applied on filter paper to make detection test paper, so as to realize real-time and visual monitoring of oxalyl chloride in the gas phase. The probe DATPA and the test strip thereof of the present invention have the advantages of high sensitivity, good selectivity, portability and the like for the detection of oxalyl chloride, and have simple preparation steps, mild reaction conditions, and good development prospects.

Description

technical field [0001] The invention belongs to the technical field of highly toxic and dangerous gas detection, and relates to a fluorescent probe, in particular to a high-sensitivity fluorescent probe for detecting oxalyl chloride, a preparation method and application thereof. Background technique [0002] Oxalyl chloride (C 2 o 2 Cl 2 ) is a highly toxic and corrosive colorless fuming liquid with a pungent odor that can severely irritate the eyes, skin and respiratory tract. At the same time, oxalyl chloride is an important chemical basic raw material, which is widely used in industrial chemical processes to produce various organic intermediates, pesticides, medicines and coatings. Accidental leakage in industrial production may be used in chemical terrorist attacks, posing a serious threat to the environment and public safety. Therefore, it is of great significance to develop a convenient, fast and reliable method for real-time detection of oxalyl chloride. [0003]...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D285/14C09K11/06G01N21/64
CPCC07D285/14C09K11/06G01N21/643C09K2211/1014C09K2211/1051
Inventor 杨柠文程轲王晓军
Owner XUZHOU NORMAL UNIVERSITY
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