Fluorescence detection test paper for quickly detecting nitroaromatic explosives, preparation method and application thereof

A technology of fluorescence detection and nitrobenzene, which is applied in the field of detection and analysis of explosives, can solve the problems of reducing the sensitivity of test paper, loss or dilution of materials, weakening of fluorescence intensity of test paper, etc., and achieves the advantages of simple production method, simple equipment and fast detection speed Effect

Inactive Publication Date: 2017-09-15
SHANDONG UNIV
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Problems solved by technology

The fluorescent materials used in traditional fluorescent test paper are all soluble. Chinese patent document CN106596493A discloses a test paper for detecting nitrobenzene explosives and its preparation method and application. Methods A water-soluble fluorescent detection system based on poly(2,5-bis(4-oxobutyrate)-1,4-phenylethylidene-alternating-1,4-phenylethylidene) (PPE-OBS) was synthesized Tes

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  • Fluorescence detection test paper for quickly detecting nitroaromatic explosives, preparation method and application thereof
  • Fluorescence detection test paper for quickly detecting nitroaromatic explosives, preparation method and application thereof
  • Fluorescence detection test paper for quickly detecting nitroaromatic explosives, preparation method and application thereof

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Example Embodiment

[0051] Example 1

[0052] 1. Take octavinyl cage silsesquioxane (OVS) and 2,2',7,7'-tetrabromo-9,9'-spirobifluorene to prepare fluorescent porous polymer as an example:

[0053] The synthetic route is as follows:

[0054]

[0055] The method for preparing fluorescence detection test paper from octavinyl cage silsesquioxane (OVS) and 2,2',7,7'-tetrabromo-9,9'-spirobifluorene is as follows:

[0056] (1) Preparation of fluorescent porous material HPP-1:

[0057] Under argon protection, combine OVS (633mg, 1mmol) with catalyst Pd(OAc) 2 (90mg, 0.4mmol), cocatalyst P(o-CH 3 Ph) 3 (193mg, 0.94mmol), acid absorbent Et 3 N (15mL) was dissolved in dry DMF (45mL), magnetically stirred at room temperature for 0.5h, and then added 2,2',7,7'-tetrabromo-9,9'-spirobifluorene (1.264g, 2mmol) , React 72h at 120°C. Post-treatment: suction filtration, washing with THF, chloroform, water, methanol, acetone, and Soxhlet extraction with THF and methanol for 24 hours, vacuum drying at 70°C for 48 hours to o...

Example Embodiment

[0064] Example 2

[0065] The method for preparing fluorescence detection test paper from octavinyl cage silsesquioxane (OVS) and 4,4'-dibromobiphenyl, the synthetic route is as follows:

[0066]

[0067] Proceed as follows:

[0068] (1) Preparation of fluorescent porous material HPP-2:

[0069] Under the protection of argon, OVS (633mg, 1mmol) and the catalyst Pd(OAc) 2 (90mg, 0.4mmol), cocatalyst P(o-CH 3 Ph) 3 (193mg, 0.94mmol), acid absorbent K 2 CO 3 (2.2g, 16mmol) was dissolved in dry DMF (45mL), magnetically stirred at room temperature for 0.5h, then 4,4'-dibromobiphenyl (1.248g, 2mmol) was added and reacted at 120°C for 72h.

[0070] Post-treatment: suction filtration, washing with THF, chloroform, water, methanol, acetone, and Soxhlet extraction with THF and methanol for 24 hours, vacuum drying at 70°C for 48 hours to obtain a white solid. The yield is about 100%.

[0071] The specific surface area and porosity of HPP-2 were analyzed with an automatic specific surface area and ...

Example Embodiment

[0075] Example 3

[0076] The method for preparing fluorescence detection test paper from octavinyl cage silsesquioxane (OVS) and tetrakis (4-bromophenyl) ethylene, the synthetic route is as follows:

[0077]

[0078] Proceed as follows:

[0079] (1) Preparation of fluorescent porous material HPP-3:

[0080] Under the protection of argon, OVS (633mg, 1mmol) and catalyst [Pd(PPh 3 ) 4 ] (63.3mg, 0.055mmol), acid absorbent Et 3 N (15 mL) was dissolved in dry DMF (45 mL), magnetically stirred at room temperature for 0.5 h, then tetrakis (4-bromophenyl) ethylene (1.29 g, 2 mmol) was added, and the reaction was carried out at 120° C. for 72 h.

[0081] Post-treatment: suction filtration, washing with THF, chloroform, water, methanol, acetone, and Soxhlet extraction with THF and methanol for 24 hours, vacuum drying at 70°C for 48 hours to obtain a yellow solid. The yield is about 100%.

[0082] The specific surface area and porosity of HPP-3 were analyzed with a fully automatic specific surfa...

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Abstract

The invention relates to a fluorescence detection test paper for quickly detecting nitroaromatic explosives, a preparation method and application thereof. The preparation method comprises the following steps: preparing a fluorescence porous material based on polyhedral silsesquioxane, and loading the fluorescence porous material on filter paper to obtain nitroaromatic explosive detection test paper. The test paper is of very bright fluorescence under an ultraviolet lamp; the explosive detection test paper is soaked into a nitroaromatic explosive solution or the explosive solution is dropped on the test paper so as to judge whether nitroaromatic explosives are contained in a sample by observing whether a fluorescence quenching phenomenon occurs on the test paper. The raw materials are easy to get, the preparation method is simple and convenient, the fluorescence intensity of the test paper is high, the detection sensitivity is high, and the test paper can be prepared through fluorescence materials with different wavelengths. The fluorescence material adopted by the test paper is an insoluble material, the influence of a solvent on fluorescence intensity weakening of the test paper caused by the attenuation of the influence material is avoided, and the fluorescence detection test paper has wide application prospects.

Description

technical field [0001] The invention relates to a fluorescence detection test paper for rapidly detecting nitrobenzene explosives, a preparation method and application thereof, and belongs to the technical field of detection and analysis of explosives. Background technique [0002] Nitrobenzene explosives are a common class of dangerous explosives, most of which are extremely explosive. Currently the most widely used nitrobenzene explosives are mainly used in military production and industrial blasting. They are highly toxic carcinogens to humans. During the production and transportation of explosives, they can easily penetrate into soil and groundwater. The environment will have a great negative impact, and it will also cause great harm to the health of the people. When humans inhale such compounds, they can cause diseases such as liver lesions, aplastic anemia, and cataracts, and even death in severe cases. Therefore, it is very important to study the impact of trace exp...

Claims

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Application Information

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IPC IPC(8): G01N21/64
CPCG01N21/643G01N2021/6432
Inventor 王灯旭孙瑞雪冯圣玉刘鸿志
Owner SHANDONG UNIV
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