Fluorescence sensor for rapid detection of explosives and preparation method thereof, and method for rapid detection of explosives

Abstract

The invention relates to a fluorescence sensor for rapid detection of explosives and a preparation method thereof, and a method for rapid detection of explosives, wherein the fluorescence sensor and the method especially have high selectivity and sensitivity in trace detection of picric acid. The fluorescence sensor is a solution having a concentration of 1*10<-4> to 1*10<-6> mol / L and prepared by dissolving a graphene composite material in a solvent. The graphene composite material comprises graphene and a polymer as shown in a formula I which is described in the specification, wherein the polymer modifies graphene in a non-covalent bond manner via in-situ reduction of graphene oxide. When the concentration of picric acid is in a range of 1.3*10<-3> to 3.3 ppm, reduction in the fluorescence intensity of the fluorescence sensor is in linear relation with the concentration of a nitro-containing explosive, and quantitative determination can be realized. The fluorescence sensor has good fluorescence characteristics and AIE effect, can realize qualitative and quantitative determination of trace picric acid and is high in sensitivity and low in cost. The method for rapid detection of explosives is simple to operate and has good application prospects.

Description

technical field

[0001] The invention belongs to the technical field of explosive detection, and in particular relates to a fluorescent sensor for rapid detection of explosives and a preparation method thereof, and also relates to a method for rapid detection of explosives using the fluorescent sensor. Background technique

[0002] Picric acid (2,4,6-trinitrophenol, PA) is an important nitroaromatic compound widely used in leather, pharmaceutical, fuel and other fields. However, picric acid is also a common explosive and highly toxic environmental pollutant, which is toxic to the skin, eyes, and respiratory tract, and long-term exposure can also cause damage to the liver and kidneys. With the rapid development of my country's industry, picric acid discharged into the environment increases with the increase of industrial wastewater discharge, causing environmental pollution and ecological damage. Therefore, the highly sensitive detection of trace amounts of picric acid in wat...

Examples

preparation example Construction

[0070] The preparation method of above-mentioned polymer, comprises the following steps:

[0071] 1) In zinc powder, TiCl 4 Under the condition of existence, dissolve 4,4'-dibromobenzophenone and compound 1 in a solvent for reflux reaction, separate and purify to obtain compound 2; the structural formulas of compound 1 and compound 2 are as follows:

[0072]

[0073] Compound 1;

[0074]

[0075] Compound 2;

[0076] 2) In the presence of an alkaline substance and a palladium catalyst, compound 2 and pinacol borate were added to a solvent for reaction, and separation and purification were performed to obtain compound 3; the structural formula of compound 3 was as follows:

[0077]

[0078] 3) In the presence of an alkaline substance and a palladium catalyst, add 3,6-dibromocarbazole and compound 3 into a solvent for reaction, separate and purify to obtain a polymer represented by formula I.

[0079] One of the polymers with aggregation-induced luminescent effect ha...

Embodiment 1

[0103] The fluorescent sensor used for rapid detection of explosives in this embodiment is made of a graphene composite material dissolved in a solvent with a concentration of 1 × 10 -5 mol / L solution; the graphene composite material includes graphene and polymer P1, and polymer P1 modifies graphene in a non-covalent bond form. The solvent is a mixed solvent formed by mixing water and tetrahydrofuran; the volume percentage of tetrahydrofuran in the mixed solvent is 10%.

[0104] The preparation method of the fluorescent sensor for rapid detection of explosives of the present embodiment comprises the following steps:

[0105] 1) Preparation of graphene composite material:

[0106] a) Take 10 mg of graphene oxide (GO), add it into THF (10 mL), and ultrasonically disperse it for 20 min to obtain a graphene oxide dispersion;

[0107] Take polymer P1 (100mg), and dissolve it in THF (20mL) to obtain a polymer solution;

[0108] b) The graphene oxide dispersion obtained in step a)...

Embodiment 2

[0112] The fluorescent sensor used for rapid detection of explosives in this embodiment is made of a graphene composite material dissolved in a solvent with a concentration of 1 × 10 -6mol / L solution; the graphene composite material includes graphene and polymer P2, and polymer P2 modifies graphene in a non-covalent bond form. The solvent is a mixed solvent formed by mixing water and tetrahydrofuran; the volume percentage of tetrahydrofuran in the mixed solvent is 5%.

[0113] The preparation method of the fluorescent sensor for rapid detection of explosives of the present embodiment comprises the following steps:

[0114] 1) Preparation of graphene composite material:

[0115] a) Take 5mg graphene oxide (GO), add it in THF (50mL), and ultrasonically disperse it for 40min to obtain a graphene oxide dispersion;

[0116] Take polymer P2 (25mg), and dissolve it in THF (5mL) to obtain a polymer solution;

[0117] b) The graphene oxide dispersion obtained in step a) is added dro...

technical field

[0001] The invention belongs to the technical field of explosive detection, and in particular relates to a fluorescent sensor for rapid detection of explosives and a preparation method thereof, and also relates to a method for rapid detection of explosives using the fluorescent sensor. Background technique

[0002] Picric acid (2,4,6-trinitrophenol, PA) is an important nitroaromatic compound widely used in leather, pharmaceutical, fuel and other fields. However, picric acid is also a common explosive and highly toxic environmental pollutant, which is toxic to the skin, eyes, and respiratory tract, and long-term exposure can also cause damage to the liver and kidneys. With the rapid development of my country's industry, picric acid discharged into the environment increases with the increase of industrial wastewater discharge, causing environmental pollution and ecological damage. Therefore, the highly sensitive detection of trace amounts of picric acid in wat...

Examples

preparation example Construction

[0070] The preparation method of above-mentioned polymer, comprises the following steps:

[0071] 1) In zinc powder, TiCl 4 Under the condition of existence, dissolve 4,4'-dibromobenzophenone and compound 1 in a solvent for reflux reaction, separate and purify to obtain compound 2; the structural formulas of compound 1 and compound 2 are as follows:

[0072]

[0073] Compound 1;

[0074]

[0075] Compound 2;

[0076] 2) In the presence of an alkaline substance and a palladium catalyst, compound 2 and pinacol borate were added to a solvent for reaction, and separation and purification were performed to obtain compound 3; the structural formula of compound 3 was as follows:

[0077]

[0078] 3) In the presence of an alkaline substance and a palladium catalyst, add 3,6-dibromocarbazole and compound 3 into a solvent for reaction, separate and purify to obtain a polymer represented by formula I.

[0079] One of the polymers with aggregation-induced luminescent effect ha...

Embodiment 1

[0103] The fluorescent sensor used for rapid detection of explosives in this embodiment is made of a graphene composite material dissolved in a solvent with a concentration of 1 × 10 -5 mol / L solution; the graphene composite material includes graphene and polymer P1, and polymer P1 modifies graphene in a non-covalent bond form. The solvent is a mixed solvent formed by mixing water and tetrahydrofuran; the volume percentage of tetrahydrofuran in the mixed solvent is 10%.

[0104] The preparation method of the fluorescent sensor for rapid detection of explosives of the present embodiment comprises the following steps:

[0105] 1) Preparation of graphene composite material:

[0106] a) Take 10 mg of graphene oxide (GO), add it into THF (10 mL), and ultrasonically disperse it for 20 min to obtain a graphene oxide dispersion;

[0107] Take polymer P1 (100mg), and dissolve it in THF (20mL) to obtain a polymer solution;

[0108] b) The graphene oxide dispersion obtained in step a)...

Embodiment 2

[0112] The fluorescent sensor used for rapid detection of explosives in this embodiment is made of a graphene composite material dissolved in a solvent with a concentration of 1 × 10 -6mol / L solution; the graphene composite material includes graphene and polymer P2, and polymer P2 modifies graphene in a non-covalent bond form. The solvent is a mixed solvent formed by mixing water and tetrahydrofuran; the volume percentage of tetrahydrofuran in the mixed solvent is 5%.

[0113] The preparation method of the fluorescent sensor for rapid detection of explosives of the present embodiment comprises the following steps:

[0114] 1) Preparation of graphene composite material:

[0115] a) Take 5mg graphene oxide (GO), add it in THF (50mL), and ultrasonically disperse it for 40min to obtain a graphene oxide dispersion;

[0116] Take polymer P2 (25mg), and dissolve it in THF (5mL) to obtain a polymer solution;

[0117] b) The graphene oxide dispersion obtained in step a) is added dro...

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