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Fluorescent reagent for detecting trichloromethane in air as well as preparation method and application thereof

A technology of chloroform and fluorescent reagents, applied in the field of fluorescence sensors, can solve the problems of difficult gas chloroform detection process, difficult gas chloroform environment simulation, time-consuming and energy-consuming, etc., and achieves simple and practical detection and fast detection. , time-consuming and labor-intensive effects

Inactive Publication Date: 2015-11-11
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of these methods are aimed at the detection of chloroform in solution. At the same time, due to earlier research, they have been maturely used by people. However, because most of the above methods involve relatively professional detection equipment, complicated detection processes and sample preparation processes, the cost is high and the cost is high. Time and energy, which brings great inconvenience to the detection work, will make its application subject to certain restrictions
At present, there are few studies on the detection of gas chloroform. The main reason is that the environment simulation of gas chloroform is difficult, and the detection process of gas chloroform is difficult.

Method used

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  • Fluorescent reagent for detecting trichloromethane in air as well as preparation method and application thereof
  • Fluorescent reagent for detecting trichloromethane in air as well as preparation method and application thereof
  • Fluorescent reagent for detecting trichloromethane in air as well as preparation method and application thereof

Examples

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Embodiment 1

[0047] A fluorescent reagent for detecting chloroform in the air, the reagent is a concentration of 1 × 10 -2mol / L solution of DPPTP in tetrahydrofuran.

[0048] A preparation method of a fluorescent reagent for detecting chloroform in the air as described in this embodiment, the specific steps of the method are as follows:

[0049] (1) Add 0.93mL of aniline, 1.02mL of benzaldehyde, 12mL of acetic acid and 0.172g of p-toluenesulfonic acid into a 100mL two-necked round-bottomed flask, stir evenly, heat up to 95°C, and react for 30min to obtain a liquid a; Add 0.44mL of diacetyl into liquid a dropwise while stirring, and react for 3h. After the reaction, cool to 20°C and filter to obtain solid a. The mixed solution is used as the eluent, and the solid a is separated by a decompression column, and then recrystallized with ethyl acetate and n-hexane to obtain a light yellow solid powder, which is characterized by a nuclear magnetic resonance spectrometer and a mass spectrometer t...

Embodiment 2

[0066] A fluorescent reagent for detecting chloroform in the air, the reagent is 1×10 -3 mol / L of DPPTP in dichloromethane solution.

[0067] A preparation method of a fluorescent reagent for detecting chloroform in the air as described in this embodiment, the specific steps of the method are as follows:

[0068] (1) Add 0.46mL of aniline, 0.51mL of benzaldehyde, 8mL of acetic acid and 0.086g of p-toluenesulfonic acid into a 100mL two-necked round-bottomed flask, stir evenly, heat up to 90°C, and react for 30min to obtain a liquid a; Add 0.22mL of diacetyl dropwise to liquid a while stirring, and react for 3.5h. After the reaction, cool to 25°C and filter to obtain solid a. Use ethyl acetate and n-hexane with a volume ratio of 1:4 The mixed solution is the eluent, and the solid a is separated by a decompression column, and then recrystallized with ethyl acetate and n-hexane to obtain a light yellow solid powder, which is characterized by a nuclear magnetic resonance spectrome...

Embodiment 3

[0081]A fluorescent reagent for detecting chloroform in the air, the reagent is a concentration of 1 × 10 -2 mol / L solution of DPPTP in tetrahydrofuran.

[0082] A preparation method of a fluorescent reagent for detecting chloroform in the air as described in this embodiment, the specific steps of the method are as follows:

[0083] (1) Add 4.6mL of aniline, 5.1mL of benzaldehyde, 50mL of acetic acid and 0.86g of p-toluenesulfonic acid into a 250mL two-necked round-bottomed flask, stir evenly, heat up to 100°C, and react for 30min to obtain a liquid a; Add 2.2mL of diacetyl into liquid a dropwise while stirring, and react for 4 hours. After the reaction, cool to 30°C and filter to obtain solid a. The mixed solution is used as the eluent, and the solid a is separated by a decompression column, and then recrystallized with ethyl acetate and n-hexane to obtain a light yellow solid powder, which is characterized by a nuclear magnetic resonance spectrometer and a mass spectrometer...

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Abstract

The invention discloses a fluorescent reagent for detecting trichloromethane in air as well as a preparation method and an application thereof, and belongs to the field of a fluorescent sensor. The fluorescent reagent is a DPPTP solution. The preparation method comprises: first adding aniline, benzaldehyde, acetic acid and p-Methylbenzene sulfonic acid into a reactor, uniformly stirring, heating, reacting for 10 to 30 minutes, adding butanedione to react for 3 to 4 hours, cooling to the room temperature, filtering, separating by passing through a column, re-crystallizing, and drying to obtain DPPTP; and dissolving the DPPTP in a good solvent to obtain the fluorescent reagent. The fluorescent reagent is simple and practical for detecting the content of trichloromethane in the air and has high selectivity, rapid response property and high sensitivity; no professional detection equipment is needed, a to-be-detected sample is simple to prepare, the detection cost is low, and less time and manpower are consumed.

Description

technical field [0001] The invention relates to a fluorescent reagent for detecting chloroform in the air, a preparation method and an application thereof, belonging to the field of fluorescent sensors. Background technique [0002] Volatile organic compounds (VOCs) have caused major safety hazards to the environment and human health due to their widespread existence in daily chemicals, architectural coatings, adhesives, groundwater and other fields. Chloroform, as one of the common colorless, harmful, non-flammable, and non-irritating odor organic volatile compounds, can inhibit the central nervous system of humans and animals when it exceeds a certain concentration in a gas or liquid environment. Anesthesia and coma can lead to liver and kidney damage and even death. Therefore, it is of great significance to detect solution and gas phase chloroform. [0003] In the past, the detection of chloroform mainly contained the following methods: (1) gas chromatography-mass spect...

Claims

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Application Information

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IPC IPC(8): C09K11/06C07D487/04G01N21/64
Inventor 佟斌彭喆董宇平石建兵支俊格
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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