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
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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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