A kind of perylene diimide bromine substitute and method and application of preparing gas-phase sensing film of Bacillus anthracis marker based thereon
A technology of perylene diimide bromide and sensing thin film, which is applied in chemical instruments and methods, preparation of test samples, resistance to vector-borne diseases, etc., can solve the problem of few gas-phase pyridinedioic acid detection methods, complicated analytical instruments, Time-consuming equipment and other problems, to achieve the effect of miniaturization, simple device preparation method, and fast response time
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Embodiment 1
[0046] Example 1: Synthesis of PBI-1Br and preparation of picolinic acid sensor
[0047] (1) Synthesis of PBI-1Br molecule:
[0048] N,N-Diisooctylamino-perylenediimide (10 mmol, 6.15 g) was dissolved in 150 mL of CH 2 Cl 2 and slowly add 34mL Br 2 , stirring at 50°C-cooling and refluxing for 48h, the flask was removed from the oil bath, after the reaction was completed and lowered to room temperature, the reaction solution was poured into a 1000mL beaker, and 5 g of sodium thiosulfate was added to the mixture and stirred overnight , to remove the unreacted bromine, after that, the mixture was vacuum filtered and washed with ultrapure water three times to obtain a dark red solid powder, which was dried in a vacuum drying oven at 50°C for 5h. Dissolve the brominated PBI crude product in dichloromethane, add silica gel to mix the sample, dissolve the brominated PBI crude product in dichloromethane, add silica gel to mix the sample, and separate the perylene diimide monobromid...
Embodiment 2
[0057] Example 2: Synthesis of PBI-2Br and preparation of picolinic acid sensor
[0058] (1) Synthesis of PBI-2Br molecule:
[0059] N,N-Diisooctylamino-perylenediimide (10 mmol, 6.15 g) was dissolved in 150 mL of CH 2 Cl 2 and slowly add 34mL Br 2 , at 50°C with stirring-cooling and refluxing for 48h, remove the flask from the oil bath, after the reaction is completed and drop to room temperature, pour the reaction solution into a 1000mL beaker, add 5 g of sodium thiosulfate to the mixture and stir overnight , to remove the unreacted bromine, after that, the mixture was vacuum filtered and washed with ultrapure water three times to obtain a dark red solid powder, which was dried in a vacuum drying oven at 50°C for 5h. Dissolve the brominated PBI crude product in dichloromethane, add silica gel to mix the sample, dissolve the brominated PBI crude product in dichloromethane, add the silica gel to mix the sample, and separate the perylene diimide dibromide by column chromatog...
Embodiment 3
[0068] Example 3: Synthesis of PBI-3Br and preparation of picolinic acid sensor
[0069] (1) Synthesis of PBI-3Br molecule:
[0070] N,N-Diisooctylamino-perylenediimide (10 mmol, 6.15 g) was dissolved in 150 mL of CH 2 Cl 2 and slowly add 34mL Br 2 , at 50°C with stirring-cooling and refluxing for 48h, remove the flask from the oil bath, after the reaction is completed and drop to room temperature, pour the reaction solution into a 1000mL beaker, add 5 g of sodium thiosulfate to the mixture and stir overnight , to remove the unreacted bromine, after that, the mixture was vacuum filtered and washed with ultrapure water three times to obtain a dark red solid powder, which was dried in a vacuum drying oven at 50°C for 5h. Dissolve the brominated PBI crude product in dichloromethane, add silica gel to mix the sample, dissolve the brominated PBI crude product in dichloromethane, add the silica gel to mix the sample, and separate the perylene diimide tribromide by column chromato...
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