A fluorescent sensor based on amino-modified polystyrene and its preparation method
A fluorescent sensor and polystyrene technology, applied in the field of sensors, can solve the problems of low volatility and difficulty in detecting micro-trace gas-phase NACs, and achieve the effects of good selectivity, good reusability, and large specific surface area
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[0039] Preferably, the preparation method of the amino-modified polystyrene is: dissolving styrene, 4-vinylbenzylamine and azobisisobutyronitrile (AIBN) in a solvent, and heating to 70±5°C for polymerization Reaction 20±5h. Further preferably, the purification step of the amino-modified polystyrene is as follows: dissolving the polymerized product in dichloromethane, and then adding ice methanol for precipitation. The ice methanol mentioned in this application means that the methanol is placed in an environment below 0°C for 5-24 hours.
[0040] The 4-vinylbenzylamine used in this application can be directly purchased or synthesized by oneself.
[0041] The present application has preferred a kind of synthetic method of 4-vinylbenzylamine, and potassium phthalimide is reacted with 4-chloromethylstyrene to obtain 4-vinylbenzylphthalamide, and 4-vinylbenzylphthalamide reacts with hydrazine hydrate to obtain 4-vinylbenzylamine. The reaction process is as follows:
[0042] ...
Embodiment 1
[0054] Amino-functionalized glass flakes (G-NH 2 ) preparation
[0055] G-NH 2 The schematic diagram of the preparation steps is shown in figure 1 shown. The cover glass was cut into 10×20 mm, and placed in a muffle furnace for calcination at a high temperature of 500° C. The purpose was to remove organic impurities on the surface to obtain a blank glass sheet (G). Then put the calcined glass piece into a flask containing a mixed solution of concentrated sulfuric acid and hydrogen peroxide (7:3), stir and react at 98°C for 1 hour, then stop the reaction, and after it is cooled to about 25°C, take it out and place it Ultrasonic wash in deionized water for 10 min, and repeat 3 times to ensure that the sulfuric acid and hydrogen peroxide are cleaned. The cleaned glass sheet was placed in a vacuum drying oven at 40° C. to remove water to obtain a hydroxylated glass sheet (G-OH).
[0056] Drop 1mL of 3-aminopropyltriethoxysilane into a three-necked flask filled with 10mL of to...
Embodiment 2
[0058] Amino-modified polystyrene (PS-NH 2 ) preparation
[0059] (PS-NH 2 ) synthetic route such as figure 2 shown. Potassium phthalimide (5.075 g, 27.4 mmol) and 4-chloromethylstyrene (4.06 g, 26.6 mmol) were dissolved in 30 mL of anhydrous DMF. in N 2 After stirring the reaction at 55° C. for 15 hours under protection, the solvent in the reaction solution was removed, and the residue was dissolved in chloroform. The solution was washed with 0.2M aqueous sodium hydroxide solution, then with water several times, and then with anhydrous MgSO 4 Drying, filtration and evaporation gave crude product. The crude product was purified by recrystallization several times in methanol solution to obtain 4-vinylbenzylphthalamide. The product was white crystals (yield: 5.46 g, 78%). 1 H NMR (CDCl 3 , ppm): 7.9-7.7 (m, 4H), 7.4-7.2 (m, 4H), 6.7 (dd, 1H), 5.8-5.2 (d, 2H), 4.8 (s, 2H).
[0060] 4-Vinylbenzylphthalimide (5.1 g, 19.3 mmol) and 80% hydrazine hydrate (1.6 g, 32 mmol) w...
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