Preparation method of fluorescent nitrogen-enriched quantum dots, products and uses thereof
A quantum dot and fluorescence technology, which is applied in the preparation of fluorescent nitrogen-rich quantum dots and its products and applications, can solve the problems of low quantum efficiency of carbon dots, complex components, difficult to repeat the reaction, etc., to achieve biological safety and biophase Good capacitive, excellent fluorescent properties, excellent repeatability effect
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Embodiment 1
[0051] The synthesis of embodiment 1 reaction raw material
[0052] Synthesis of 2-Azidoimidazole
[0053] 2-Azidoimidazole sulfate (3.30g, 25.0mmol) was dissolved in HCl aqueous solution (5.0mol / L, 20mL), cooled to 0°C in an ice-water bath, and then NaNO was added dropwise 2 (1.73g, 25.1mmol) aqueous solution and NaN 3 (1.63g, 25.1mmol) in water. The mixture was slowly increased from 0°C to room temperature, and then stirred and reacted at room temperature for 20 h. Stop the reaction with solid NaHCO 3 After adjusting the pH to neutral, ethyl acetate extraction (3 × 50mL), anhydrous Na 2 SO 4 Dry, filter, and the filtrate is spin-dried to obtain a yellow powder. The obtained yellow powder was purified by silica gel column (petroleum ether: ethyl acetate = 1:1 as the developer), and finally 2.31 g of yellow crystalline solid was obtained, with a yield of 84.7%. 1 HNMR (DMSO) δ [ppm] 6.88 (s, 1H); 13 CNMR (DMSO) δ [ppm] 139.91, 127.33, 116.24. FTIR (cm -1 )-N 3 2132c...
Embodiment 2
[0061] Example 2 Preparation of fluorescent nitrogen-enriched quantum dots
[0062]Method 1: 2-Azidoimidazole (0.360 g) in methanol solution (75 ml) was stirred and reacted at 70° C. for 24 hours. After the reaction, the methanol was removed by rotary evaporation under reduced pressure, dried, and the obtained residue was washed with ethyl acetate for 3 to 4 times until the reaction raw material (2-azidoimidazole) disappeared, and then dried; , 0.45 μm and 0.22 μm filter membranes, and the filtrate was freeze-dried in vacuum to obtain 0.120 g of a reddish-brown solid, and the yield of the crude product was 33%. The obtained crude nitrogen-rich quantum dots were further purified by Sephadex G-25 chromatographic column (the inner diameter of the chromatographic column used is 1.5cm, the height of the gel column is 20-30cm, the loading amount is <100mg, and the flow rate is about 0.2ml / min) , The developer is water:methanol=95:5, according to the elution sequence (the first elut...
Embodiment 3
[0067] Example 3 Preparation of fluorescent nitrogen-enriched quantum dots under different reaction temperature conditions
[0068] Nitrogen-rich quantum dots with different fluorescent properties can also be obtained by changing the reaction temperature for generating carbon quantum dots from 2-azidoimidazole.
[0069] After the methanol solution of 2-azidoimidazole was reacted at 50°C for 24 hours, the obtained crude nitrogen-rich quantum dots had similar spectral properties to N-dot3, and the emission peak was fixed at around 515nm, as shown in figure 2 (a). When the reaction temperature is changed to 100°C and other conditions remain unchanged, the obtained crude nitrogen-rich quantum dots have similar spectral properties to N-dot1. As the excitation wavelength changes, the emission peak changes accordingly, as shown in figure 2 (c). Therefore, by controlling the reaction temperature of 2-azidimidazole to generate carbon quantum dots, the progress of the reaction and t...
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