A kind of humic acid modified nano Fe 2 o 3 Material preparation method and application of removing estradiol
A humic acid and fe2o3 technology, applied in chemical instruments and methods, water/sludge/sewage treatment, water/sewage treatment, etc., can solve the problems of high cost, secondary pollution, cumbersome steps, etc., and achieve a large specific surface area , high removal efficiency, fast and simple preparation method
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Embodiment 1
[0019] Humic acid modified nano-Fe 2 O 3 The specific preparation method of the material is as follows:
[0020] (1) Weigh 40g of Fe(NO 3 ) 3 ·9H 2 Dissolve O in 500mL deionized water preheated to 90℃, add 300mL of 1mol / L KOH solution preheated to 90℃, and add 50mL of 1 mol / L NaHCO preheated to 90℃ 3 , Keep in a water bath at 90℃ for 48h with a lid.
[0021] (2) Pour the supernatant, precipitate and separate, remove excess OH - And NO 3 - ,dry.
[0022] (3) Weigh 25g of the obtained solid and place it in a beaker, add 500mL of humic acid solution and mix with a solid-to-liquid ratio of 1:20. Use 0.1mol / L NaOH solution or HCl solution to adjust the pH to 8.0, Shake at a constant temperature of 25°C for 48h, and then centrifuge at 4000r / min for 15min.
[0023] (4) Pour the supernatant liquid, centrifuge and rinse the solid repeatedly with deionized water until the organic carbon concentration in the supernatant liquid no longer changes significantly, freeze-dry the solid at -45°C for 48...
Embodiment 2
[0026] The humic acid modified nano-Fe prepared in Example 1 2 O 3 The material is used to remove 17β-estradiol, the specific method is as follows:
[0027] (1) Prepare a 17β-estradiol solution with a concentration gradient of 0.025-1 mg / L.
[0028] (2) Weigh 0.05g of humic acid modified nano Fe 2 O 3 Put the materials into a brown glass bottle, add 10 mL of the above-mentioned 17β-estradiol solutions of different concentrations, and shake at a constant temperature for 48 hours at 25°C.
[0029] (3) After the adsorption equilibrium, take the suspension and centrifuge, pass the 0.22μm glass filter membrane and add it to a 1mL sample bottle, and use LC-MS to determine the concentration of the solution after the reaction. The results are shown in Table 1:
[0030] Table 1: Adsorption capacity under different initial conditions of 17β-estradiol
[0031] Initial concentration (mg / L) Adsorption capacity (mg / kg) 123.26 0.621.89 0.417.61 0.210.58 0.15.98 0.051.73 0.0251.13
[0032] It can...
Embodiment 3
[0034] The humic acid modified nano-Fe prepared in Example 1 2 O 3 The material is used to remove 17β-estradiol, the specific method is as follows:
[0035] (1) Weigh 0.05g of humic acid modified nano Fe 2 O 3 Materials As for the conical flask, add 100 mL of 0.1 mg / L 17β-estradiol solution and shake at a constant temperature of 25°C for 48 hours.
[0036] (2) Centrifuge the suspension at different intervals of 0-250min, then add it to a 1mL sample bottle after passing through a 0.22μm glass filter membrane, and measure the concentration of the solution after the reaction by LC-MS.
[0037] The adsorption capacity results at different times are as follows figure 2 Shown by figure 2 It can be seen that the humic acid modified nano-Fe 2 O 3 The adsorption capacity of the material on 17β-estradiol increased with time. Between 0-120min, the adsorption capacity increased rapidly and gradually reached saturation after 120min.
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