Preparation method of highly dispersed ultra-small zero-valence iron nano-cluster and application
A technology of nano-clusters and zero-valent iron, which is applied in nanotechnology, chemical instruments and methods, water/sludge/sewage treatment, etc., can solve the difficulty of recovery and circulation of nano-zero-valent iron, is easy to be oxidized, and cannot control nano-zero Iron valence crystal growth and other problems, to achieve high catalytic reduction performance, the effect of mild conditions
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Embodiment 1
[0024] Step S1: Add the surfactant CTAB (10mmol) to deionized water and stir for 30 minutes to form a micelle solution (its concentration is greater than the critical micelle concentration 0.9mmol / L), and FeCl 3 ·6H 2 O (1mmol) is dissolved in hydrochloric acid solution to form Fe 3+ / Hydrochloric acid mixed solution, then Fe 3+ / Hydrochloric acid mixed solution was added dropwise to the micellar solution to obtain mixed solution A;
[0025] Step S2: Add thiourea (1mmol) to deionized water and stir for 30 minutes to form a thiourea solution, dissolve sodium hydroxide (5mmol) in deionized water to form a sodium hydroxide solution, and then add the sodium hydroxide solution dropwise to In the thiourea solution, stir and mix to obtain mixed solution B;
[0026] Step S3: Drop the mixed liquid B into the mixed liquid A and stir and mix uniformly to obtain the mixed liquid C, and add NaBH 4 (25mmol) was added to the mixture C to react to prepare a zero-valent iron nanocluster suspension. ...
Embodiment 2
[0029] In order to evaluate the reactivity of the synthesized zero-valent iron nanoclusters, the zero-valent iron nanoclusters were used to catalytically reduce and remove p-nitrophenol in the solution. The specific steps are as follows:
[0030] Step S1: Add 40 mL of prepared zero-valent iron nanocluster suspension (0.46 mM) and 0.005 g of NaBH into a 50 mL Erlenmeyer flask. 4 And 1.4mL of p-nitrophenol (4mM), the solution should be magnetically stirred at 20℃;
[0031] Step S2: After stirring for 1 min, take 1.4 mL of the reaction solution for filtration, and then scan and analyze with an ultraviolet-visible spectrophotometer;
[0032] Step S3: Add 0.005g of NaBH before proceeding to the next cycle experiment 4 , Then add 1.4:mL p-nitrophenol aqueous solution (4mM), NaBH 4 And the concentration of p-nitrophenol remains constant at the beginning of each cycle. In the same NaBH 4 At the same concentration, the same zerovalent iron nanoclusters were cyclically reacted 8 times.
[0033]...
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