Pd/Fe@Fe3O4 compound catalyst as well as preparation method and application thereof
A composite catalyst, sodium borohydride technology, applied in the field of environmental remediation and water treatment, can solve the problems of incomplete degradation of pollutants, secondary pollution of iron sludge, easy loss of catalysts, etc., to reduce secondary pollution, slow down passivation and The effect of agglomeration and promotion of Fenton reaction
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Embodiment 1
[0040] (1) Culture Enterococcus faecalis in LB medium at 37°C for 3 days, filter, wash with deionized water for 3 to 5 times, and make freeze-dried powder for later use; take 0.2g freeze-dried powder into a container , add chloropalladium acid solution, cultivate at 37°C for 30 minutes to obtain a bacterial suspension, the concentration of chloropalladic acid in the bacterial suspension is 1.5mmol / L, and the concentration of the freeze-dried powder is 3g / L; add sodium formate to the above mixture The solution was incubated at 37°C for 48 hours and collected by filtration; then, it was ultrasonically crushed for 30 minutes, centrifuged at 10,000 rpm for 6 minutes, and washed by centrifugation until the supernatant was neutral; finally, it was dried at 80°C for 6 hours to obtain biologically recovered palladium;
[0041] (2) Under ultrasonic conditions, 1.35g FeCl 3 ·6H 2 O and 1.39 g FeSO 4 ·7H 2O was mixed evenly in 20 mL of water, and added dropwise to 10 mL of ammonia wat...
Embodiment 2
[0045] Other steps are with embodiment 1, just in step (3) biological recovery palladium is in Pd / Fe@Fe 3 o 4 The mass fractions in the composite catalysts are 1%, 2%, 3%, 5% and 10%; Pd / Fe@Fe 3 o 4 Fe and Fe in the composite catalyst 3 o 4 The mass ratio of sodium borohydride is 1:1; the molar ratio of sodium borohydride to ferrous salt is 2.5:1. Then vacuum filtration and cleaning with anaerobic water until the filtrate was neutral; then freeze-dried at -40°C for 48 hours, and ground into powder to prepare composite catalysts with different palladium content, which were stored in centrifuge tubes for later use.
Embodiment 3
[0047] Investigate a Pd / Fe@Fe prepared by Example 1 under different concentrations of hydrogen peroxide 3 o 4 The degradation efficiency of composite catalyst to diclofenac sodium (DS):
[0048] Dilute the DS stock solution to 10 mg / L with ultrapure water, and add 0.5 mol / L H 2 SO 4 and NaOH solution to adjust the initial pH of DS solution to 7.0. Take 100mL of 10mg / L DS solution in the serum bottle, add the Pd / Fe@Fe freshly prepared in Example 1 with a loading rate of 1g / LPd at 5% 3 o 4 The compound and the hydrogen peroxide with concentrations of 0.01mol / L, 0.03mol / L, 0.05mol / L, 0.1mol / L and 0.3mol / L are sealed, ultrasonic (200W) for 5min to make it evenly mixed, and placed at 25°C. In a constant temperature shaker at 165r / min, samples were taken every 20 minutes, and immediately filtered with a 0.22 μm filter head, quenched to be tested, and the reaction time was 2 hours. Three parallel experiments were performed. The mensuration of diclofenac sodium concentration: t...
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