Co/Ni-Keggin type heteropolyacid-carbon nanofiber electrode and preparation method and application thereof
A carbon nanofiber, porous carbon fiber technology, applied in chemical instruments and methods, water/sewage treatment, chemical/physical processes, etc., to achieve the effects of high porosity, improved electrical conductivity, enhanced mass transfer and pollutant degradation
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Embodiment 1
[0031] A kind of preparation method of Co-Keggin type heteropolyacid-carbon nanofiber electrode, concrete steps are as follows:
[0032] (1) Preparation of Co-Keggin type heteropolyacid: weigh 0.712g (CH 3COO) 2 Co 4H 2 O dissolved in 16 mL of 0.5 mol / L CH 3 In the COOK solution, adjust the pH to 8 with HCl, and stir for 15 min. To the above solution was added 1.977g Na 10 (α-SiW 9 o 34 )·19H 2 O, stirred at 40°C for 45min, cooled the mixture to room temperature, and put it in a refrigerator (-5°C) for 10min. The slurry was separated by centrifugation, and the obtained product was freeze-dried, placed in a quartz crucible, and high-purity N 2 (Purity 99.999%) Calcined under atmosphere protection, gas flow rate 100-200 mL / min, temperature raised to 700 °C at a rate of 5 °C / min, and calcined for 12 hours to obtain Co-Keggin type heteropolyacid.
[0033] (2) Preparation of Co-Keggin type heteropolyacid-carbon nanofiber composites by electrospinning: take 0.5g of Co-Keggi...
Embodiment 2
[0037] A kind of preparation method of Co / Ni-Keggin type heteropolyacid-carbon nanofiber electrode, concrete steps are as follows:
[0038] (1) Preparation of Co / Ni-Keggin type heteropolyacid: weigh 0.352g (CH 3 COO) 2 Co 4H 2 O and 0.336 g (CH 3 COO) 2 Ni·4H 2 O dissolved in 16 mL of 1mol / L CH 3 In the COOK solution, adjust the pH to 8 with HCl, and stir for 15 min. To the above solution was added 1.977g Na 10 (α-SiW 9 o 34 )·19H 2 O, stirred at 40°C for 45min, cooled the mixture to room temperature, and put it in a refrigerator (-5°C) for 10min. The slurry was separated by centrifugation, and the obtained product was freeze-dried, placed in a quartz crucible, and high-purity N 2 (Purity 99.999%) Calcined under atmosphere protection, gas flow rate 100-200mL / min, temperature raised to 700°C at a rate of 5°C / min, and calcined for 12h, to obtain Co / Ni-Keggin type heteropolyacid.
[0039] (2) Preparation of Co / Ni-Keggin type heteropolyacid-carbon nanofiber composites ...
Embodiment 3
[0044] The Co / Ni-Keggin type heteropolyacid-carbon nanofiber composite material that embodiment 2 makes is used as anode in the electrochemical oxidation device (the sewage of laboratory simulation), with common refractory erythromycin and high Toxic algae toxins are the target of degradation, and their degradation efficiency on typical highly toxic and refractory pollutants in actual industrial wastewater is investigated.
[0045] like image 3 Shown is that the Co / Ni-Keggin type heteropolyacid-carbon nanofiber composite material that embodiment 2 makes is used for degrading the degradation rate figure of erythromycin and algae toxin, by image 3 It can be seen that the Co / Ni-Keggin type heteropoly acid-carbon nanofiber composite material has a removal rate of more than 90% to erythromycin in 40 minutes, and a removal rate of algae toxins in 60 minutes has reached more than 90%. And the degradation effect of algae toxin is obvious.
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