The invention provides a preparation method of a Ni-loaded hollow carbon
microsphere NaBH4 electro-oxidation catalyst. The method comprises the steps of (1) mixing
styrene and
divinylbenzene with deionized water, introducing N2 into the
mixed solution, feeding CC14, and maintaining the temperature of 60 DEG C; after that, feeding K2S2O8 and NaCl, stirring, gradually heating up to 70 DEG C, and carrying out reaction for 10-12 hours to obtain an
emulsion; cleaning by
alcohol and centrifuging; carrying out
vacuum drying for 8-10 hours at the temperature of 50 DEG C to obtain
polystyrene microspheres; (2) putting the obtained
polystyrene microspheres into
dichloromethane, swelling for 30 minutes, feeding concentrated
sulfuric acid, and carrying out reaction for 2-4 hours at the temperature of 80-90 DEG C; adjusting the pH value to be 10-12, and
drying for 5-6 hours at the temperature of 50 DEG C to obtain
sodium polystyrenesulfonate cation exchange resin microspheres; (3) soaking the obtained
sodium polystyrenesulfonate cation exchange resin microspheres into NiCl solution for 8-10 hours, then taking out the product, and
drying for 4-5 hours at the temperature of 50 DEG C to obtain Ni-loaded cation exchange resin microspheres; and (4) calcining the Ni-loaded cation exchange resin microspheres for 5-6 hours under the
nitrogen atmosphere at the temperature of 650-750 DEG C to obtain the Ni-loaded hollow carbon
microsphere catalyst. After the method is adopted, the electro-oxidation performance and the
utilization rate of the NaBH4 can be greatly improved.