A method for easy and fast regeneration of aqueous periodate solutions from dialdehyde cellulose (DAC) production by ozone treatment is presented, along with a direct and reliable simultaneous quantification of iodate and periodate by reversed-phase HPLC. The influence of iodate and ozone concentration, solution pH, and reaction time on the regeneration efficiency was studied, as well as the reaction kinetics. Regeneration of spent periodate solutions by ozone was successfully performed in alkaline medium, which favors the formation of free (.) OH radicals, as supported by the addition of radical scavengers and quantum mechanical calculations. At pH 13 and an ozone concentration of approximately 150 mg L(-1) , periodate was completely regenerated from a 100 mm solution of iodate within 1 h at room temperature. A cyclic process of cellulose oxidation and subsequent regeneration of spent periodate with 90 % efficiency has been developed. So far, commercial applications of DAC have been hampered by difficulties in reusing the costly periodate. This work overcomes this hurdle and presents a highly efficient, clean, and low-cost protocol for the preparation of DAC with integrated periodate recycling, with the possibility of scaling the process up.
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