An excellent electrocatalyst for producing H2O2 was prepared from pristine CMK3 by microwave and subsequent liquid nitrogen treatments in 1 minute.

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Hydrogen peroxide (H2O2) is considered an essential chemical and is widely used in many fields. The in situ electrochemical production of H2O2 using oxygen reduction has become promising in H2O2 applications because it can reduce the danger and costs of the storage and transportation of H2O2. Developing high‐performance and metal‐free electrocatalysts with cheap and commercially available source materials for in situ H2O2 production remains challenging. Here, the N, O‐co‐doped microporous carbons derived from abundant biomass (bean dregs) were prepared by a simple hydrothermal treatment and annealing process. Electrochemical measurement results showed a high selectivity (up to 98 %) of the typical product in 0.1 M KOH, a satisfactory disk current density and a high productivity of H2O2 (380 mg L−1 h−1) with an excellent faradaic efficiency (up to 97.0 %), which were achieved through RRDE technology and flow cell. Additionally, the system equipped with a (GDE, containing N‐O‐MC‐750) as the cathode exhibited high performance in removing formaldehyde, and it may have potential application in the treatment of wastewater containing formaldehyde. This method can avoid the danger and costs of the storage and transportation of H2O2. This work is helpful for developing a high‐performance electrocatalyst for the production of H2O2, and for its practical application.