Abstract In the context of achieving continuous synthesis of acyl peroxides using microreactors, continuous preparation of alkaline hydrogen peroxide (AHP) solution is required. However, two key issues, Na 2 O 2 precipitation and H 2 O 2 decomposition, need to be considered or addressed. For the precipitation of Na 2 O 2 during NaOH and H 2 O 2 mixing, experiments revealed that precipitation could be avoided by appropriate selection of operation window. For the risk of violent H 2 O 2 decomposition when NaOH and H 2 O 2 solutions are one‐step mixed, theoretical approaches were adopted. Simulation‐derived mixing time is combined with decomposition kinetics to find a direct relationship between operation‐structure parameters and percentage of decomposed H 2 O 2 . This percentage is estimated to be in the order of 10 −4 for micromixing devices, which indicates that micromixing devices can be used to one‐step mix NaOH and H 2 O 2 solution without causing violent H 2 O 2 decomposition. This work provides insights into the preparation of AHP solution and facilitates its continuous preparation.