To investigate the sizing-up effects of microchannel reactors, a 0.6 mm i.d. microchannel reactor along with a 2 mm i.d. tube reactor, a 3 mm i.d. tube reactor, and a 4 mm i.d. tube reactor was assembled, and their micromixing performance was evaluated experimentally with the I − /IO 3 − parallel competitive reaction system at different Re. The results showed that at low Re, the segregation index X S (used to characterize the micromixing efficiency) of all tube reactors decreased (indicating strengthened micromixing efficiency) noticeably with increasing Re, and the X S of tube reactors with a bigger inner diameter was much larger than that of the reactors with a smaller inner diameter at the same Re. When Re was bigger than 5584, the X S of all tube reactors with different inner diameters would become almost the same as ∼3.4 × 10 −4 and remained unchanged with further increasing Re, suggesting a negligible sizing-up effect of the microchannel reactor on the micromixing performance at sufficiently high Re. In addition, Ni−Co−S composites were prepared in the four different tube reactors at the optimal Re of 6700, and the physical and electrochemical properties of the prepared Ni−Co−S composites were almost the same, further demonstrating the negligible sizing-up effects of the microchannel reactor at high Re.