Metal particle on a support material should be small and homogeneous in size, which is desirable when using it as a catalyst. In this study, we investigated to introduce Pd nanoparticles (NPs) with narrow size distribution into NH2‐MIL‐53, which was prepared by the reaction of aluminum(III) nitrate with 2‐aminoterephthalic acid. Only by immersing it in an aqueous PdCl2 solution, followed by the reduction with NaBH4, Pd NPs of about 2 nm with unform distribution were formed in NH2‐MIL‐53 up to 3.5 wt.% Pd loadings. Amino group on the linkers in NH2‐MIL‐53 played a critical role for the introduction of (PdCl3)– as a precursor for Pd NPs, while no Pd was introduced into MIL‐53 without amino group. The obtained catalysts (Pd@NH2‐MIL‐53) showed high catalytic performance for reduction of nitrite in water. The specific activity per Pd site exposed on the surface changed greatly depending on the Pd loadings despite the size of Pd NPs unchanged. Pd@NH2‐MIL‐53 with low Pd loadings showed higher specific activity (TOF = 2.9×102 h‐1), which might be due to the preferential exposure of Pd(111) facet on Pd NPs.
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