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Rapid and efficient removal of organic pollutants in water has become a challenge for human environmental protection. Herein, the adsorption performances of four 3D polyoxometalate-based metal-organic frameworks (POMOFs): H{Ln 4 L 2 (H 2 O) 21 [Zr 3 (OH) 3 (PW 9 O 34) 2 ]}⋅15H 2 O (1−4) (Ln = La (1), Ce (2), Pr (3), Nd (4); L = 3,5-pyridine dicarboxylic acid) on organic dyes were systematically studied. The results revealed that compounds 1−4 exhibited highly sensitive selective adsorption behavior to cationic dye methylene blue (MB), which was attributed to the introduction of oxygen-rich surface POM. Especially, compound 4 showed a high adsorption rate, up to 60 mg g−1 min−1, and the maximum adsorption capacity of 4 was up to 441.5 mg g−1. In addition, the adsorption process well fitted the pseudo-second-order model kinetic model and Langmuir isotherm model. This study provides a new idea for the adsorption and separation of cationic dyes in wastewater, the emphasis of which is on the construction of new materials with a large amount of charge on the surface. Four 3D polyoxometalate-based metal-organic frameworks (POMOFs) materials were adopted as adsorbents for the removal of dyes in an aqueous solution. Ultra-fast and selective adsorption towards methylene blue was observed for them with the fastest adsorption rate of 60 mg g−1 min−1 among the POM materials reported so far. [Display omitted] • POM-based MOFs 1−4 displayed a selective response to MB dye even in the presence of other dyes. • The fastest adsorption rate was observed among the POM materials reported so far. • The maximum adsorption capacity was up to 441.5 mg g−1 for 4 , higher than typical adsorbents. [ABSTRACT FROM AUTHOR]