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The tetramethylammonium hydroxide (TMAH)-controlled alkaline etching of nickel hexacyanoferrate (NiHCF) mesocrystals is explored. The alkaline etching enables the formation of hollow framework structures with an increased surface area, the exposure of active Ni and Fe sites and the retention of morphology. The ambient reaction conditions enable the establishment of a sustainable production. Our work reveals novel perspectives on the eco-friendly synthesis of hollow and colloidal superstructures for the efficient degradation of the organic contaminants rhodamine-B and bisphenol-A. In the case of peroxomonosulfate (PMS)-mediated bisphenol-A degradation, the rate constant of the etched mesoframes was 10,000 times higher indicating their significant catalytic activity.