A series of boehmite microspheres with highly effective adsorption performance for Congo red (CR) were successfully prepared via amides assisted hydrothermal method at 180 degrees C. Effects of dosages and hydrolysates of N,N-dimethylformamide (DMF), amides species including DMF, N-methylformamide (MF) and formamide (FA), and reaction times on their physicochemical properties were studied in detail. It was found that increase on their crystallinity and shell thickness results from the different hydrolysis rates of the amides; amorphous alumina hydrate, boehmite core-shell structure and hollow microspheres were obtained at hydrothermal times of 60, 140 and 360 min, respectively due to the Ostwald ripening. Especially, dimethylamine (DMA) as a hydrolysate of DMF, can effectively regulate the morphologies of the boehmites together with the sulfate ions, and make their pore sizes distribution (PSD) centering at 3-4 nm. Importantly, the boehmite microspheres with specific surface area of 221.3 m(2)/g shows the maximum adsorption capacity of 847.5 mg/g for CR calculated from Langmuir isotherm model, and its adsorption amount reached a high value of 484.1 mg/g at 60 min due to the mentioned PSD. This template-free hydrothermal method using DMF as precipitant provides an alternative approach for preparing high-performance hydrated alumina for environmental applications. (C) 2020 Elsevier Inc. All rights reserved.