Magnesium aluminum carbonate hydrotalcites (MgAl‐LDHs) were prepared by a coprecipitation method using magnesium nitrate and aluminum nitrate as raw materials, and then calcined at high temperature to obtain hydrotalcite‐like MgAl layered double oxides (MgAl‐LDOs). With ciprofloxacin hydrochloride as the target pollutant, and the adsorption kinetics of ciprofloxacin hydrochloride by MgAl‐LDOs were assessed. The results show that: MgAl‐LDHs and MgAl‐LDOs are both mesoporous adsorbent materials. After MgAl‐LDHs were calcined at 400°C, their layered structure began to collapse partially. At the same time, their specific surface area, pore volume, and average pore diameter increased from 123.593 m2/g, 0.666 cm3/g, and 21.54 nm to 185.908 m2/g, 1.414 cm3/g, and 30.42 nm, respectively. The ability of MgAl‐LDOs to remove ciprofloxacin hydrochloride in water is much greater than that of MgAl‐LDHs. The research has shown that when the concentration of ciprofloxacin hydrochloride solution is 10 mg/L, at a pH of 5, and a temperature of 25°C, the equilibrium adsorption capacity can reach 22.69 mg/g in 420 min. The results of the quasi‐first‐order kinetic model and the quasi‐second‐order kinetic model show that the parameter R2 of MgAl‐LDOs adsorption of ciprofloxacin hydrochloride exceeds 0.94. The fitting parameters qe = 22.96 mg/g (10 mg/L) and qe = 107.02 mg/g (50 mg/L) in the quasi‐first‐order kinetic model, and the fitting parameters qe = 25.02 mg/g (10 mg/L) and qe = 112.72 mg/g (50 mg/L) in the quasi‐second‐order kinetic model are practically consistent with the measured equilibrium adsorption capacity.

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