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In the study, MgAl binary water talc (MgAl-CO3-LDHs) was firstly synthesized by a steady-state co-precipitation method and then characterized by XRD, SEM and ICP-OES methods. The effects of n(Mg2+)/n(Al3+) in mixed salt solutions, pH and roasting temperature on the properties of MgAl-CO3-LDHs were mainly explored. The optimal adsorption condition of VO3- on MgAl-CO3-LDHs was determined as synthesis temperature of 25 °C, n(Mg2+)/n(Al3+) ratio of 3:1, pH 8 ± 0.1 and roasting temperature of 517 °C. The adsorption characteristics of MgAl-CO3-LDHs on VO3- were better fitted with Langmuir's isothermal equation and quasi-secondary kinetic equation. The adsorption mechanism was close to the monolayer adsorption with a saturated adsorption capacity of 53.73 mg/g. [ABSTRACT FROM AUTHOR]