Graphical abstractAbstractRecently, layered double hydroxides (LDHs) have attracted much consideration due to their versatility and easily manipulating properties and their potential applications such as anion exchangers, support of catalysts, flame retardants, biomedical drug delivery. A novel method for the in-situ preparation in situ of LDHs, using electrocoagulation (EC) processes was developed, the EC process was performed under two different conditions, at 5?mA?m-2, changing polarity of the electrodes to find out the composition that leads to LDHs generation. The final product was characterized using XRD, BET and FTIR techniques.This method presented the following advantages: (1) Simultaneously LDHs synthesis and wastewater treatment by ion removal; (2) Polarity control allows to manipulate the M2+/M3+ molar ratio, LDHs properties and its potential applications; (3) The method spent less time to carry out the synthesis and; (4) it did not need complicated solid-liquid separation processes.