There is a need for a method that can effectively remove wastewater containing small-sized particles such as TiO2. In this study, we attempted to remove TiO2 wastewater using electrocoagulation-electroflotation two-step separation. The TiO2 wastewater was effectively removed via batch electrocoagulation-electroflotation separation. However, in the batch process, the simultaneous operation of electrocoagulation and electoflotation was challenging due to the high residual turbidity. In the continuous operation, electrocoagulation and electoflotation reactors were kept separate. The turbidity removal in continuous operation was similar to that in the batch process, nevertheless, the residual Al concentration was high, leading to the conclusion that counterterm ensures against residual Al were necessary.