This work focused on the treatment efficiency of dyestuff wastewater by hybrid processes of flotation and membrane. The removal efficiency was the highest when dodecylamine among three collectors (i.e., 1-hexadecylamine, dodecylamine, and octylamine) was employed for the removal of dyestuff. It was also found that the removal efficiency was dependent on the solution pH when the molar ratio of the collector amount to the dye concentration was less than 1.0, while the efficiency was independent when the molar ratio was greater than 1.0. On the other hand, the effect of the flow rate on the color removal efficiency was negligible under the condition of the least color removal efficiency of 30% in the flotation process, followed by microfiltration treatment. Interestingly, the addition of powdered activated carbon into the solution enhanced the color removal efficiency up to 96% because of the higher adsorption capacity of dyestuff onto microporous activated carbon.