Textile and dyeing industry have a large production network and rapid growth. However, the use of large quantities of industrial dyes and untreated wastewater pollutes the soil and water environment and directly affects human, animal and plant health. Therefore, the most important thing is to develop new adsorbents with high removal efficiency and fast separation rate to handle a large amount of waste. In this study, Mg/Al LDHs materials were successfully synthesized by hydrothermal method. The SEM images, which can be observed from the low–magnification, show that Mg/Al LDHs have morphology similar to hierarchical flower. In addition, strong intensities in XRD result indicates the high purity and good crystallization in LDH-type materials. Three factors affecting Congo red (CR) adsorption capacity include: Influence of CR solution concentration, effect of solution pH and reaction time conducted by response surface method (RSM) to find the optimal conditions for CR removal. The experimental results showed that at CR concentration 52.32 mg/L, the reaction time of 118 minutes and pH 5.8 obtained the maximum CR adsorption capacity of 42.57 mg/g. Through the surface response method (RSM) shows the optimization of the influential conditions.