Composite based Zn/Al layered double hydroxide and biochar was successfully synthesized by liquid deposition treatment following characterization using x-ray, infrared, nitrogen adsorption desorption, thermal, and morphology analyses. Composite was used as removal agents of methylene blue in aqueous solution. Factors that influencing adsorption such as pH medium, adsorption time, initial concentration, and temperature adsorption were studied systematically. The performance of adsorbent was evaluated by adsorption regeneration process. The results showed that composite has diffraction peak at 10.10o and 21.30o due to diffraction of Zn/Al and biochar. Composite has higher surface area properties (58.461 m2/g) than Zn/Al layered double hydroxide (9.621 m2/g) and biochar (50.936 m2/g). Thermal analysis showed that composite has two endothermic peaks at 90o and 120ºC also one exothermic peak at 500ºC. Methylene blue removal on composite was achieve at pH 5 and follow PS-O kinetic model with k2 lower than starting materials. The adsorption energy of composite in the range of 17.309 kJ/mol and categorized as physical adsorption. Composite has high reusability of adsorbent until three cycles process without loss significant adsorption ability, which has different with biochar and Zn/Al layered double hydroxide.