Abstract: The high surface area activated carbons by KOH activation were made by the mixing method of solid and solid, using petroleum coke as raw material. The effects of technological parameters on the adsorption capacity of Iodine and methylene blue of the resultant activated carbons was investigated. The porous structure of high surface area activated carbon was analyzed by adsorption method of liquid nitrogen. The results showed that pretreatment temperature, flow rate of nitrogen activation temperature, ratio of alkali to raw material, particle size of raw material, and activation time had a remarkable effect on the adsorption capacity of Iodine and methylene blue. The optimum adsorption capacity of Iodine and methylene blue accursed with the variety of each of technological parameters. High surface area activated carbon was prepared with BET surface area more than 3 000 m2/g, pore volume of 1.80 cm3/g, the adsorption capacity of Iodine of 2 714 mg/g and that of methylene blue of 510 mg/g. The adsorption characteristics of activated carbon could be regulated by the modifying the petroleum coke and optimization of technology parameters.