The effects of different activation temperatures (Ta), ranging from 300 to 750 °C, on the ash content, yield, ignition point, microcrystalline structure, surface functional group, pore structure, and adsorption performance of activated carbon in preparing activated carbon by phosphoric acid (H3PO4) were systematically studied. The yield and volatile content of activated carbon decreased with the increase of Ta, while the ash content, ignition point, and graphitization degree showed the opposite results. The turning point of ash content increasing rate of activated carbon occurred at 500 °C. The thermal decomposition temperature of phosphonate compounds was approximately 450 °C. With increased Ta, micropores were generated first, followed by mesopores. The ignition point of activated carbon was related to the volatile content and the degree of graphitization. Activated carbon with low ash content, high yield, well-developed pore structure and good adsorption performance was prepared at 350 to 425 °C. With increased Ta, the volatile content decreased, and the ignition point of activated carbon increased. At Ta higher than 500 °C, the aromatic and condensed ring structure, graphitization degree, and mesopore ratio of the activated carbon increased, yielding decreased adsorption performance.