A dihydroxybenzene isomers electrochemical sensor based on bamboo activated carbon (MCPBAC) sensitive material activated by mechanochemistry and low-dosage phosphoric acid was fabricated in this work. The sensor, modified by MCPBAC with GCE, can significantly distinguish and sensitively measure hydroquinone (HQ) and catechol (CC). The MCPBAC exhibits a well-developed porous structure, high specific surface area, and good electrical conductivity. Using differential pulse voltammetry (DPV), wide linear ranges for both HQ and CC are 0.6-600 μM, with low detection limits (S/N = 3) for both of 0.2 μM. The dihydroxybenzene isomers electrochemical sensor has wide application prospects in the determination of trace HQ and CC in environmental water.