Experiments on the treatment process of 1,2,4-acid wastewater combined ferric-carbon microelectrolysis with Fenton oxidation process are carried out. The 1,2,4-acid wastewater is produced in the production process of 6-nitry（6-nitro-1-diazo oxygen naphthalene-4-acid）. The experimental conditions of Ferric-Carbon microelectrolysis, including pH value, react time, react temperature, Fe/C ratio and dosage of active carbon are studied. Fenton oxidation conditions of pH value, dosage of H2O2 and the economy data of the process are analyzed. Through single-factor experiments, the conditions for treating acid wastewater are found out. pH value is 1, Fe and C mass ratio is 3〖DK〗∶1, and iron-carbon micro-electrolysis reaction time is 3 h. Filter the iron-carbon micro-electrolysis water to adjust its pH value into 3, and then adding 2.5% wastewater of H2O2 with mass fraction of 30 %, react at room temperature for 1 h, adjust the pH value into 7~8, and then filter the iron-carbon micro-electrolysis water. The removal efficiency of COD of raw water can be improved to more than 95%. The cost of wastewater treating is 5.4 yuan/m3.〖HQ〗