Plasticizer wastewater of high concentration was experimentally studied by the process of pretreatment of acidification demulsion and Fe-C micro-electrolysis and combined process of UASB and A/O aiming at the CODCr removal in this work. The result showed that the CODCr removal rate of pretreatment process arrived at 56.2% after Fe-C micro-electrolysis reaction of 160 min on the optimal condition of pH 3.5 of acidification demulsion and 1:1.2 of the Fe/C ratio, and meanwhile improved the biodegradability of wastewater. On the other hand, UASB-A/O process could afford 80~85% of the CODCr removal rate under the optimized condition of temperature 30~35 °C, HRT 48h, pH 6.5 for UASB and HRT of aerobic zone 10~12 h, DO of about 3mg/L for A/O basin. The whole system could run at the total CODCr removal rate of 94.53~96.36%, and the system effluent CODCr was 500 mg/L or less.