[目的]焦磷酸盐体系电镀铜与化学镀镍混合废水因含有高浓度重金属离子及其络合物、氨氮、次磷酸盐、焦磷酸盐、有机物等，采用常规化学沉淀法处理难以稳定达标。本研究旨在探索芬顿氧化破络法对该类高络合电镀废水的处理效果，为工程应用提供参考。[方法]以实际车间混合废水为研究对象，通过单因素实验考察初始pH、反应时间、H₂O₂与Fe²⁺物质的量比对污染物去除率的影响，并在最优条件下分析不同稀释倍数废水的处理效果，同时采用X射线衍射仪(XRD)对沉淀产物进行表征，结合反应过程分析破络机理。[结果]芬顿反应的较佳条件为：初始pH 4，H₂O₂与Fe²⁺物质的量比2∶1，反应时间40 min。在此条件下，原水中总磷、氨氮、总铜、总镍、化学需氧量(COD)的去除率分别达到97%、70%、98%、99%和74%以上。稀释2倍后，出水各指标均可满足GB 21900—2008《电镀污染物排放标准》中“表2”要求。XRD分析表明，芬顿沉淀物呈非晶态多组分特征，证实其有效破坏了金属络合物并促使多种污染物共沉淀。[结论]芬顿法可通过产生强氧化性羟基自由基有效破络，同时去除铜镍废水中的重金属、磷、氨氮和有机物，后续结合简单沉淀即可实现稳定达标，是处理高络合电镀废水的可行技术。

[Objective] The mixed wastewater from pyrophosphate-based copper electroplating and electroless nickel plating contains high concentrations of heavy metal ions and their complexes， ammonia nitrogen， hypophosphite， pyrophosphate， and organic matter， making it difficult to consistently meet discharge standards using conventional chemical precipitation. This study aims to study the treatment efficiency of the Fenton oxidation decomplexation method for such highly complexed electroplating wastewater and to provide a reference for engineering applications. [Method] Using actual mixed wastewater from a workshop， single-factor experiments were conducted to examine the effects of initial pH， reaction time， and the molar ratio of H₂O₂ to Fe²⁺ on pollutant removal rates. The treatment efficiency at different dilution ratios was evaluated under the optimized conditions， and the precipitate was characterized by X-ray diffractometry (XRD) to elucidate the decomplexation mechanism in conjunction with the reaction process. [Result] The Fenton reaction conditions were optimized as follows: initial pH 4， molar ratio of H₂O₂ to Fe²⁺ 2:1， and reaction time 40 min. Under the conditions， the removal rates of total phosphorus， ammonia nitrogen， total copper， total nickel， and chemical oxygen demand (COD) in the raw wastewater exceeded 97%， 70%， 98%， 99%， and 74%， respectively. After two-fold dilution， all effluent parameters met the requirements of “Table 2” in the national standard GB 21900—2008 Emission Standard of Pollutants for Electroplating. XRD analysis revealed that the Fenton precipitate was amorphous and multi-component， confirming the effective destruction of metal complexes and the co-precipitation of various pollutants. [Conclusion] The Fenton process can effectively break complexes by generating strongly oxidizing hydroxyl radicals， enabling the simultaneous removal of heavy metals， phosphorus， ammonia nitrogen， and organic substances from copper- and nickel-containing wastewater. Coupled with simple subsequent precipitation， stable compliance with discharge standards can be achieved， demonstrating that the Fenton process is a feasible technology for treating highly complexed electroplating wastewater.