Fenton-like process has important implications for water treatment due to its effective degradation of refractory contaminants. However, sluggish conversion of Fe³⁺ back to Fe²⁺ strongly restricts its practical application. Herein, a novel N, S co-doped porous carbon (S-ZCN) derived from ZIF-8 was prepared as a metal-free heterogeneous catalyst to accelerate the redox cycle of Fe³⁺/Fe²⁺, leading to more efficient peroxymonosulfate (PMS) activation. With only 20 mg/L S-ZCN added, sulfamethoxazole (SMX) could be removed completely by the S-ZCN/Fe³⁺/PMS system within 40 min. Reactive oxygen species (ROS) were identified by quenching experiments, electron paramagnetic resonance (EPR), and probe experiments. It was revealed that hydroxyl radical (HO^•) was the primary ROS, which contributed 79.2 % to SMX degradation. Verified by Fe concentration detection, chelating agent experiments and the results of XPS and FT-IR spectra, the synergistic effect of N, S co-doping and formation of Fe-N_x sites promoted the electron transfer from sp²-hybridized C to surface-associated Fe³⁺ to reconstruct Fe²⁺/PMS system. Based on the detection results of intermediates by Q-TOF analysis, potential degradation pathways for SMX in the S-ZCN/Fe³⁺/PMS system were proposed. Wide range of pH applicability and strong degradation to various pollutants exhibited the advantages in practical applications. This work provides a novel approach involving metal-free catalysts to break the bottleneck in the field of traditional Fenton-like reaction.

类芬顿过程由于能够有效降解难降解污染物，因此对水处理具有重要意义。^{然而，Fe 3+}向Fe ²⁺的缓慢转化严重限制了其实际应用。^{在此，制备了一种源自 ZIF-8 的新型 N、S 共掺杂多孔碳（S-ZCN）作为无金属多相催化剂，以加速 Fe 3+} /Fe ²⁺的氧化还原循环，从而产生更有效的过一硫酸盐（经前综合症）激活。^{仅添加20 mg/L S-ZCN，S-ZCN/Fe 3+}即可完全去除磺胺甲恶唑(SMX)/PMS系统40分钟内。通过猝灭实验、电子顺磁共振（EPR）和探针实验来鉴定活性氧（ROS）。结果表明，羟基自由基（H2O ^·）是主要的ROS，对SMX降解贡献了79.2%。通过Fe浓度检测、螯合剂实验以及XPS和FT-IR光谱结果验证，N、S共掺杂和Fe-N x 位点形成的协同作用促进了sp 2 杂化C到_表面^的电子转移-关联Fe ³⁺重建Fe ²⁺ /PMS系统。根据Q-TOF分析中间体的检测结果，SMX在S-ZCN/Fe ^{3+中的潜在降解途径}/PMS系统被提出。pH适用范围广，对多种污染物的降解能力强，在实际应用中展现出优势。这项工作提供了一种涉及无金属催化剂的新方法，打破了传统芬顿反应领域的瓶颈。