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Current treatments (e.g., the Claus process) are energy\u2010intensive and generate secondary waste. Electrochemical sulfide oxidation (SOR) offers an energy\u2010efficient alternative for simultaneous H\n                    <jats:sub>2<\/jats:sub>\n                    S removal and recovery of high\u2010purity hydrogen and sulfur, but its application is hindered by anode deactivation due to sulfur deposition. Here, we report a dynamic microenvironment engineering strategy using pulsed electrolysis (PE) to achieve sustainable SOR. Coupled with a Sc\u2010doped NiFe\u2010LDH electrocatalyst optimized for intermediate adsorptions, we achieve periodical modulation of metal\u2010sulfur redox, enabling efficient sulfur release and active site regeneration. This synergy enables continuous H\n                    <jats:sub>2<\/jats:sub>\n                    S destruction and hydrogen production for over 500 h with a Coulombic efficiency of 99.8% and a low energy consumption of 2.19\u00a0kWh m\n                    <jats:sup>\u22123<\/jats:sup>\n                    . Furthermore, using bio\u2010derived formic acid, the acidification process is capable of co\u2010production high\u2010purity sulfur (99.5%) and sodium formate. This integrated process, validated also with industrial syngas and seawater electrolyte, increases the overall profit by 121% to US$1,294.7 per tonne of hydrogen. Overall, this report demonstrates a circular and economically viable strategy for H\n                    <jats:sub>2<\/jats:sub>\n                    S treatment and resource recovery, which is also implacable to other electrochemical systems facing catalyst poisoning.\n                  <\/jats:p>","DOI":"10.1002\/adma.73096","type":"journal-article","created":{"date-parts":[[2026,4,17]],"date-time":"2026-04-17T10:30:57Z","timestamp":1776421857000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["Pulsed Electrolysis Prevents Sulfur Poisoning for Sustained Sulfide Valorization"],"prefix":"10.1002","volume":"38","author":[{"given":"Zhiyan","family":"Hou","sequence":"first","affiliation":[{"name":"State Key Laboratory of Materials Low\u2010Carbon Recycling College of Materials Science and Engineering Beijing University of Technology  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yangbo","family":"Ma","sequence":"additional","affiliation":[{"name":"Department of Chemistry The University of Hong Kong  Hong Kong SAR China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yufeng","family":"Wu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Materials Low\u2010Carbon Recycling College of Materials Science and Engineering Beijing University of Technology  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Weijin","family":"Cao","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Materials Low\u2010Carbon Recycling College of Materials Science and Engineering Beijing University of Technology  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5404-3215","authenticated-orcid":false,"given":"Zhengxiao","family":"Guo","sequence":"additional","affiliation":[{"name":"Department of Chemistry The University of Hong Kong  Hong Kong SAR China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9710-812X","authenticated-orcid":false,"given":"Changlong","family":"Wang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Materials Low\u2010Carbon Recycling College of Materials Science and Engineering Beijing University of Technology  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2026,4,17]]},"reference":[{"key":"e_1_2_8_2_1","doi-asserted-by":"crossref","unstructured":"U.S.G. 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