Novel processable sulfur copolymer (poly(S-r-CEA)) was synthesized via facile inverse vulcanization of elemental sulfur with 2-carboxyethyl acrylate (CEA). This polysulfide was electrospun producing sulfur-rich nanofiber and tested for heavy metal sequestration. Adsorption experiments show very high and efficient Hg2+ adsorption. This work extends the novelty of inverse vulcanization chemistry by developing method for preparation of material based on inverse vulcanized polysulfide. Consequently, a new and cheap yet effective material was prepared for heavy metal sequestration from contaminated water. This work was supported by Basic Science Research Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Science, ICT and Future Planning (2015R1A2A1A15055407) and by the Ministry of Education (No. 2009-0093816).