As　a　promising　conjugated　polymer,　binary　carbon　nitride　has　attracted　extensive　attention　as　a　metal-free　and　visible-light-responsive　photocatalyst　in　the　area　of　photon-involving　purification　of　water　and　air.　Herein,　we　report　sulfur-doped　polymeric　carbon　nitride　microrods　that　are　synthesized　through　thermal　polymerization　based　on　trithiocyanuric　acid　and　melamine　(TM)　supramolecular　aggregates.　By　tuning　the　polymerization　temperature,　a　series　of　sulfur-doped　carbon　nitride　microrods　are　prepared.　The　degradation　of　Rhodamine　B　(RhB)　and　the　reduction　of　hexavalent　chromium　Cr(VI)　are　selected　as　probe　reactions　to　evaluate　the　photocatalytic　activities.　Results　show　that　increasing　pyrolysis　temperature　leads　to　a　large　specific　surface　area,　strong　visible-light　absorption,　and　accelerated　electron-hole　separation.　Compared　to　bulk　carbon　nitride,　the　highly　porous　sulfur-doped　carbon　nitride　microrods　fabricated　at　650C　exhibit　remarkably　higher　photocatalytic　activity　for　degradation　of　RhB　and　reduction　of　Cr(VI).　This　work　highlights　the　importance　of　self-Assembly　approach　and　temperature-control　strategy　in　the　synthesis　of　photoactive　materials　for　environmental　remediation.　©　2017　by　the　authors.