The　fabrication　of　non-metallic　semiconductor　heterojunction　with　superior　redox　capability　for　hydrogen　(H2)　evolution　from　water　and　environmental　remediation　has　been　emerging　as　a　prospective　strategy.　Herein,　a　novel　two-dimensional　(2D)　g-C3N4/Ni-MOF　Z-scheme　heterojunction　was　prepared　by　a　facile　sonication-gel　self-assembly　method　with　g-C3N4　and　nickel　metal-organic　framework　(Ni-MOF)　nanosheets.　The　ultra-thin　nanosheet　structure　of　Ni-MOF　was　conducive　to　the　formation　of　stable　2D　heterojunctions.　The　opposite　surface　charge　and　matched　band　difference　caused　the　charge　flow　from　g-C3N4　to　Ni-MOF,　resulting　in　an　interfacial　built-in　electric　field.　The　optimized　NMF/CN-9　attained　the　optimal　3aphotocatalytic　activity　towards　the　degradation　of　tetracycline　(TC)　and　H2　evolution　from　water.　Under　visible　light　irradiation,　the　reaction　rate　for　TC　degradation　(0.00497　min−1)　and　H2　evolution　(15.6　μmol·h−1)　over　NMF/CN-9　was　nearly　2.4　and　2.1　folds　higher　than　that　of　g-C3N4,　respectively.　Besides,　the　photocatalytic　performance　of　NMF/CN-9　was　also　nearly　2　times　higher　than　that　of　g-C3N4　under　simulated　solar　illumination.　Such　improvements　were　originated　from　higher　photo-excited　charge　separation　and　superior　redox　ability　derived　from　Z-scheme　interfacial　charge　transfer.　A　possible　photocatalytic　mechanism　was　also　proposed　and　the　results　indicated　that　efficient　photo-induced　electrons　and　reactive　hole　(h+),　superoxide　radical　(·O2-)　and　hydroxyl　radical　(·OH)　played　a　major　role　during　the　photocatalytic　route.　This　work　offers　an　intense　insight　into　the　construction　of　non-metallic　semiconductor　2D　heterojunctions　for　H2　evolution　and　environmental　wastewater　treatment.　©　2024　Elsevier　B.V.