properties [4][5][6][7] and are also demonstrating broad application potentials in the energyrelated fields, [8][9][10][11][12][13][14][15][16][17][18] electronic devices, [19][20][21][22] and molecular chemistries. [23,24] Notably, the scalable synthesis of 2D TMDCs is an essential prerequisite, and considerable efforts have also been made, including mechanical/chemical exfoliation, [25,26] wet chemical synthesis, [27][28][29][30] ion intercalation, [31][32][33][34] and chemical vapor deposition (CVD). [35][36][37][38] However, some bottlenecks have been proposed for these approaches, such as complex growth processes, highcost, low-yield, and environmental pollution. In this regard, it is highly desirable to develop a scalable and high-efficiency method to synthesize 2D TMDCs with a high yield.As a kind of high-efficient and clean secondary energy, H 2 is emerging as a splendid alternative for fossil fuels due to its high energy density and zero carbon emission. [39] Recent years have witnessed revolutionary progress in exploiting electrocatalysts for hydrogen/oxygen evolution reactions (HER/OER). [3,40] Nevertheless, in consideration of the incompatible activity over different pH ranges, the excellent HER and OER performances are not obtained in the same electrolytes for the most of reported electrocatalysts. [41] In addition, the development of OER is sluggish and consumes a mass of electricity input producing relatively low-value products. [42] It is thus highly urgent to explore new electrocatalysts for reducing electricity consumption and enhancing the H 2 evolution. Interestingly, the sulfion oxidation reaction (SOR) is much more thermodynamically favorable than OER in view of the fact that the S 2− is more prone to offer electrons. [43] Therefore, the electrocatalytic SOR should be investigated as the alternative of OER for the H 2 evolution by coupling with cathodic HER. Moreover, as a kind of toxic by-product in the industrial production, the S 2− should be removed or recycled. [44] However, the SOR performances of most of the reported electrocatalysts are still unsatisfactory.To tackle such issues, we design a high-throughput, highyield, and low-temperature strategy for the direct synthesis of 2D VSe 2 nanosheets and SnSe 2 nanoflowers, respectively. This provides us with an opportunity for the exploration of energy applications. In particular, a plentiful of wrinkles and unique hierarchical structures are observed in ultrathin VSe 2 nanosheets and SnSe 2 nanoflowers, respectively, which offerThe electrocatalytic sulfion (S 2− ) recycling and hydrogen (H 2 ) evolution play indispensable roles in converting waste into sustainable energy and boosting hydrogen economy. However, the development of such promising technologies is hindered by the lack of electrocatalysts with low-cost, high-efficient, and robust stability. 2D VSe 2 and SnSe 2 hold great application potentials in the energy-related fields yet face daunting challenges in terms of large-scale synthesis. Herein, a gram-scale and high-yield strate...