Large amount of coal ash is produced as industrial waste during the electricity generation through the combustion of lignite. Toxic elements arsenic exists in the coal ash, which hinders the subsequent recycling processes. Moreover, coal ash could be recycled further to retrieve scattered metals germanium and tungsten. It is believed that traditional recycling methods present barriers to scaled application, especially serious secondary pollution, such as toxic residue and waste liquid. In this work, a novel sequential vacuum distillation with disulphide method is proposed to separate arsenic, germanium and tungsten from coal ash. First, arsenic can be volatilized completely out of the reaction system at temperatures below 550 °C. Subsequently, Ge and W volatilized in the form of sulfide in the presence of Na2S2O3. The optimal condition was 1050 °C, the mass ratio of 0.6 with reaction a pressure of 1 Pa and a time duration of 120 min demonstrated the best evaporation ratio. For coal fly ash, chemical species As2S3, GeS, and WOx (x < 3)/WS2 were the main condensed products. For coal bottom ash, As2S3, GeS, and WO3/WS2 were dominant chemical components. Mechanisms for the process of release and evaporation of As, Ge, and W from coal ash, vacuum reaction, evaporation, and condensation were analyzed. In summary, the vacuum distillation method deserves to be further developed as it provides an eco-friendly method to recycle coal ash.
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