This paper presents the results of laboratory studies for the distillation of mercury from depleted coal sorbents produced in gold recovery factories using CIP technology. The mercury content in these materials is more than 1%. The developed technology was tested in a large-scale laboratory on a pilot vacuum sublimation electric furnace with the rheological movement of dispersed material. The use of this equipment makes it possible to demercurize various materials with fairly high moisture (up to 20%). It eliminates the use of an additional technological operation—drying the material in a vacuum drying oven. It has been shown that a high degree of mercury distillation is achieved (more than 99.8%) at 350–400 °C in the reaction space and residual pressure in the system of less than 1.33 kPa, with residual mercury content in the material of less than 0.001% (10 mg/kg), which complies with the European environmental standards. Mercury-free coal sorbents are sent for combustion for the additional extraction of precious metal composites. The proposed vacuum technology is characterized by its environmental safety because the process is performed in sealed equipment, eliminating toxic emissions of mercury vapor into the atmosphere. The proposed vacuum technology equipment is characterized by reliability and ease of use.