Monoethylene glycol (MEG) is a desiccant widely used in the Oil and Gas and Sugar Cane Alcohol industries and generates a large volume of MEG-water mixture effluent. This original study explores the use of a new pilot-scale distillation system for separating MEG from a MEG-water mixture. The distillation tests were performed with a single-tube falling film distillation column assisted by a thermosyphon system operating at atmospheric pressure (Destubcal Technology). The results attained high MEG contents, with a MEG loading of 66.00% (m/m), yielding a MEG separation of 88.61%. Additionally, a distillation arrangement with two single-tube falling film distillation columns in series was able to reach values of separation similar to those used by companies in the Oil and Gas sector, while operating at atmospheric pressure. It was also found that Destubcal Technology leads to a 46.93% reduction of the energy required and is more compact than a conventional-industrial distillation column. (C) 2019 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.