In this paper, the phase behaviour of a cellulose nanocrystal (CNCs) dispersion in sulphuric acid solutions was investigated, aimed at the development of an energy efficient separation method for this mixture. The system in consideration was a mixture of 30 wt% aqueous sulphuric acid (ρl = 1219 kg/m3) containing 12.6 mg/ml of cellulose nanocrystals (CNCs) (ρs = 1590 kg/m3, volume fraction of CNCs less than 1%). This volume filling mixture was obtained directly from a CNC extraction process, as obtained after the hydrolysis of cotton using 64 wt% sulphuric acid at ca. 45 ̊C for 45 minutes (this condition was required for the extraction of CNCs from cotton) followed by quenching the hydrolysis with water. The CNCs form the desired product and need to be separated from the acid that can then be recycled. Conventionally this separation has been difficult and requires a large input of energy. This work addresses this problem by investigating into the phase behaviour and physicochemical and hydrodynamic character of this mixture. This understanding led to the development of a very energy efficient separation mechanism for this mixture, which is 5 orders of magnitude more energy efficient than the most widely used centrifugation systems.