Low density, highly porous and hydrophobic cellulose-based new material, Xerocellulose, was prepared and characterised. First, tritylcellulose with different degrees of substitution (DS) was synthesised in homogeneous conditions. Xerocellulose was then prepared from tritylcellulose via dissolution-coagulation-drying route, similar to other polysaccharide-based aerogels, but drying was performed in ambient room conditions. The new material has a density between 0.1 and 0.2 g/cm(3) and is highly hydrophobic with contact angle 140A degrees for DS = 0.72. Compared with cellulose aerogel and pristine microcrystalline cellulose, Xerocellulose obtained from tritylcellulose with DS = 0.72 showed a drastically decreased water vapour uptake. The evolution of Xerocellulose density and morphology as a function of the DS is presented and discussed.