New hyaluronic acid-based hydrogels have been synthesized. The carboxylate groups of hyaluronan were activated in order to bind the amino terminal groups of the di-amine cross-linking reagent. Different hydrogels were obtained according to the different di-amine cross-linking agents (1,3-diaminepropane, 1.6-diaminohexane, PEG500 di-amine. and PEG800 di-amine). The cross-linked polymer (C.L.Hyal) was then sulphated (C.L.HyalS) by a heterogeneous reaction using sulphur trioxide pyridine complex (SO3-Py). The thermo-mechanical properties and swelling degree were evaluated and are discussed in relation to the chemical structure and the hydrophilic character of the gels. The different behaviours of C.L.Hyal and C.L.HyalS indicate the important role of sulphated groups.