Abstract The stabilisation of insoluble lignin microparticulates produced through solvent attrition in aqueous media containing surfactants has been investigated. In the absence of added surfactants, addition of solvent solubilised lignin to water caused extensive precipitation and annealing of lignin, leading to the formation of large, agglomerated structures in the approximate size range of 20–200 μm. Addition of high HLB non-ionic surfactants (Polysorbate 20/sucrose ester) to the aqueous solution prior to lignin precipitation had only limited effect on the size of agglomerates produced, with a partial decrease in mean aggregate size at elevated surfactant concentrations, and no observed effect at low surfactant concentrations. In contrast, addition of either negatively (SDS) or positively (CTAB) charged ionic surfactants at concentrations Findings indicate that adsorption of charged surfactants to the surface of lignin particles during precipitation is able to provide effective electrostatic stabilisation; however, no such stabilising effect is provided by non-ionic surfactants. Furthermore, it appears that the size and stability of the particles produced is dependent on the conditions within the aqueous phase during precipitation. In this way, it may be possible to produce lignin microparticles with tailored particle distributions.