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In this paper, we describe a novel method for the polymerisation of acrylamide in the context of developing more effective sedimentation of red mud. Poly(o-methylstyrene-acrylamide-propenohydroxamic acid was synthesised by the copolymerisation of acrylamide as the aqueous phase and o-methylstyrene as the dispersed phase in a microemulsion system using Span-20 as a surfactant. The molecular weights were measured through the small-angle laser-light scattering method and the copolymers were characterised by Fourier transform infrared radiation, ultraviolet and Differential Scanning Calorimetry. By varying the temperature and pH during polymerisation, the optimal effect of the polymer structure on the process of red mud settling was investigated. The results show that the hydroxamic acid flocculant, which contains 10·5% o-methylphenylethylene with a molecular weight of 14 × 106, has excellent performance in the sedimentation and provides dramatically lower overflow solids at high mud settling rate compared to using hydroxamic acid alone as flocculant. [ABSTRACT FROM AUTHOR]