In this work, highly dispersed silica is obtained using a precipitation technique from emulsion medium. The selected emulsifier, applied in the process, allows production of silica with almost ideally spherical particles. To examine the tendency to aggregation, the silica powder is treated with commercially available silane coupling agents: 3-mercaptopropyltrimethoxysilane (A-189), N-2-(aminoethyl)-3-aminopropyltrimethoxy silane (A-1120) and 3-methacryloxypropyltrimethoxysilane (A-174). The silica microstructure is characterised by scanning electron microscopy (SEM). Size distribution of primary particles, aggregates and agglomerates structures is determined using dynamic light scattering (DLS) method. Surface treatment of silica generally enhances powder dispersibility. The pristine spherical silica and silica modified with silanes are introduced to poly(butylene terphthalate) (PBT). Dispersion of nanosize precipitated silica particles in PBT matrix is studied by SEM technique. For the visualisation of silica particles covered by polymer layer, the composite fracture surfaces are etched by air-plasma. The agglomerates of untreated silica are not efficiently destroyed during the extrusion process, whereas surface treatment by selected silanes leads to a significant reduction of agglomerate number. However, a large number of small, strongly bonded aggregates still occupied the composite structure.