The suspended solids in wastewater from Rekabak oilfield, Kazakhstan, were characterized and treated with flocculants to enhance settling. The wastewater contained a high concentration of total dissolved solids and calcium ion. Scanning electron microscopy and energy dispersive X-ray analyses showed that suspended solids were mainly composed of corrosion products (iron oxides) and silicon dioxide particles. Also, much salt deposition from wastewater caused a large increase in the suspended solids value. The settling of solid particles in wastewater was investigated by turbidity decrease within 60 min. The particle settling was enhanced by adding polyaluminum chloride (PAC) as coagulant and hydrolyzed polyacryamide (HPAM) or cationic polyacrylamide (CPAM) as flocculant. At optimal dose, the particle settling ability with PAC and CPAM was better than that with PAC and HPAM. Particle size analysis showed that HPAM or CPAM with high molecular weight played an important role for enlarging the particle size. The experiments with simulated wastewater showed that particle settling by using HPAM deteriorated significantly compared to that by CPAM at high calcium ion. This study provides further understanding about the effect of high salinity and Ca2+ on solids formation, flocculant performance and particle settling. Meanwhile, the results are also helpful to develop novel flocculants used for high salinity wastewater.