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The flocculation and sedimentation of recalcitrant organic compounds of high molecular weight using natural polyelectrolytes, extracted from the cactus Cereus peruvianus and Opuntia ficus indica, have been studied. Organic compounds of high molecular weight from effluents of paper and pulp industries are difficult for biological degradation. However, using a mixture of aluminum salts and natural polyelectrolytes, the aggregation and settling properties of recalcitrant organics were increased if compared with conventional methods of wastewater treatment using only aluminum or iron sulfate. After flocculation, sedimentation, and filtration, the effluent was submitted to biological degradation by activated sludge process. The main advantages of using a mixture of aluminum salts and natural polyelectrolytes were shorter time of flocculation, floccus of larger size and easier for filtration.The removal efficiency observed were:85-90% of aromatic compounds, 70-85% of chemical oxygen demand,and 91-97% of colour