Aromatic sulfonates having, respectively, preferential oil-, and water- and alcohol-solubility are prepared by reacting aromatic compounds and sulfuric acid in a medium capable of liquid-liquid extraction with water; the product stream is then subjected to countercurrent extraction against water in a first multi-stage column; the water stream is next subjected to countercurrent extraction against a water-immiscible higher alcohol in a second multi-stage column; and the sulfonate having preferential water- and alcohol-solubility, which has transferred from the product stream, to the water stream, and finally to the higher alcohol, is recovered from the latter as the free acid or as a salt thereof. The process is especially adapted to the production of dinonylnaphthalene disulfonic acid.