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The electrokinetic properties and flotation of diaspore, kaolinite, pyrophyllite and illite with quatary ammonium salts collectors were studied. The results of flotation tests show that the collecting ability of quatary ammonium salts for the four minerals is in the order(from strong to weak) of octadecyl dimethyl benzyl ammonium chloride(ODBA), cetyl trimethyl ammonium bromide(CTAB), dodecyl trimethyl ammonium chloride(DTAC). Under the condition of alkalescence, it is possible to separate the diaspore from the silicate minerals such as kaolinite, illite and pyrophyllite using quatary ammonium salts as collector. Isoelectric points (IEP) of diaspore, kaolinite, pyrophyllite and illite are pH=6.0, 3.4, 2.3 and 3.2, respectively. Quatary ammonium salts can change ζ-potential of the aluminosilicate minerals obviously. The flotation mechanisms were explained by ζ-potential and Fourier transform infrared spectrum (FT-IR) measurements. The results demonstrate that only electrostatic interaction takes place between aluminosilicate minerals (diaspore, kaolinite, pyrophyllite and illite) and quatary ammonium salts.