Samples from the pyrophyllite reserves in the Malatya–Pütürge region, used in the production of the whitest cement in Europe, were beneficiated using flotation. The mineralogical composition of the natural pyrophyllite, as determined using X-ray diffraction, includes pyrophyllite, kaolinite, quartz, illite–mica and feldspar. The chemical composition of pyrophyllite contains 69.75% SiO2 and 23.04% Al2O3. The pyrophyllite percentage (40–45 wt.%) of the natural sample increased to 60–80 wt.% after flotation. In flotation experiments, the effects of reagent amounts, types and their mixtures were investigated. Methyl isobutyl carbinol (MIBC) and pine oil as frothers and kerosene as a collector were used in the flotation studies. The use of reagents as mixtures has a positive effect on the beneficiation compared to use on their own. The best result was obtained for a mixture of MIBC with kerosene, which is a non-ionic hydrocarbon oil, yielding a concentrate containing 26.63% Al2O3. Improved results were also observed for kerosene plus frother mixtures after flotation cleaning circuits. The bubbles formed during flotation were photographed and the bubble diameters were measured using the ImageJ program. The Al2O3 content was evaluated by correlating the bubble diameters. In general, selectivity decreased during experiments in which bubble diameters were reduced.