The invention discloses a preparation method of octaphenyl
silsesquioxane. The preparation method comprises the steps of firstly, placing a reactor into an ice-water bath, adding a
mixed solution of an
organic solvent and deionized water into the reactor, and then, adding
phenylsilane; then, starting to stir to carry out
hydrolysis reaction for 20-60 minutes, then, standing, washing an organic phase, and
drying to obtain a precursor
hydrolysis product; adding the precursor
hydrolysis product into an original reaction vessel, then, adding a mixture of a catalyst and a
solvent into the original reaction vessel, and carrying out
backflow reaction at the temperature of 20-250 DEG C for 5-100 hours to separate out a great number of white sediments; and then, purifying in a way of filtering, washing or dissolving and re-crystallizing the sediments, and
drying to obtain octaphenyl
silsesquioxane. According to the preparation method, octaphenyl-functionalized POSS with relatively high molecular weight and relatively high yield is controllably prepared by taking
phenylsilane as a
raw material through a low-temperature feeding and two-step hydrolysis process; in addition, the preparation process is simple, the yield is relatively high, and the preparation period is short.