MQ silicone resins, which represent a broad range of hydrolytic condensation products of monofunctional silane (M) and tetrafunctional silane (Q), were synthesized by reaction of water glass with hexamethyldisiloxane. The optimum reaction time and the optimal reaction temperature is 30 min and 30-40 degrees C, respectively. Concentrated hydrochloric acid is the best one among those catalysts tested. In large-scale experiments (4201680 mL), the favorable feeding order is catalyst first, and then water glass, the mixture of hexamethyldisiloxane and ethanol last and most MQ silicone resin was observed. The structure of MQ silicone resin was characterized by FT-IR and GPC spectra. The MQ silicone resin shows narrow molecular weight distribution and the number average molecular weight of MQ silicone resin is 2917. The silicone pressure sensitive adhesive prepared from as-synthesized MQ resin has good tack (29#) and 180 degrees peel adhesion (5.630N/20 mm). (C) 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012