The invention relates to the technical field of environment-friendly industry waste acid recycling, in particular to an organosilicone waste acid contained tributylamine, siloxane and aluminum chloride recycling technology. The technology comprises the steps of acid and oil separation, aluminum chloride film separation, hydrochloric acid salting analysis, tributylamine and salt separation and salt evaporation and concentration. Equipment of the technology comprises a waste hydrochloric acid groove, a waste acid feeding pump, an acid and water separator, a siloxane recycling tank, a film filter, an aluminum chloride collecting tank, a hydrochloric acid tundish, a hydrochloric acid entrance pump, an analysis tower, a first reboiler, a two-phase separator, a primary condenser, a secondary cooler, a tributylamine recycling tank, an evaporator, a calcium chloride recycling pump, a second reboiler, a tributylamine recycling pump, a wastewater condensation groove and a wastewater pump; the organosilicone waste acid contained tributylamine, siloxane and aluminum chloride recycling technology has the advantages of lowering the treatment operation cost, meanwhile, recycling lost catalysts, siloxane, aluminum chloride and other substances, and improving economic benefits of an enterprise.