Chlorosilanes such as dimethyldichlorosilane are hydrolyzed in a first super-azeotropic hydrochloric acid distillation column A to produce cyclosiloxanes, chlorosiloxanes, and hydrogen chloride gas. The cyclosiloxanes and the chlorosiloxanes are washed and separated according to their volatility in a second sub-azeotropic hydrochloric acid distillation column B, to produce a substantially chloride free volatile cyclosiloxane stream and a substantially chloride free non-volatile siloxane stream. The process is substantially chloride efficient.