This paper describes a new multivariable adaptive decoupling controller combining a decoupling compensator with a generalized minimum variance technique. The controller can completely decouple closed-loop systems both dynamically and in the steady state. It can control an unstable and/or non-minimum phase system and it can control the process with an arbitrary time delay structure. The proof of global convergence for the algorithm is also given. Successful experimental results of the adaptive decoupling control for a pilot-scale binary distillation column demonstrate the effectiveness of the proposed adaptive decoupling algorithm.