Abstract: Disclosed is a process for manufacturing polyarylene sulfide comprising pre-polymerizing a dihalogeno-aromatic compound with a liquid or gaseous sulfur compound in the presence of a lithium compound in an aprotic organic solvent followed by further polymerizing the resulting pre-polymerized system; which is characterized in that sufficient water is added to the pre-polymerized solution (I) to separate it into a tick polymer phase and a solvent phase, then a solvent is added to the thus-separated, thick polymer phase and the resulting polymer phase is further polymerized, for efficiently manufacturing high-purity polyarylene sulfide. The process does not require any complicated steps of washing the polymer with a multi-stage washing system and is free from the increase in the production costs of the polymer. In the process, the lithium salt used can be recovered efficiently.