The invention discloses a process for separating and purifying polyphenylene 
sulfide. The process includes (1), separating the granular polyphenylene 
sulfide from mixtures with the polyphenylene 
sulfide by centrifugal machines, and mixing the remaining mixtures and diatomaceous earth with one another in mixing kettles to obtain mixtures A; (2), connecting outlets of the mixing kettles with pumps,connecting outlets of the pumps with regulating valves, connecting the regulating valves with plate hermetic filters, conveying the mixtures A to the plate hermetic filters by the pumps and filteringthe mixtures A to obtain 
solid materials and filter liquor B; (3), delivering the filter liquor B into rectification systems and rectifying the filter liquor B. The process has the advantages that theself-operated regulating valves and the plate hermetic filters are used with one another, the diatomaceous earth is applied to procedures for separating and purifying the polyphenylene sulfide, accordingly, the problems of pump and rectification 
tower blockage due to materials, the requirement on detaching 
tower equipment for clearing or washing the 
tower equipment and material leakage can be effectively solved by the aid of the process, product loss further can be reduced, environmental 
pollution can be abated, and the productivity can be improved.