I am trying to prepare polymeric microcapsules via. a W/O/O emulsion synthesis process. So my technique essentially begins with formation of a W/O1 emulsion system formed by homogenization where the O1 phase is DCM (dichloromethane) in which the polymer PCL(polycaprolactone) is dissolved. A low HLB value surfactant is being used for the synthesis of this system to give water in oil droplet configuration.
Then this system is being put into another O2 phase essentially silicone oil with addition of a high HLB value surfactant and homogenized to form a W/O1/O2 assembly. So the idea is the DCM would eventually evaporate and lead to formation of polymeric spheres (particles) encapsulating the water moeity inside and these spheres remain suspended in the silicone oil phase. (The turbid appearance of the system is a manifestation of these freely suspended particles, which is otherwise clear).
Post synthesis, we try to wash these particles with suitable solvent to remove the silicone oil and collect these particles by centrifugation or other separation technique like filtration. But the particles stick to each other and form a paste kind of substance. After that, on trying to disperse the particles in an aqueous phase they don't disperse into finer particles as they were once in the silicone oil system and hence our particle analysis are way off from the expected values. So how can I overcome this problem. Is there a need to alter my selection of surfactants/reagents or is it the procedure that requires any modification?