Isolation of Pharmaceutical Intermediates through Solid Supported Evaporation. Semicontinuous Operation Mode
2012 (English)In: Industrial & Engineering Chemistry Research, ISSN 0888-5885, E-ISSN 1520-5045, Vol. 51, no 45, 14814-14823 p.Article in journal (Refereed) Published
Solid supported evaporation (SSE) is a simple, nonselective method for isolating nonvolatile compounds from a solution. The solution is put in contact with porous polymer beads onto which the compound deposits upon evaporation of the solvent. This brings some advantages over direct evaporation to dryness in terms of safety, thermal decomposition, and solid handling, as the loaded beads form a free flowing granular material that is easily recovered. In this paper, SSE in a semicontinuous operating mode is investigated where the solution is continuously fed to (respectively sprayed over) an agitated bed of dry beads put under vacuum. It is found that under conditions where the solvent evaporation fate is high with respect to the feed rate, high bead loadings can be achieved before extensive sticking of beads and compound to the vessel walls occurs. The type of compound and solvent had little influence on the process performance, and, in cases where this was explored, the bead loading was found to be homogeneous. Based on a balance equation for the solvent fed to the system, a model is developed that results in a simple scale up criterion. The latter was successfully applied for transferring SSE from lab to the kilo lab scale.
Place, publisher, year, edition, pages
2012. Vol. 51, no 45, 14814-14823 p.
Microreactor Technology, Scale-Up, Crystallization, Accurel, Immobilization, 21st-Century, Revolution, Adsorption, Industry, Solvents
IdentifiersURN: urn:nbn:se:kth:diva-107613DOI: 10.1021/ie301359cISI: 000311191600022ScopusID: 2-s2.0-84869397805OAI: oai:DiVA.org:kth-107613DiVA: diva2:577767
FunderEU, European Research Council, 228867
QC 201212172012-12-172012-12-142012-12-17Bibliographically approved