Refining of Benzene Sulfonyl Chloride from Benzene-Chlorosulfonic Acid Sulfonation Mass

Abstract

This thesis represents the investigations and application of various chemical and engineering principles that may prove useful in designing an efficient and economical method for producing benzene sulfonyl chloride from benzene-chlorosulfonic acid sulfonation mass. Phase separation of the sulfonation mass with water followed by countercurrent extraction of the acids from the sulfonation mass proved to be a more efficient and economical process than a batch drowning process. Centrifuging and low temperature vacuum distillation of the benzene suIfonyl chloride emulsion appeared to be an efficient method or clarification. In brief, the conclusion summery was outlined as follows: In the refinement of benzene chlorosulfonic acid sulfonation mass, the continuous agitated- phase-separation and counter-current extraction process with clarification by centrifuging and vacuum distillation appeared much more efficient than the batch- drowning process for I. Hydrolysis losses a) were not greatly increased by agitation b) were reduced tor use of smaller volumes of drowning water, c) were repressed in agitated phase separation d) were less when the wash water was more efficiently used e) were less when proper temperature control was obtained f) were reduced as the period of contact with water was shortened II. Entrainment losses were reduced by a) use or less water overflow b) the action of the column packing III. Clarification was made possible a) by removal of water by centrifuging b) by removal of water by vacuum distillation IV. Man-hours were more efficiently used by a) reducing the process time b) reducing requirements for rigid control