In this work, a continuous system to produce multi-hundred-gram quantities of aryl sulfonyl chlorides is described. The scheme employs multiple continuous stirred-tank reactors (CSTRs) and a continuous filtration system and incorporates an automated process control scheme. The experimental process outlined is intended to safely produce the desired sulfonyl chloride at laboratory scale. Suitable reaction conditions were first determined using a batch-chemistry design of experiments (DOE) and several isolation methods. The hazards and incompatibilities of the heated chlorosulfonic acid reaction mixture were addressed by careful equipment selection, process monitoring, and automation. The approximations of the CSTR fill levels and pumping performance were measured by real-time data from gravimetric balances, ultimately leading to the incorporation of feedback controllers. The introduction of process automation demonstrated in this work resulted in significant improvements in process setpoint consistency, reliability, and spacetime yield, as demonstrated in medium- and large-scale continuous manufacturing runs.

Different types of molten salts are proposed or in use for nuclear fission, fusion, and concentrated solar power, such as fluorides, chlorides, carbonates, and nitrate-based salts. For the different clean energy technologies, the components that interface with the molten salts as coolants and/or nuclear/fusion fuels require research and development before deployment. This research and development includes experimental validation where lower cost and lower hazard surrogate fluids can be used for specific sets of physics. These surrogate fluids can emulate the heat transfer and fluid mechanics phenomena of molten salts at reduced temperature scales, safety requirements and as a result, costs. Previously, certain surrogate fluids have been proposed for fluorides, chloride, and nitrate salts; however, better surrogate fluids in terms of the aforementioned benefits and enhanced scaling of behavior are sought after. In this work, the Dynalene family of fluids was investigated and shown to work as surrogate fluids for fluoride, chloride, and nitrate based salts. The most important outcome is that these Dynalene fluids are demonstrated to scale well to molten salts. This is as compared to the previously identified surrogate fluids, specifically, Dowtherm-A and Therminol VP-1, at reduced cost and improved material compatibility.

This study presents a kinetic model that simulates the consumption of 4-hydroxybenzoic acid (4-HBA), the formation of di-isopropyl benzoic acid (DIPBA) via a Friedel–Crafts alkylation reaction, and the generation of key impurities.