4.6 Article

Energetic Material Synthesis: Scale-up Using a Novel Modular Microflow Reactor Setup

Journal

ORGANIC PROCESS RESEARCH & DEVELOPMENT
Volume -, Issue -, Pages -

Publisher

AMER CHEMICAL SOC
DOI: 10.1021/acs.oprd.2c00398

Keywords

Energetic material; continuous flow; flow reactor; upscaling; silica coating; high corrosion; nitroguanidine

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The advantages of microflow reactors, such as excellent cooling ability, allow for safe exothermic reactions. However, transitioning from small to industrial scale production remains a challenge. A reactor setup has been developed to overcome this limitation and enable the use of highly corrosive materials. As proven by the successful synthesis of nitroguanidine on a lab scale, the new setup improves safety and production rate, making industrial scale-up feasible.
The advantages ofmicroflow reactors have proven to be manifold,e.g., the excellent cooling ability, which allows performing exothermicreactions like nitrations safely. A critical point remains the transitionfrom gram scale to industrial production. On an industrial scale,they are often designed for specific syntheses and are therefore lessuseful for a conventional research laboratory. A reactor setup wassuccessfully developed mitigating these shortcomings and allowingthe use of highly corrosive materials, like fuming inorganic acids(e.g., nitric, sulfuric acid), bases (e.g., bleach solutions), andchlorinated solvents. As a proof of functionality, the synthesis ofnitroguanidine has been performed on a lab scale and was significantlyimproved over reported batch syntheses in terms of safety and productionrate. A scale-up to industrial scale has hence become feasible.

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