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Modular Energetic Materials Synthesis Platform


The technology within this topic is restricted under the International Traffic in Arms Regulation (ITAR), 22 CFR Parts 120-130, which controls the export and import of defense-related material and services, including export of sensitive technical data, or the Export Administration Regulation (EAR), 15 CFR Parts 730-774, which controls dual use items. Offerors must disclose any proposed use of foreign nationals (FNs), their country(ies) of origin, the type of visa or work permit possessed, and the statement of work (SOW) tasks intended for accomplishment by the FN(s) in accordance with section 3.5 of the Announcement. Offerors are advised foreign nationals proposed to perform on this topic may be restricted due to the technical data under US Export Control Laws. OBJECTIVE: To create a scalable, highly-modular, platform that can accommodate a wide variety of synthesis strategies to produce a large number of fine/specialty chemicals relevant to the energetics community, economically and on-demand. This platform needs to be nimble enough to take advantage of new and old synthetic routes to manufacture traditional energetic materials to maximize cost and efficiency as well as put new compounds into production. DESCRIPTION: Ingredients used in explosive, propellant, and pyrotechnic formulations comprise a wide array of chemistries, including organic (C, H, N, O based) and inorganic explosives and oxidizers, polymeric and oligomeric binders, metal fuel particles, plasticizers, catalysts, burn rate modifiers and a variety of other additives. For common formulation ingredients that are used in large volume such as high explosives, bulk-production generally occurs at large-scale specialty manufacturing plants. In contrast, boutique ingredients that are used either in smaller fractional amounts in energetic formulations or are only needed for periodic production runs are increasingly difficult to procure. Often the only available sources for these critical ingredients and precursors are now OCONUS, if available at all. This dearth of US sources and market drivers strong enough to produce in-service ingredients makes it difficult to rapidly prototype new, higher performing energetic formulations. Causes of this divestiture are multifaceted and include: being unfamiliar with unique synthetic processes such as nitration and reactions on highly strained systems, a lack experience with qualification specification requirements, and a lack of flexibility when it comes to handling sporadic and highly-variable (in terms of quantity) production runs. Coupled with the necessity for scalable synthesis platforms to produce critical, already-fielded ingredients; there is a similar need for small-scale, agile production to support synthesis of new and emerging energetic ingredients for rapid formulations development leading to higher performing propellants and explosives. The time between energetic molecule discovery to scaled-up batch synthesis in sufficient quantity for formulation and safety testing can often take many years. This lack of high-throughput synthetic strategies and tools at developmental quantities severely hinders the ability to rapidly prototype, test, and transition new energetic formulations. Considering recent progress in theoretical/predictive chemical synthesis [1] [2], scalable flow chemistry methods [3] [4] [5] and microfluidics [6], in-situ diagnostics to inform synthetic strategies, feedback control [7], modular chemical processes [8] [9] [10] [11] [12], and related advances pushed by pharmaceuticals [13] [14] [15] [16] [17] [18] and other chemical industries [19] [20] [21] [22] [23], it is anticipated that safe [24], cost-effective [25], switchable, and modular chemical synthesis platforms with a small and portable footprint can now be developed to change the paradigm of “less-than-bulk” production for critical/fielded and emerging energetic ingredients and precursors. PHASE I: Design on paper a modular and scalable synthetic platform that is configurable to produce representatives of four or more classes of energetic material ingredients and/or precursors with minimal configurational changes. The platform can integrate any synthetic process (continuous flow, microfluidics, batch, etc.) that is amendable to the modular and switchable platform goals. Other emerging advances in synthesis S&T should be exploited, examples including theoretical synthesis planning strategies [1], electro- and photo-catalysis [8], etc. Selected reactions should be justified by the ability to showcase platform chemical variability. The design should outline configuration changes (time, effort, cleanup, etc.) necessary to accommodate switching between the selected ingredients/precursors and cost analysis should be prepared comparing to current production cost as appropriate. Issues of scalability should be addressed; i.e., if scaling to progressively larger quantities is accomplished by larger volume or more rapid reagent throughput, parallel modules to multiply output, or some other means. Emphasis should be placed on creating the on-demand ability to switch between target material syntheses through system modularity, accounting for material handling safety concerns. Remote operation for safety considerations should be integrated into overall design. Phase I should present two or more “modules” that perform particular chemical synthesis and/or diagnostic functions. Elements within the modules can include regulated solid and or liquid reagent addition/dispensing, mixing protocols, exquisite control of temperature, chemical separation/purification steps. Control hardware and software must be included in the overall description of each module. In situ chemical diagnostics may be an integral part of the platform modules, but at least one should be dedicated to evaluate the synthetic strategy (FTIR, HPLC, GCMS, etc.) and should back-feed into any theoretical predictive strategies. The process modules can be COTS or custom built, but should be rationally chosen to facilitate multiple kinds of reaction environments with relevance to energetic materials chemistry. Details to integrate each of the modules is not required in phase I; however, plans to integrate into the complete synthetic platform should be outlined in the overall platform paper design. Emphasis is to be placed on any modules/operations that are special to new/emerging energetic materials synthesis strategies, but are not confined to particular end products. For example, nitration reaction strategies, cage formations, feedback to theoretical synthesis tools, etc. PHASE II: Prototype the switchable, modular on-demand synthesis capability to produce representatives of four or more classes of energetic material ingredients and/or precursors based on the Phase I design. Selected ingredients should be justified by critical need and (lack of) availability, DoD importance, and ability to showcase platform chemical variability. All appropriate synthesis process modules should be physically integrated into the overall platform with appropriate in situ diagnostic modules to inform/streamline synthetic strategies. Necessary process control hardware and software should be complete and running the modules. Capability to switch between and produce the example ingredients/precursors to completion (readiness to be formulated) should be confirmed. Ingredients produced using the new synthesis platform should be characterized and compared to ingredient/precursor specifications and requirements (MIL-SPEC, MIL-STD, ASTM, etc.) where possible. Platform scalability (grams to kilograms) should be demonstrated for at least one of the example ingredients. Pursue efforts to partner with appropriate DoD or other DoD contractor points of contact (POCs) for transition of manufacturing capabilities. PHASE III DUAL USE APPLICATIONS: Work with DoD or DoD contractor energetic material production community to duplicate and integrate new modular synthetic platform(s) to best fill critical EM material needs. Efforts will be guided by Navy TPOC and other SMEs, including the Critical Energetic Materials Working Group (CEMWG), Energetic Materials ManTech, and other stakeholders. REFERENCES: [1] T. Martinez. [Online]. Available: [2] C. W. Coley, W. H. Green and K. F. Jensen, "Machine Learning in Computer-Aided Synthesis Planning," Accounts of Chemical Research, vol. 51, no. 5, pp. 1281-1289, 1 May 2018. [3] J. Britton, "The assembly and use of continuous flow systems for chemical synthesis," Nature Protocols, vol. 12, pp. 2423-2446, 26 October 2017. [4] J. Britton and C. L. Raston, "Multi-step continuous-flow synthesis," Chemical Society Review, vol. 46, pp. 1250-1271, 2017. [5] J. Wegner, S. Ceylan and A. Kirschning, "Flow Chemistry – A Key Enabling Technology for (Multistep) Organic Synthesis," Advanced Synthesis & Catalysis, vol. 354, no. 1, pp. 17-57, 2012. [6] P. J. A. Kenis, R. F. Ismagilov, S. Takayama, G. M. Whitesides, S. Li and H. S. White, "Fabrication inside Microchannels Using Fluid Flow," Accounts of Chemical Resesarch, vol. 33, no. 12, pp. 841-847, 8 September 2000. [7] B. J. Reizman and J. F. Klavs, "Feedback in Flow for Accelerated Reaction Development," Accounts of Chemical Research, vol. 49, no. 9, pp. 1786-1796, 15 August 2016. [8] M. Elsherbini and T. Wirth, "Electroorganic Synthesis under Flow Conditions," Accounts of Chemical Research, vol. 52 , no. 12, p. 3287–3296, 2019. [9] Y.-H. Kim, L. K. Park, S. Yiacoumi and C. Tsouris, "Modular Chemical Process Intensification: A Review," The Annual Review of Chemical and Biomolecular Engineering, vol. 8, pp. 359-380, June 2017. [10] J. A. Selekman, J. Qiu, K. Tran, J. Stevens, V. Rosso, E. Simmons, Y. Xiao and J. Janey, "High-Throughput Automation in Chemical Process Development," Annual Review of Chemical and Biomolecular Engineering, vol. 8, pp. 525-547, 2017. [11] N. Krasberg, "Selection of Technical Reactor Equipment for Modular, Continuous Small-Scale Plants," Processes, vol. 2, no. 1, pp. 265-292, 10 March 2014. [12] M. Baumann, I. R. Baxendale, S. V. Ley, N. Nikbin, C. D. Smith and J. P. Tierney, "A modular flow reactor for performing Curtius rearrangements as a continuous flow process," Organic & Biomolecular Chemistry, vol. 6, no. 9, pp. 1577-1586, 12 March 2008. [13] B. J. Doyle, P. Elsner, B. Gutman, O. Hannaerts, C. Aellig, A. Macchi and D. M. 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A pharma perspective," Journal of medicinal chemistry, vol. 55, no. 9, pp. 4062-4098, 2012. [18] M. Baumann, T. S. Moody, M. Smyth and S. Wharry, "A Perspective on Continuous Flow Chemistry in the Pharmaceutical Industry," Organic Process Research & Development, vol. 20, no. 10, p. 1802–1813, 2020. [19] N. Krasberg, L. Hohmann, T. Bieringer, C. Bramsiepe and N. Kockmann, "Selection of Technical Reactor Equipment for Modular, Continuous Small-Scale Plants," Processes, vol. 2, no. 1, pp. 265-292, 2014. [20] "The Concept of Chemical Generators: On-Site On-Demand Production of Hazardous Reagents in Continuous Flow," Accounts of Chemical Research, vol. 53, no. 7, pp. 1330-1341, 2020. [21] "Advanced-Flow Reactors," Corning, [Online]. Available: [Accessed 2 February 2021]. [22] J. Zhang, C. Gong, X. Zeng and J. Xie, "Continuous flow chemistry: new strategies for preparative inorganic chemistry," Coordination Chemistry Reviews, vol. 324, pp. 39-53, 1 October 2016. [23] A. I. o. C. Engineers, "The Rapid Advancement in Process Intensification Deployment (RAPID) Institute," American Institute of Chemical Engineers, [Online]. Available: [Accessed 2 February 2021]. [24] "Taming hazardous chemistry by continuous flow technology," Chemical Society Reviews, vol. 45, no. 18, pp. 4892-4928, 25 July 2016. [25] S. D. Schaber, D. I. Gerogiorgis, R. Ramachandran, J. M. B. Evans, P. I. Barton and B. L. Trout, "Economic Analysis of Integrated Continuous and Batch Pharmaceutical Manufacturing: A Case Study," Industrial & Engineering Chemistry Research, vol. 50, no. 17, p. 10083–10092, 2011. KEYWORDS: Energetic Materials; Energetic Ingredients; Critical Chemicals; Chemical Synthesis; Explosives; Oxidizers; Propellants; Pyrotechnics
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