Synthesis and Kinetics of Highly Energetic Intermediates by Micromixers: Direct Multistep Synthesis of Sodium Nitrotetrazolate

A modular silicon micromixer is designed and fabricated for high-flow rapid mixing at a wide range of reaction conditions. The mixer operates by splitting two inlet flows into a large number of channels, interdigitating them, and constricting the laminated flow to create submicrometer diffusion leng...

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Bibliographic Details
Published in:Industrial & engineering chemistry research 2010-05, Vol.49 (9), p.4132-4139
Main Authors: Zaborenko, Nikolay, Murphy, Edward R, Kralj, Jason G, Jensen, Klavs F
Format: Article
Language:English
Subjects:
Applied sciences
Chemical engineering
Exact sciences and technology
Kinetics, Catalysis, and Reaction Engineering
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Summary:A modular silicon micromixer is designed and fabricated for high-flow rapid mixing at a wide range of reaction conditions. The mixer operates by splitting two inlet flows into a large number of channels, interdigitating them, and constricting the laminated flow to create submicrometer diffusion lengths. Mixing is quantified using the Villermaux−Dushman method, with UV−vis detection of the photoactive species, and compared against a commercial micromixer. Micromixers and tubing are then used to perform a quantitative kinetic study of the direct two-step synthesis of sodium nitrotetrazolate (NaNT) by a Sandmeyer type reaction via a reactive diazonium intermediate. Orders of reactions and temperature dependence of both steps, as well as pH and ionic strength dependence of the second step, are evaluated. Successful production of 4.4 g/h of NaNT in solution is ultimately achieved in a compact footprint using the kinetic data, verifying the potential for scaling to typical production amounts.
ISSN:0888-5885
1520-5045
DOI:10.1021/ie100263p