期刊
JOURNAL OF FLOW CHEMISTRY
卷 5, 期 3, 页码 178-182出版社
AKADEMIAI KIADO RT
DOI: 10.1556/1846.2015.00016
关键词
flow nitration; microreactor; energetic materials; LLM-105
资金
- Joint DoD/DOE Munitions Program (JMP)
- LLNL LDRD [13-ER-051]
- U.S. Department of Energy by Lawrence Livermore National Laboratory [DE-AC52-07NA27344]
The secondary high explosive 2,6-diamino-3,5-dinitropyrazine-1-oxide, or LLM-105, has been synthesized using a commercially available flow microreactor system. Investigations focused on optimizing flow nitration conditions of the cost effective 2,6-diaminopyrazine-1-oxide (DAPO) in order to test the feasibility and viability of flow nitration as a means for the continuous synthesis of LLM-105. The typical benefits of microreactor flow synthesis including safety, tight temperature control, decreased reaction time, and improved product purity all appear to be highly relevant in the synthesis of LLM-105. However, the process does not provide any gains in yield, as the typical 50-60% yields are equivalent to the batch process. A key factor in producing pure LLM-105 lies in the ability to eliminate any acid inclusions in the final crystalline material through both a controlled quench and recrystallization. The optimized flow nitration conditions, multigram scale-up results, analyses of sample purity, and quenching conditions for purity and crystal morphology are reported.
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