Abstract
This paper describes the nitration of 2,4-dinitrotoluene (DNT) and its conversion to 2,4,6-trinitrotoluene (TNT) at a gram scale with the use of a fully automated flow chemistry system. The conversion of DNT to TNT traditionally requires the use of highly hazardous reagents like fuming sulfuric acid (oleum), fuming nitric acid (90–100%), and elevated temperatures. Flow chemistry offers advantages compared to conventional syntheses including a high degree of safety and simpler multistep automation. The configuration and development of this automated process based on a commercially available flow chemistry system is described. A high conversion rate (>99%) was achieved. Unlike established synthetic methods, ordinary nitrating mixture (65% HNO3/98% H2SO4) and shorter reaction times (10–30 min) were applied. The viability of flow nitration as a means of safe and continuous synthesis of TNT was investigated. The method was optimized using an experimental design approach, and the resulting process is safer, faster, and more efficient than previously reported TNT synthesis procedures. We compared the flow chemistry and batch approaches, including a provisional cost calculation for laboratory-scale production (a thorough economic analysis is, however, beyond the scope of this article). The method is considered fit for purpose for the safe production of high-purity explosives standards at a gram scale, which are used to verify that the performance of explosive trace detection equipment complies with EU regulatory requirements.
Highlights
The synthesis of 2,4,6-trinitrotoluene (TNT) has gained a lot of scientific and industrial interest since it was the first high explosive that was able to fulfil the expectations of producers and the military.It was first synthesized in the 1860s and was later produced in large quantities during World War I and World War II [1]
TNT synthesis et al, of thisliquid step ofenergetic nitrationmaterials is performed in a batch mode due towas the flow chemistrydescribed methodsby forMillar synthesis
The experimental design approach used to study and optimize the conditions for the flow chemistry system, the conditions adopted for both flow chemistry and batch synthesis, and the analytical methods applied to characterize the obtained products are described
Summary
The synthesis of 2,4,6-trinitrotoluene (TNT) has gained a lot of scientific and industrial interest since it was the first high explosive that was able to fulfil the expectations of producers and the military It was first synthesized in the 1860s and was later produced in large quantities during World War I and World War II [1]. This explosive is a moderately powerful, high-energy material, with satisfactory thermal stability and reduced mechanical sensitivity. It is still used in many explosive mixtures today by military and special branches of industry This is facilitated by its low cost and the fact that it is relatively insensitive, as well as readily melt-castable. Still a main component in many explosive mixtures, some of which were developed several decades ago, such as Amatol, Baratol, Comp B, H-6, Tritonal, and Torpex [2]
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