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2,4,6-trinitro-2,4,6-nitro-triazacyclohexanone Synthesis and Its Process Optimization

Author: TanQingQing
Tutor: LiYongXiang
School: University of North
Course: Chemical Engineering
Keywords: Keto-RDX Process optimization Nitrification crystal morphology Impactensitivit
CLC: TQ560.1
Type: Master's thesis
Year: 2014
Downloads: 5
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Abstract


High-energy insensitive explosives are an important direction of the design and synthesisof explosive, which should both have high energy and good stability.2,4,6–trinitro-2,4,6-nitro-triazacyclohexanone(Keto-RDX) with high density, detonation pressure, high detonationvelocity, has good oxygen balance, thermodynamics and hydrolysis stability, which alsooutput further energy than Octogen (HMX). Keto RDX is a kind of high energy densitycompound belonging to urea ring series and it is also a kind of important organicintermediates, which is mainly used for loading sunder armor and non primary explosivedetonator. So the research on the synthesis technology and properties of Keto-RDX is ofimportant practical significance.With urea and methenamine as raw material, the nitration synthesize of Keto-RDX canbe implement through using nitro-sulfuric acid. In consequence of the improvement of theprocess after the nitrificationn for the first time, the safety of the process has been improvedgreatly. The solubility of Keto-RDX in some solvents is obtained by the dynamic method,thus filling the gaps of its solubility data and providing further research reference andtheoretical basis. According to the difference of the solubility between Keto-RDX andRDX,the research on the separation of Keto-RDX and RDX mixture can be proposed bychoosing the different solvent. In this way, the optimum process conditions for keepingKeto-RDX and RDX apart can be obtained: considering acetone as the solvent, considering1:50as the best mass ratio of the materials, consider ing5-10℃as the solution temperature.NIHT·HCl was prepared via nitroguanidine, methenamine as raw materials.Keto RDXwas synthesized via nitration of NIHT·HCl. The optimal reation conditions for preparing were:under38℃, the reaction of12h. For the first time by nitrate-P2O5green nitrating agentsynthesis Keto-RDX. The results showed that the reation conditions for Keto-RDX were: themolar ratio of n(nitric acid): n(P2O5)=10:1, reaction temperature25℃, the reaction time35min,, the yield of Keto-RDX was up to87%.Explored using urea as raw materials, Keto-RDX was obtained by nitration, hydrolysis,and Mannich condensation. The suitable solvent can be chosen by virtue of the simulated result of crystal habit in thesolvent under MS software to conduct the study on the recrystallization process of Keto-RDX.Keto-RDX is obtained by the experiment of recrystallization better process conditions:cyclohexanone as solvent, water as anti-solvent, recrystallization temperature90℃,dropping speed of the anti-solvent is0.10mL/min, stirring speed of200r/min, solvent andanti-solvent ratio of1:1. The experiment was abrasion Keto-RDX from recrystallization.Recrystallization of Keto-RDX was added to the saturated solution of Keto-RDX at roomtemperature. The process conditions for abrasion experiment were as follows: heating up to40℃, stirring speed of100r/min, reaction time4h. Characteristics drop height of abrasiveobtained the Keto-RDX crystal is48.98cm, compared with ordinary Keto-RDX, the impactsensitivity obviously decreased.

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