2691-41-0Relevant articles and documents
Deuterium Isotope Effects in Condensed-Phase Thermochemical Decomposition Reactions of Octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine
Shackelford, S. A.,Coolidge, M. B.,Goshgarian, B. B.,Loving, B. A.,Rogers, R. N.,et al.
, p. 3118 - 3126 (1985)
The deuterium isotope effect was applied to condensed-phase thermodinamical reactions of HMX and HMX-d8 by using isothermal techniques.Dissimilar deuterium isotope effects revealed a mechanistic dependence of HMX upon different physical states which may singularly predominate in a specific type of thermal event.Solid-state HMX thermodinamical decomposition produces a primary deuterium isotope effect (DIE), indicating that covalent C-H bond rupture is the rate-controlling step in this phase.An apparent inverse DIE is displayed by the mixed melt phase and can be attributed to C-H bond contraction during a weakening of molecular lattice forces as the solid HMX liquefies.The liquid-state decomposition rate appears to be controlled by ring C-N bond cleavage as evidenced by a secondary DIE and higher molecular weight products.These results reveal a dependence of the HMX decomposition process on physical state and lead to a broader mechanistic interpretation which explains the seemingly contradictory data found in current literature reviews.
Solubility of 3,7-Dinitro-1,3,5,7-tetraazabicyclo [3.3.1] Nonane in Ethanenitrile, Methanol, 1,1-Dichloroethane, Dimethyl Sulfoxide, Acetone, and Mixed Solvents
Xue, Min,Wu, Siyu,Liu, Wenjin,Zhu, Qiao,Meng, Zihui,Lin, Zhihui
, p. 1683 - 1687 (2015)
The solubility of 3,7-dinitro-1,3,5,7-tetraazabicyclo [3.3.1] nonane (DPT) was measured in ethanenitrile, methanol, 1,1-dichloroethane, dimethyl sulfoxide (DMSO), acetone, ethyl acetate, ethyl acetate and methanol mixture, and acetonitrile and water mixture from 288.15 K to 308.15 K. In this paper, the determination method of DPT was first established by high-performance liquid chromatography (HPLC) with optimized chromatographic conditions. The solubility of DPT in all solvents was measured upon this chromatographic method. Experimental results show that the order of solubility can be represented as DMSO > acetonitrile > ethyl acetate > ethyl acetate/methanol (9:1, v/v) > ethyl acetate/methanol (7:3, v/v) > acetone > acetonitrile/water (9:1, v/v) > ethyl acetate/methanol (5:5, v/v) > acetonitrile/water (7:3, v/v) > 1,1 - dichloroethane > methanol. Moreover, its solubility increased with raising the temperature. The thermodynamic properties of DPT, such as solution enthalpy, have also been calculated.
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Cady et al.
, p. 617,623 (1963)
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An efficient synthesis of l,3,5,7-tetranitro-l,3,5,7-tetraazacyclooctane (HMX) by ultrasonic irradiation in ionic liquid
Qian, Hua,Liu, Dabin,Lv, Chunxu
, p. 184 - 187 (2011)
New process to synthesize HMX from 3,7-dinitro-1,3,5,7- tetraazabicyclo[3,3,1]nonane (DPT) using ultrasound in ionic liquid was developed. The reaction has been carried out in ultrasonic bath and the effect of various parameters such as presence and absence of ultrasound, volume and type of solvent, temperature, concentration of nitrating agent has been investigated with the aim of obtaining the optimum conditions for the synthesis of HMX. It was observed that yield was significantly enhanced from 42.3% up to 87.4% through the ultrasonically promoted nitrolysis of DPT to HMX at ambient condition.
Method for directly preparing beta-HMX with different particle sizes
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Paragraph 0012-0025, (2021/01/04)
The invention discloses a method for directly preparing beta-HMX with different particle sizes. The method comprises the following steps of: carrying out nitration reaction on 1-nitroso-3, 5, 7-trinitro-1, 3, 5, 7-tetraazacyclooctane (MNX) and fuming nitric acid at room temperature; slowly dropwise adding dilute nitric acid and water in two stages for crystallization, filtering, washing and dryingto obtain beta-HMX with different particle sizes. The product obtained by the method is high in purity, and the yield reaches 92.2%; and the use of procedures such as oxidative crystallization or recrystallization is avoided, the production process is simplified, the production cost is reduced, the environmental pollution is reduced, and the production safety is improved.
Preparation method of HMX
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Paragraph 0029; 0037-0039; 0047; 0055; 0063, (2017/10/31)
The invention discloses a preparation method of HMX. The preparation method comprises the steps of dissolving dinitrogen pentoxide into an organic solvent to form a nitrating agent; slowly adding ammonium salt into the nitrating agent, and adding DPT in batches to obtain reactants; controlling the temperature of the materials to be 0-10 DEG C in a feeding process, heating the reactants up to 20-35 DEG C, and carrying out a reaction at the constant temperature for 20-60min; after the reaction is finished, carrying out solid-liquid separation to obtain solid; washing the obtained solid, drying in the air, and purifying to obtain the HMX, wherein the organic solvent is selected from acetonitrile and dichloromethane, and the ammonium salt is selected from tetramethyl ammonium chloride, ammonium carbonate, ammonium acetate and ammonium oxalate. The preparation method provided by the invention is mild in reaction conditions and easy in separation of products, and needs a less amount of acid; the system does not produce waste acid, thus being low in treatment cost; furthermore, the preparation method greatly increases the yield of the HMX.
