4,10-Dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo[5.5.0.0<sup>5,9</sup>0<sup>3,11</sup>]dodecane Synthesis

Maksimowski, Paweł; Gołofit, Tomasz

doi:10.1080/07370652.2012.716490

Cited by 11 publications

(9 citation statements)

References 5 publications

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“…Materials TEX was synthesized in the Department of High-Energetic Materials of the Warsaw University of Technology [28]. The purity of compound was determined using high-performance liquid chromatography (HPLC) and equals 99.5 %.…”

Section: Methodsmentioning

confidence: 99%

“…Obtained kinetic parameters were the resultant of all reactions. For this reason, the calculated activation energy in the next part of this manuscript was called apparent activation energy ( a E a ) [20,28]. The apparent activation energy and logarithm of pre-exponential factor were calculated using Friedman's isoconversional method according to the ICTAC recommendation [29].…”

Section: Kinetic Analysismentioning

confidence: 99%

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Thermal properties of TEX decomposition or sublimation

Gańczyk

Zygmunt

Gołofit

2016

J Therm Anal Calorim

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TEX is a thermostable compound and less sensitive to external stimuli. It sublimates and decomposes at high temperature. The influence of DSC and TG measurement conditions and substance mass on the thermal decomposition of TEX was determined. It was observed that substance mass, pan type and fulfillment degree of pan influence the thermal decomposition and kinetic parameters of TEX decomposition. Sublimation of the sample was the main observed process; thermal decomposition was the secondary process during the heating of TEX in open pans. With increasing substance mass, the participation of thermal decomposition of TEX increased. Uncontrolled thermal decomposition was observed for larger mass of a sample. The sublimation and decomposition processes were confirmed by FT-IR method. Thermal decomposition was the main process observed during heating the sample of TEX in hermetic pans. Sublimation of a sample was marginal. The sublimation effect decreased with increasing the degree of fulfillment pan. The kinetic parameters were determined with the Friedman's isoconversional method. The conversion, mass of sample and the type of pan caused the large changes in the values of kinetic parameters. The apparent activation energy varied from 128 to 355 kJ mol -1 and logA varied from 9.95 to 30.64 in initial step (a = 0.02) for different condition of measurements. The low values of apparent activation energy (about 130 kJ mol -1 ) were associated with sublimation process and the high values (about 340 kJ mol -1 ) with the decomposition process.

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Section: Methodsmentioning

confidence: 99%

Section: Kinetic Analysismentioning

confidence: 99%

Thermal properties of TEX decomposition or sublimation

Gańczyk

Zygmunt

Gołofit

2016

J Therm Anal Calorim

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“…These results are in good agreement with literature values. 36 The comparison between DSC of DFTHP and TEX is depicted in Figure 6. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59…”

Section: Dscmentioning

confidence: 99%

“…During the course of the reaction, part of diformyl piperazine may decompose to glyoxal. 36 The isowurtzitane cage structure thus produced undergoes nitrolysis by action of the available According to the mechanism depicted above, the yield of TEX was calculated assuming the fact that DFTHP undergoes partial decomposition to give glyoxal (one DFHP molecule yields two glyoxal molecules) and the remaining DFTHP reacts with the produced glyoxal. If we presume that all the available glyoxal molecules reacted with DFTHP then the utmost yield with respect to DFTHP would be equal to 66.7%.…”

Section: Probable Mechanismmentioning

confidence: 99%

An Improved and Scalable Synthesis of Insensitive High Explosive 4,10-Dinitro-2,6,8,12-tetraoxa-4,10-diazaisowurtzitane (TEX)

Deshmukh

Borse

Mahulikar

et al. 2016

Org. Process Res. Dev.

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4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazaisowurtzitane (TEX), a well-known nitramine category explosive, is much less sensitive to impact and friction stimuli as compared to the familiar explosives, RDX and HMX. TEX is currently produced on pilot plant scale and is being pursued as an insensitive explosive. Herein a newer, improved, efficient and high yielding protocol is developed for the synthesis of TEX by using solid acidic silica sulfuric acid as an efficient and recyclable catalyst. Sequentially for process parameters optimization, a study was carried out with variation of catalyst loading, nitric acid and mole ratio of reactants. The process scale-up is also achieved successfully.

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“…TEX has high density, good thermal stability, excellent detonation characteristics, and low sensitivity to external stimuli [9][10][11][12]. Earlier works have mostly focused on synthesis, thermal stability, explosion property, sensitivity, and its use in explosives [13][14][15][16][17][18]. However, the dissolution properties of its solution at different temperatures have never been reported so far.…”

Section: Introductionmentioning

confidence: 99%

Dissolution properties of 4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazaisowutrzitane in N-methyl pyrrolidone

Xiao

Luo

Zhao

et al. 2015

J Therm Anal Calorim

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The dissolution properties of 4,10-dinitro-2, 6,8, in Nmethyl pyrrolidone (NMP) were studied with a RD496-2000 Calvet microcalorimeter at four different temperatures. The heat effects were measured for TEX in NMP. The molar enthalpies and the differential molar enthalpies for TEX in NMP were also obtained at the same time. The corresponding kinetic equations that describe the four dissolution processes are da/dt = 10 -2.64 (1-a) 1.31 (T = 298.15 K), da/dt = 10 -2.58 (1-a) 1.31 (T = 303.15 K), da/dt = 10 -2.54 (1-a) 1.51 (T = 308.15 K), da/dt = 10 -2.49 (1-a) 1.03 (T = 313.15 K), and respectively. The values of activation energy E a and preexponential factor A for TEX in the dissolution process are 16.84 kJ mol -1 and 10 0.32 s -1 .

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4,10-Dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo[5.5.0.0^5,90^3,11]dodecane Synthesis

Cited by 11 publications

References 5 publications

Thermal properties of TEX decomposition or sublimation

Thermal properties of TEX decomposition or sublimation

An Improved and Scalable Synthesis of Insensitive High Explosive 4,10-Dinitro-2,6,8,12-tetraoxa-4,10-diazaisowurtzitane (TEX)

Dissolution properties of 4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazaisowutrzitane in N-methyl pyrrolidone

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4,10-Dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo[5.5.0.05,903,11]dodecane Synthesis

Cited by 11 publications

References 5 publications

Thermal properties of TEX decomposition or sublimation

Thermal properties of TEX decomposition or sublimation

An Improved and Scalable Synthesis of Insensitive High Explosive 4,10-Dinitro-2,6,8,12-tetraoxa-4,10-diazaisowurtzitane (TEX)

Dissolution properties of 4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazaisowutrzitane in N-methyl pyrrolidone

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Product

Resources

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4,10-Dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo[5.5.0.0^5,90^3,11]dodecane Synthesis