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  • Author or Editor: Rongzu Hu x
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Abstract  

A device of measuring the thermal conductivity of pellet of propellants and explosives has been constructed. A method and a calculation formula for determining the thermal conductivity of pellet of propellants and explosives under constant radial heat flow conditions by use of Joule effect is presented. Using this device and a microcalorimeter, type RD496-II, and two standard samples with known thermal conductivity, two instrument constant have been determined and the thermal conductivities of seven materials: plexiglass, teflon, DB propellant DB-2 (nitrocellulose(NC)/nitroglycerine(NG)/dinitrotoluene/dimethyl centralite/vaseline/PbO/CaCO3, 59.6/25/8.8/3/1.2/1.2/1.2), DB propellant SQ(NC/NG/diethyl phthalate(DEP)/binder, 59/29/7/5), DB propellant RHN-149 (NC/NG/triacetin (TA)/binder-I, 52/25/8/15), DB propellant RHN-190 (NC/NG/TA/ binder-II, 52/26/7/15), 2, 4, 6-trinitrotoluene (TNT) at 298 K are measured. The results show that (1) the reproducibility of measurement for the heat (q) retained in investigated system after cutting the Joule current and the amount of heat flux through the wall of the investigated cylinder (Q s) are less than 0.50% and within 0.10%, respectively; (2) the standard deviation of the thermal conductivity determined by using this method is less than 1.0%; (3) the values ofq, Q s and internal radius of the cylinder are three principal factors affecting the magnitude of the thermal conductivity of these materials.

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Journal of Thermal Analysis and Calorimetry
Authors: Hu Rongzu, Li Jiamin, Liang Yanjun, Wu Shanxiang, Sun Lixia, and Wang Yaping

The enthalpies of the crystal transformation from I to II and from II to III and the melting enthalpy of 2,2,2-trinitroethyl-4,4,4-trinitrobutyrate (TNETB) are determined by means of Calvet microcalorimeter. On cooling, the supercooing from liquid to solid does not appear, and form II will transform to form I when 71.8° C is reached. The phase diagrams of TNETB-2,4,6-trinitrotoluene (TNT) and TNETB-polyester systems have been constructed by differential scanning calorimetry (DSC). The eutectic temperatures are 56° C and 34° C respectively. The compositions corresponding to the eutectic points are 52 and 46 weight percent TNETB respectively.

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Under linear temperature increase condition the thermal behavior, mechanism and kinetic parameters of the exothermic first-stage decomposition reaction of the title compound have been studied by means of DSC, TG, DTA, IR and mass spectrometry. The mechanism of above-mentioned reaction could be expressed by the following scheme. The apparent activation energy, pre-exponential constant and reaction order of this reaction are 112 kJ/mol, 109.62sec−1 and 0 respectively.

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Journal of Thermal Analysis and Calorimetry
Authors: Xing Xiaoling, Xue Liang, Zhao Fengqi, Yi Jianhua, Gao Hongxu, Xu Siyu, Pei Qing, Hao Haixia, and Hu Rongzu

Abstract

The enthalpies of dissolution in ethyl acetate and acetone of hexanitrohexaazaisowurtzitane (CL-20) were measured by means of a RD496-2000 Calvet microcalorimeter at 298.15 K, respectively. Empirical formulae for the calculation of the enthalpy of dissolution (Δdiss H), relative partial molar enthalpy (Δdiss H partial), relative apparent molar enthalpy (Δdiss H apparent), and the enthalpy of dilution (Δdil H 1,2) of each process were obtained from the experimental data of the enthalpy of dissolution of CL-20. The corresponding kinetic equations describing the two dissolution processes were for dissolution process of CL-20 in ethyl acetate, and for dissolution process of CL-20 in acetone.

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Abstract  

The thermal decomposition mechanism of hydrazine 3-nitro-1,2,4-triazol-5-one (HNTO) compound was studied by means of differential scanning calorimetry (DSC), thermogravimetry and derivative thermogravimetry (TG-DTG), and the coupled simultaneous techniques of in situ thermolysis cell with rapid scan Fourier transform infrared spectroscopy (in situ thermolysis/RSFTIR). The thermal decomposition mechanism is proposed. The quantum chemical calculation on HNTO was carried out at B3LYP level with 6-31G+(d) basis set. The results show that HNTO has two exothermic decomposition reaction stages: nitryl group break first away from HNTO molecule, then hydrazine group break almost simultaneously away with carbonyl group, accompanying azole ring breaking in the first stage, and the reciprocity of fragments generated from the decomposition reaction is appeared in the second one. The C–N bond strength sequence in the pentabasic ring (shown in Scheme 1) can be obtained from the quantum chemical calculation as: C3–N4 > N2–C3 > N4–C5 > N1–C5. The weakest bond in NTO is N7–C3. N11–N4 bond strength is almost equal to N4–C5. The theoretic calculation is in agreement with that of the thermal decomposition experiment.

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Abstract

A novel energetic material, 4,5-dihydroxyl-2-(dinitromethylene)-imidazolidine (DDNI), was synthesized by the reaction of FOX-7 and glyoxal in water at 70 °C. Thermal behavior of DDNI was studied with DSC and TG-DTG methods, and presents only an intense exothermic decomposition process. The apparent activation energy and pre-exponential factor of the decomposition reaction were 286.0 kJ mol−1 and 1031.16 s−1, respectively. The critical temperature of thermal explosion of DDNI is 183.78 °C. Specific heat capacity of DDNI was studied with micro-DSC method and theoretical calculation method, and the molar heat capacity is 217.76 J mol−1 K−1 at 298.15 K. The adiabatic time-to-explosion was also calculated to be a certain value between 14.54 and 16.34 s. DDNI presents lower thermal stability, for its two ortho-hydroxyl groups, and its thermal decomposition process becomes quite intense.

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Journal of Thermal Analysis and Calorimetry
Authors: Liang Xue, Feng-Qi Zhao, Xiao-Ling Xing, Zhi-Ming Zhou, Kai Wang, Hong-Xu Gao, Jian-Hua Yi, Si-Yu Xu, and Rong-Zu Hu

Abstract

The thermal decomposition behaviors of 1,2,3-triazole nitrate were studied using a Calvet Microcalorimeter at four different heating rates. Its apparent activation energy and pre-exponential factor of exothermic decomposition reaction are 133.77 kJ mol−1 and 1014.58 s−1, respectively. The critical temperature of thermal explosion is 374.97 K. The entropy of activation (ΔS ), the enthalpy of activation (ΔH ), and the free energy of activation (ΔG ) of the decomposition reaction are 23.88 J mol−1 K−1, 130.62 kJ mol−1, and 121.55 kJ mol−1, respectively. The self-accelerating decomposition temperature (T SADT) is 368.65 K. The specific heat capacity was determined by a Micro-DSC method and a theoretical calculation method. Specific heat capacity equation is (283.1 K < T < 353.2 K). The adiabatic time-to-explosion is calculated to be a certain value between 98.82 and 100.00 s. The critical temperature of hot-spot initiation is 637.14 K, and the characteristic drop height of impact sensitivity (H 50) is 9.16 cm.

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BTATz-CMDB propellants

High-pressure thermal properties and their correlation with burning rates

Journal of Thermal Analysis and Calorimetry
Authors: Jian-Hua Yi, Feng-Qi Zhao, Ying-Hui Ren, Bo-Zhou Wang, Cheng Zhou, Xiao-Ning Ren, Si-Yu Xu, Hai-Xia Hao, and Rong-Zu Hu

Abstract

The high-pressure thermal properties and their correlation with burning rates of the composite modified double base (CMDB) propellants containing 3,6-bis (1H-1,2,3,4-tetrazol-5-yl-amino)-1,2,4,5-tetrazine (BTATz), a substitute of hexogen (RDX), were investigated using the high-pressure differential scanning calorimetry (PDSC). The results show that there is a main exothermal decomposition process with the heating of each propellant. High pressure can restrain the volatilization of NG, accelerate the main decomposition reaction, and make the reaction occur easily. High pressure can change the main decomposition reaction mechanism function and kinetics, and the control process obeys the rule of Avrami–Erofeev equation at high pressure and chemical reaction at normal pressure. However, the mechanism function can not be changed by the ballistic modifier. The correlation between PDSC characteristic values and burning rates was carried out and found that u and keep a good linear relation, k u keeps a similar changing trend with u, and it can be used to study the effect of the ballistic modifier or the other component on the burning rates.

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Journal of Thermal Analysis and Calorimetry
Authors: Liang Xue, Feng-Qi Zhao, Xiao-Ling Xing, Zhi-Ming Zhou, Kai Wang, Hong-Xu Gao, Jian-Hua Yi, and Rong-Zu Hu

Abstract

The thermal decomposition behavior of 3,4,5-triamino-1,2,4-triazole dinitramide was measured using a C-500 type Calvet microcalorimeter at four different temperatures under atmospheric pressure. The apparent activation energy and pre-exponential factor of the exothermic decomposition reaction are 165.57 kJ mol−1 and 1018.04s−1, respectively. The critical temperature of thermal explosion is 431.71 K. The entropy of activation (ΔS ), enthalpy of activation (ΔH ), and free energy of activation (ΔG ) are 97.19 J mol−1K−1, 161.90 kJ mol−1, and 118.98 kJ mol−1, respectively. The self-accelerating decomposition temperature (T SADT) is 422.28 K. The specific heat capacity of 3,4,5-triamino-1,2,4-triazole dinitramide was determined with a micro-DSC method and a theoretical calculation method. Specific heat capacity (J g−1K−1) equation is C p = 0.252 + 3.131 × 10−3 T (283.1 K < T < 353.2 K). The molar heat capacity of 3,4,5-triamino-1,2,4-triazole dinitramide is 264.52 J mol−1 K−1 at 298.15 K. The adiabatic time-to-explosion of 3,4,5-triamino-1,2,4-triazole dinitramide is calculated to be a certain value between 123.36 and 128.56 s.

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Abstract

The thermal decomposition behavior of composite modified double-base propellant containing hexanitrohexaazaisowurtzitane (CL-20/CMDB propellant) was studied by microcalorimetry. The kinetic and thermodynamic parameters were obtained from the analysis of the heat flow curves. The effect of different proportion of CL-20 to the thermal decomposition behavior, kinetics, and thermal hazard was investigated at the same time. The critical temperature of thermal explosion (T b), the self acceleration decomposition temperature (T SADT), and the adiabatic decomposition temperature rise (ΔT ad) were calculated to evaluate the thermal hazard of the CL-20/CMDB propellant. It shows that the CMDB propellant with 38% CL-20 has relative lower values of E and lgA, and with 18% CL-20 has the highest potential hazard.

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