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Solubility study and selective purification of HMX explosive in organic electrolyte solution of zinc acetate/diethylene glycol

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Defence Technology（防务技术） 2023年第11期29卷 15-23页

作者： Javad Ghorbani sajjad damiri Hamid Reza Pouretedal Faculty of Applied Sciences Maleke-ashtar University of TechnologyP.O.Box83145/115Iran

In this study, an organic electrolyte solution based on zinc acetate/diethylene glycol(ZA/DEG) is introduced for the selective purification of cyclotetramethylene tetranitramine(HMX) high explosive from its identical homologue cyclotrimethylene trinitramine(RDX). The dielectric constant of various organic solutions were investigated through Electrochemical Impedance Spectroscopy(EIS) in the range of 1.0 Hz—30 MHz. and some quantum-chemical descriptors of RDX and HMX dissolutions in the ZA cosolvent were analyzed using Density Functional Theory(DFT). The results show dielectric constant and solubility of RDX is higher than that of HMX, and by increasing of ZA concentration in DEG solvent, the values of dielectric constants were enhanced. Furthermore, the presence of ZA cosolvent on the solubility of two explosives was statistically investigated by Central Composite Design(CCD) of experiment, and some solubility parameters including activity coefficient, dissolving enthalpy, and mixing enthalpies were determined. The experimental results indicate that the weight ratio of RDX to HMX solubility in the proposed organic electrolyte changes up to 30 times, which provides a selective and sequential separation method to separate two materials with similar chemical properties with a separation efficiency>98% and HMX purity> 99.8%. The X-Ray Diffraction(XRD) analysis, High-Performance Liquid Chromatography(HPLC), Laser-Induced Breakdown Spectroscopy(LIBS), and Fourier Transform Infrared Spectroscopy(FT-IR) approves the acceptable quality of the separated materials. The proposed method makes the efficient and safe purification of high-quality HMX for application in oil and gas well perforating gun charges, using a nonvolatile and inflammable organic electrolyte.

关键词： Organic electrolyte Purification Solubility HMX RDX Diethylene glycol

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The non-isothermal gravimetric method for study the thermal decomposition kinetic of HNBB and HNS explosives

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Defence Technology（防务技术） 2020年第1期16卷 251-256页

作者： Hamid Reza Pouretedal sajjad damiri Zahra Bighamian Faculty of Applied Chemistry Malek-ashtar University of TechnologyShahin-ShahrIran

The hexanitrostilben(HNS) is a thermally stable explosive that can be prepared from hexanitrobibenzyl(HNBB).Therefore,the investigation of thermal stability of HNBB can be important in the yield of preparation of *** decomposition kinetic of HNBB and HNS are studied by non-isothermal gravimetric *** TG/DTG curves in non-isothermal method are obtained in range of 25℃-400℃at heating rates of 3℃/min,5℃/min,8℃/min,10℃/min and 12℃/*** data of weighttemperature are used for calculation of activation energy(E_a) of thermal decomposition reactions by methods of Ozawa,Kissinger,Ozawa-Flynn-Wall(OFW) and Kissinger-Akahira-Sunose(KAS) as modelfree methods and Strink's equation as model-fitting *** compensation effect is used for prediction of mechanism and determination of pre-exponential factor(InA) of the decomposition reaction.A reduction 60 kj/mol for the average of activation energy of thermal decomposition reaction of HNBB is obtained versus *** result shows the lower thermal stability of HNBB in comparison to HNS,The Avrami equation(A_(3/2)) with function f(α)=3/2(1-α)[-In(1-α)]^(1/3) indicates the predicted mechanism for thermal decomposition reaction both explosives.

关键词： HNS HNBB Decomposition Thermal Kinetic

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Study the operating conditions on agglomeration of RDX particles in anti-solvent crystallization by using statistical optimization

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Defence Technology（防务技术） 2019年第2期15卷 233-240页

作者： Hamid Reza Pouretedal sajjad damiri Ali Zandi Department of Chemistry Faculty of Science Malek-Ashtar University of Technology

The unfavorable growth and agglomeration of micro-particles of RDX explosive was almost observed in manufacture process. For preventing of growth of micro-particles and agglomeration in anti-solvent crystallization process, the effect of additives glucose, sucrose and poly ethylene glycol-2000 and wetting solvent of isopropyl alcohol were studied. Taguchi experimental design was used for optimization of the operating conditions. The type of additive, the amount of additive(%wt.), solvent of wetting and wetting time were selected for optimization of the conditions. By using 4 factor and 3 levels, 27 experiments were conducted(L27). Results showed that in the presence of 2 %wt. of sucrose additive and isopropyl alcohol solvent, the agglomerations of particles were decreased so that a decrease 30-50% in the average of particles size was seen. Addition additives were effective in storage container and for reduce the agglomeration of particles during storage. Also, the agglomeration rate of particles was reduced over time at optimized conditions. Imaging optical microscopy, scanning electron microscopy(SEM), and particle size analyzer(PSA) methods were used for particles size analyzing as a response in statistical optimization and quality control of the final product. The sensitivity to some mechanical and shock stimuli on the RDX in presence of sucrose additive was tested and the obtained results showed the insignificant effect of additive on the safety properties of pure RDX.

关键词： RDX explosive Taguchi experimental design Agglomeration Additive Anti-solvent

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Increasing of photostability of HNS explosive in the presence of UV photostabilizers

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Defence Technology（防务技术） 2021年第2期17卷 338-342页

作者： Hamid Reza Pouretedal sajjad damiri Zynab Karami Faculty of Applied Sciences Malek Ashtar University of TechnologyIran

The photostabilies of hexanitrostillbene(HNS)were studied at 1%*** *** photostabilizers of Chiguard BP-12(UV-531),ADK STAB LA-326(UV-326),ADK STAB LA-32(UV-P),Irganox 1010 and Everstab LS944 were used in this study.A photoreactor including a 30 W monochromatic UV lamp was used for investigation of photodegradations of solid *** changes in surface area of HNS peak in HPLC chromatogram at time intervals of 2,4,6 and 8 h were used for calculation of kinetic rate constants of photodegradation *** compound of UV-P photostabilizer was found to have the greatest effect on enhancing photostability for HNS among the investigated *** kinetic rate constants were obtained 6.2×10^(-2) and 4.1×10^(-2)h^(-1),respectively,for photodegradation process of HNS in absence and in presence of UV-P.

关键词： HNS explosive Photodegradation Photostabilizer Kinetic rate constant

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Modification of RDX and HMX crystals in procedure of solvent/anti-solvent by statistical methods of Taguchi analysis design and MLR technique

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Defence Technology（防务技术） 2018年第1期14卷 59-63页

作者： Hamid Reza Pouretedal sajjad damiri Abolfazl Shahsavan Faculty of Applied Chemistry Malek-ashtar University of Technology (MUT)

Many of the physical and functional properties of RDX and HMX explosives are related to the crystalline structure of these materials. Crystalline defects affect the quality of the explosives. Therefore, in order to enhance the quality of these materials, it is necessary to form crystals with the lowest defects. In this research, we report the optimization of recrystallization process of RDX and HMX by statistical techniques. The solvent/anti-solvent procedure was used for recrystallization of HMX and RDX particles. The four parameters of i) ratio of anti-solvent to solvent, ii) ratio of solute to solvent, iii) aging time, and iv)cooling rate of mixture, were optimized by Taguchi analysis design. Taguchi L16 orthogonal array was used with sixteen rows corresponding to the number of tests in four columns at four levels. The apparent density of recrystallized of RDX and HMX particles was considered as the quality characteristic with the concept of "the larger-the-better". The obtained graphs showed that the studied parameters were optimized in ratio 1:1 for anti-solvent to solvent, ratio 0.1 g,m L^(-1) for solute to solvent, aging time of 2 h and cooling rate of 1℃,min^(-1). Also, the correlation between the investigated parameters and apparent density of crystals were studied by multiple linear regressions(MLR) method for obtaining a model of prediction of apparent density. The P-values were indicated that in confidence level of 95%, the null hypothesis is rejected and a meaningful addition is observed in the proposed model.

关键词： HMX RDX Solvent/anti-solvent Taguchi analysis Apparent density

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Micro-seeding and soft template effects on the control of polymorph and morphology of HMX micro particles in solvent-antisolvent process

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Defence Technology（防务技术） 2017年第6期13卷 392-396页

作者： sajjad damiri Shahriar Namvar Hadi Panahi Department of Applied Chemistry Maleke-ashtar University of TechnologyShahin-shahrEsfahanIran

A seeding strategy was developed in the preparation of cyclotetramethylenetetranitramine(HMX)explosive micro-particles by solvent-antisolvent method, to control their polymorphs from dangerous gamma(y) type to the desired and standard beta(β) form with the size distribution of <10.0 μm, by using a low concentration of β-HMX fine particles as micro-seed in the antisolvent medium. All products were characterized by X-ray diffraction(XRD), scanning electron microscopy(SEM), and dynamic light scattering particle size analyzer. In the next step, the effective factors on the sizes and morphologies of micro-particles in the presence and absence of two soft templates of poly(ethylene glycol)-400(PEG-400) polymer and coconut fatty acid diethanolamide(lauramide) surfactant were investigated. The results of experiments showed that using of water-soluble PEG-400 in the low antisolvent temperatures leads to the production of very spherical particles. Also non-ionic surfactant of lauramide, direct the crystal growth to needle-like structures. The advantages of this method are its capability for the simple production of β-HMX micro-particles in the large scale production process, with the various crystal structures and particles size distributions.

关键词： Micro seeding Polymorph HMX Explosive Micro-particle Solvent-antisolvent process

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The kinetic of mass loss of grades A and B of melted TNT by isothermal and non-isothermal gravimetric methods

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Defence Technology（防务技术） 2018年第2期14卷 126-131页

作者： Hamid Reza Pouretedal sajjad damiri Parvaneh Nosrati Ehsan Forati Ghaemi Faculty of Applied Chemistry Malek-ashtar University of Technology

The kintic and activation energy of mass loss of two grades of melted TNT explosive, grade A and grade B, with freezing points of 80.57 and 78.15 ℃, respectively, were studied by isothermal and nonisothermal gravimetric methods. In isothermal method, the mass loss of samples in containers of glass and aluminum was followed in temperatures of 80, 90 and 100 ℃. The kinetic of the mass loss of the samples in the aluminum container was higher than the kinetic of it in the glass container that can be related to the effects of heat transfer and catalytic of aluminm metal. Also, the presence of impurities in grade B was due to increasing of kinetic of mass loss of it versus grade A. The non-isothermal curves were obtained in range of 30-330 ℃ at heating rates of 10,15 and 20 ℃·min^(-1).The TG/DTG data were used for determination of activation energy(E_a) of mass loss of TNT samples upon degradation by using Ozawa, Kissinger, Ozawa-Flynn-Wall(OFW) and Kissinger-Akahira-Sunose(KAS) methods as model free methods. The activation energies of grades of A and B of TNT was obtained 99-120 and 66-70 kJ mol^(-1)respectively. The lower values of activation energy of the degradation reaction of grade B confirm the effect of impurities in the kinetics of mass loss of this grade.

关键词： TNT Isothermal Non-isothermal Kinetic Mass loss

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