ZHOU Cheng , ZHOU Yan-shui , HUO Huan , BI Fu-qiang , WANG Bo-zhou , MA Ya-nan
2011, 19(3):243-246. DOI: 10.3969/j.issn.1006-9941.2011.03.001
Abstract:1,1-Diamino-2,2-dinitroethylene (FOX-7) was investigated in oxidation reactions. 1-Chloro-1,1-dinitro-2- (N-chloro-amidino)-ethane was obtained in a mixture of potassium permanganate and concentrated hydrochloric acid with the yield of 70%. The reactivity of electrophilic substitution reaction of FOX-7 was confirmed,and the reaction mechanism was investigated. The structure was identified by NMR,IR,MS and elemental analysis. The single crystal of 1-chloro-1,1-dinitro-2-(N-chloro- amidino)-ethane was cultivated from dichloromethane. The crystal structure was determined by a X-ray single crystal diffractometer. Results show that the empirical formula is C2H2Cl2N4O4 and the formula weigh is 216.98,the crystal is orthorhombic system,space group Pbcn with crystal parameters of a=0.9940(17) nm,b=1.0628(19) nm,c=1.4487(3) nm,V=1.5304(5) nm3,Z=8,Dc=1.883 g·cm-3,F(000)=864 ,R1=0.0325,ωR2=0.0784. The compound′s melting point is 90 ℃,decomposition temperature is 136.6 ℃,so,the thermal stability is short of FOX-7.
LI Ya-ni , YANG Jian-ming , YU Qin-wei , XUE Yun-na , Lü Jian
2011, 19(3):247-251. DOI: 10.3969/j.issn.1006-9941.2011.03.002
Abstract:Through the reaction of ethylenediamine (EDA) and derivatives of triazole and imidazole with N,N-dinitrourea (DNU),six energetic ionic salts were prepared. Among them,EDA gave diacidic salt,others derivatives gave monoacidic ones. The effects of solvent,reaction temperature and time on yield of salt from 4-aminotriazole and DNU were analyzed. The yield could be up to 85% in acetonitrile and 71% in ethanol at 10 ℃ for 2 h. Generally,polar solvents with high dielectric constant are beneficial to the salt-forming reaction. The structures of all salts prepared were confirmed and discussed by IR,1H NMR,13C NMR and elemental analysis. The thermal stability of most salts surpasses DNU,for instance,EDA-DNU salt started its decomposition at 125 ℃ (ca. 55 ℃ higher than that of DNU),exhibited the largest mass loss rate at 165 ℃ in TGA curve.
WANG Nai , SHI Yu , YANG Hong-wei , CHENG Guang-bin , Lü Chun-xu
2011, 19(3):252-257. DOI: 10.3969/j.issn.1006-9941.2011.03.003
Abstract:Direct nitrolysis of hexamethylenetetramine(HA) catalyzed by ionic liquids (ILs) was studied. The effects of dosage of IL and different ILs on the nitrolysis were investigated in the systems of 95% HNO3 and N2O5/HNO3.In the system of 95%HNO3,[Hmim]NO3 shows the best catalytic activity in all of ILs we screened. The optimal reaction condition is 1.5mol% IL loading,12:1 of quality ratio of 95% HNO3 to HA and 90 min of reaction time at -5~0 ℃. RDX can be obtained in yield of 75.9% using IL as catalyst under optimized condition,while RDX can be gererated in lower yield of 68.3% without adding IL. In the system of N2O5/HNO3,[Bmim]BF4 shows the best catalytic activity. The optimal reaction conditions are 5mol% IL loading,9:1 of mass ratio of 100% HNO3 to HA,2:1 of quality ratio of 100% HA to N2O5 and 60 min of reaction time at -5~0 ℃. Under optimized conditions,77.6% yield of RDX can be obtained without adding IL,while yield of RDX can be improved to 85.4% using IL as catalyst. It indicates that ILs have observably catalytic activity on the direct nitrolysis of HA.
ZHANG Gong-zheng , XIANG Xing , FANG Yong-xi , WANG Xiao-chuan
2011, 19(3):258-261. DOI: 10.3969/j.issn.1006-9941.2011.03.004
Abstract:2,2-Dinitropropyl acrylate - styrene (DNPA-St) copolymer was synthesized by free radical polymerization in ethyl acetate by using azobisiosbutyronitrile as initiator. The structure and properties of DNPA-St copolymer were also characterized by FTIR,1H NMR and DSC measurements. The behavior of the copolymerization between 2,2-dinitropropyl acrylate (DNPA) and styrene (St) was studied,the composition of the copolymer was determined using infrared spectrum method, and the reactivity ratios of DNPA and St were measured. Results show that the reactivity ratios of DNPA and St was obtained by using the Fineman-Ross method,rDNPA=0.911 and rSt=0.038,respectively. The polymerization of DNPA with St is a non-ideal copolymerization,and the products are random copolymers. The glass transition temperature and thermal decomposition temperature of the DNPA-St copolymer is 63.3 ℃ and 251.4 ℃. It is compatible with RDX and HMX,and thermal stability.
LI Ya-nan , ZHANG Zhi-zhong , ZHOU Yan-shui , WANG Bo-zhou , GE Zhong-xue
2011, 19(3):262-268. DOI: 10.3969/j.issn.1006-9941.2011.03.005
Abstract:3,4-Bis(3′,5′-dinitrobenzene-1′-yl)furoxan was synthesized via five-step reactions of oximation,diazotization,denitrification,cyclization and nitration using benzonitrile as starting materials. The reaction conditions were optimized,and the cyclization could be performed at 2~10 ℃ within 3 h and Na2CO3 in excess of 20% with a yield of about 64.7%. The product′s structure was characterized by IR,NMR,MS and elemental analysis. In addition,the mechanism of the key reaction-cyclization was suggested. The vicarious nucleophilic substitution of hydrogen(VNS) reaction of the target compound was explored,and it could not go under the conditions applied by the authors. Furthermore,the thermal decomposition of this furoxan was studied with differential scanning calorimetry(DSC),IR,and thermogravimetry/mass spectrum(TG/MS),and the related mechanism was proposed and analysed in detail. The initial step of decomposition is dissociation of N—O bond with coordination oxygen in furoxan ring.
HU Huan , YANG Hong-wei , CHENG Guang-bin , Lü Chun-xu
2011, 19(3):269-271. DOI: 10.3969/j.issn.1006-9941.2011.03.006
Abstract:5-Aminotetrazole was synthesized via a novel route by diazotization and intramolecular cyclization conditioning the reaction system at basic,and aminoguanidine nitrateas as starting material. The resulting 5-aminotetrazol was characterized by IR,13C NMR,and Ms etc. The mechanism of the reaction was proposed. The key factors affecting the yield,such as acidity or basicity of reaction system,reaction temperature and time, were also investigated. The optimized procedures are as follows: for diazo-reaction: pH=2~3,T=20~30 ℃ and t=0.5 h; for intramolecular cyclization: pH=8~9,T=85~90 ℃ and t=3.5 h. The yield of 5-aminotetrazole could be up to 77.2%.
ZHENG Wei , WANG Jiang-ning , XIE Bo , SONG Xiu-duo , TIAN Jun , YUAN Zhi-feng
2011, 19(3):272-275. DOI: 10.3969/j.issn.1006-9941.2011.03.007
Abstract:The physic-chemical properties,safety properties,combustion properties and inner ballistic properties of composite modified double-based propellant containing hexanitrohexaazaisowurtzitane(CL-20) (CL-20/CMDB) propellants were studied. Results show that the burning rate of CL-20/CMDB propellant is 2.5~8.94 mm·s-1 higher than that of RDX/CMDB propellant at 6~20 MPa. The pressure exponent of CL-20/CMDB propellant is greater,which is up to 0.28 at 10~20 MPa. CL-20/CMDB propellant has higher density,explosion heat and specific volume than that of RDX/CMDB propellant. The density,explosion heat and specific volume of CL-20/CMDB propellant is 1.76 g·cm-3,5034 J·g-1 and 658 L·kg-1,respectively. CL-20/CMDB propellant has the same chemical stability as RDX/CMDB propellant,lower impact sensitivity than RDX/CMDB propellant,but higher friction sensitivity,up to 100%; the specific impulse of CL-20/CMDB propellant can achieve 2226.1 N·s·kg-1(227 s) in Φ36 rocket motor.
HAO Hai-xia , PEI Qing , NAN Bao-jiang , ZHANG Heng , XIAO Li-bai , ZHAO Feng-qi
2011, 19(3):276-281. DOI: 10.3969/j.issn.1006-9941.2011.03.008
Abstract:Laser ignition characteristics of double-based (DB) propellant SQ-2 and RDX-CMDB propellants were studied by CO2 laser ignition at different laser fluxes. The effects of content of RDX,Al powder and burning catalysts on ignition characteristics of RDX-CMDB were discussed. Results show that the laser ignition delay time of DB propellant SQ-2 and RDX-CMDB propellants except the sample containing Al powder becomes shorter with the heat fluxes increasing,and its change slows down. The influence of the content of RDX,the additives of Al powder and the burning catalysts on the ignition delay time was related with the laser fluxes. The content of other components had little effect on the laser ignition delay time of propellants. Al powder could prolong the delay time at lower heat fluxes,and the delay time increased with increasing of the content of RDX,and Al powder and the catalysts in the propellant had both great influence on the laser ignition process and the delay time of the propellants at the higher heat fluxes.
LI Liang-liang , WANG Jiang-ning , KONG Jun-li
2011, 19(3):282-286. DOI: 10.3969/j.issn.1006-9941.2011.03.009
Abstract:The influence of ratio of 3, 4-bisnitrofurazanfuroxan(DNTF) to RDX on dynamic mechanical properties for modified double-based propellants(DNTF/RDX-CMDB,DFR) was studied by dynamic mechanical analyzer(DMA). The characteristic values of dynamic mechanical properties at multi-frequency for DFR series propellants were obtained. Results show that the ratio of DNTF to RDX content can obviously affect the dynamic mechanical properties of DFR propellants. Two β-relaxations(signed β1 and β2 respectively),besides α-relaxation,appear on DMA curves of DFR propellants,and one of them(β1-relaxation) is due to the effect of DNTF,that′s to say,the plasticization of DNTF to NC molecular can not be affected by adding RDX. The whole β-relaxations peak values(∑tanδ) for CMDB,both the DNTF and RDX added,is bigger than that only RDX added,hence,the plastic or toughness has been improved while the ability to resist external forces increased at low temperature. The DFR propellant that mass ratio of DNTF to RDX is 10:40 has optimal plastic or toughness at low temperature.
WANG Ying , ZHANG Xiao-hong , CHEN Xue-li , XIE Wu-xi , FU Xiao-long
2011, 19(3):287-290. DOI: 10.3969/j.issn.1006-9941.2011.03.010
Abstract:The mechanical properties of single-chamber dual thrust grain were studied especially on the interface of the two propellant grains. The tensile strength and the elongation of propellants with different compositions prepared by different technologies were measured at 20 ℃,50 ℃,and -40 ℃. The surface appearance and the element distribution on the failure surface were analyzed by scanning electron microscopy (SEM) and X-ray photoelectron spectrum (XPS). Results show that the interfacial mechanical properties are close to that of cast propellant,and the mechanical properties of the interface has almost no effect on the whole mechanical properties of propellant. Al2O3 powders,one of the components in the propellant,are found to cumulate around the interface.
ZHENG Shen-sheng , GUAN Li-feng , DONG Lan , WU Kui-xian
2011, 19(3):291-294. DOI: 10.3969/j.issn.1006-9941.2011.03.011
Abstract:Hydroxyl-terminated polybutadiene(HTPB)/N100 reaction kinetics was investigated by method of the ratio of concentration and time. Matlab software was applied to calculate the reaction order and rate constant under different temperatures. The effects of various additions of catalyst on reaction rate,and the relationship between time and viscosity for HTPB/N100 reaction were studied. Results show that the reaction of HTPB/N100 belongs to the first order reaction,and activation energy is 70.57 kJ·mol-1. With the increasing of catalyst proportion,the reaction rate constants increase,and the established exponential model for time-dependent of reaction system reveals their quantitative relationship.
DONG Jun , ZHAO Sheng-xiang , HAN Tao , GAN Xiao-xian , ZHOU Wen-jing , ZHENG Lin , FENG Xue-song , WANG Cai-ling
2011, 19(3):295-298. DOI: 10.3969/j.issn.1006-9941.2011.03.012
Abstract:In order to investigate the effect of the energetic thermoplastic polyurethane elastomer (ETPE) with number average molecular weight of about 20000 as binder synthesized by 3,3-bisazidemethyl oxetane (BAMO) and 3-azidemethyl-3-methyl oxetan (AMMO) on the sensitivity of RDX-Al moulding powder,the contact angle of ETPE with RDX and Al powder was measured. The adhesion work and spread modulus between ETPE and RDX as well as ETPE with Al powder were calculated by the contact angle data. The scanning electron microscopy (SEM) photography and mechanical sensitivity of the explosive moulding powders with different contents of ETPE were observed and measured. The results show that in RDX-Al system,ETPE is easily coated on the surface of RDX particle. With increasing the dosage of ETPE from 2% to 5% in the RDX/Al system,the viscosity of the explosive system increases,the hot-spots are easy to form under the impact condition and the mechanical sensitivity of the explosive moulding powder increases from 0% to 40%,considering that when the ETPE with number average molecular weight about 20000 is used in pressed RDX-Al system explosives,the dosage of ETPE should be controlled within 5%.
SHANG Yan , YE Zhi-hu , WANG You-bing , LI Ya-nan , WANG Bo-zhou
2011, 19(3):299-304. DOI: 10.3969/j.issn.1006-9941.2011.03.013
Abstract:Ultra-fine 2,2′,4,4′,6,6′-hexanitorstilbene(HNS-IV) was prepared by using solvent/anti-solvent recrystallization method. The effects of solvent factors,drying methods and process parameters,such as different solvents,anti-solvents,washing solvents,temperature,drying methods on the particle size,particle size distribution and morphology of HNS,were investigated. Results show that suitable solvents as follows: dimethylformamide(DMF) was solvent,and H2O was anti-solvent and methanol was wash solvent. The particle size and size distribution can be controled by verifying the amount of solvent,amount of anti-solvent,amount of surfactant,temperature and drying methods. Crystal appearance of HNS is smooth with particle size from 0.5 μm to 1.0 μm.
YUN Sheng , LIU Yu-cun , YU Yan-wu , WANG Jian-hua , GAO Sen
2011, 19(3):305-309. DOI: 10.3969/j.issn.1006-9941.2011.03.014
Abstract:Microspherical and desensitized HMX was prepared by pneumatic spray thinning method. The crystal shape,particle size and thermostability of ultrafine HMX were analyzed by scanning electron microscope and differential scanning calorimetry(DSC),and the impact sensitivity was measured by impact sensitivity analyzer. The results show that: the microspherical and desensitized HMX with average particle size of 450 nm was prepared when pressure was 0.5 MPa,and water temperature was 10 ℃,and concentration was 0.2 g·mL-1,and volume ratio for water to the solution was 80/1. The thermostability of ultrafine HMX is enhanced by 1.0% compared to that of the initial HMX,and the impact sensitivity of ultrafine HMX is decreased by 87% compared to that of the initial HMX.
HAN Bao-cheng , LEI Hong-fei , XU Yu-xin , WANG Shu-shan
2011, 19(3):310-314. DOI: 10.3969/j.issn.1006-9941.2011.03.015
Abstract:For the design of fire-extinguishing ammunition,the mathematic relationship between dynamic action area and stand-off distance was presented. Based on the engineering requirements from optimization design of fuse-warhead cooperate on the fire-extinguishing ammunition,the experiments of static action on the warhead and dynamic dispersed on the simulation ammunition were conducted. The processes of static action and dynamic dispersed were analyzed according to the experimental results. A computational mathematics method on dynamic dispersed processes for the fire-extinguishing ammonization was set up,the correlation between dynamic dispersed area of the fire-extinguishing ammunition and the stand-off distance was obtained by calculation. The calculated results agree well with the experimental results.
NI Xiao-jun , SHEN Zhao-wu , YANG Chang-de
2011, 19(3):315-320. DOI: 10.3969/j.issn.1006-9941.2011.03.016
Abstract:In order to study shock attenuation in aluminum foams,the different thickness of aluminum foam shells were made,shock attenuation in its was preliminarily investigated. Two types of PETN charges were used,one is the PETN itself,the others are confined by aluminum foam shell with thickness of 1.5 cm,2.5 cm and 3.5 cm. The shock wave pressure-time curves were obtained at 0.5 m away from the charge. The experimental data analysis show that aluminum foams shell not only can weaken the peak pressure,but also effectively absorbs the specific impulse and the specific energy of shock wave. Moreover,the whole deforming,crushing and moving processes of the shells were recorded by the underwater camera system. Results show that the attenuation of shock pressure,specific impulse and specific energy in aluminum foams shell was induced by itself deformation and breakup. At the same time,the thickness of aluminum foams shell impacted on the shock attenuation in aluminum foams.
JIANG Zhi-hai , LONG Xin-ping , HAN Yong , JIANG Hong-bin
2011, 19(3):321-324. DOI: 10.3969/j.issn.1006-9941.2011.03.017
Abstract:The high-speed framing photography was applied to observe the shell distorting,expanding fracture mechanism of different thickness shell driven by detonation,and jet forming,developing process of explosion scattering. Scanning electron microscopy (SEM) photographs of fractures in axial and circumferential directions for different thickness fragments were obtained. There are different fracturing modes of the two thickness shells from macroscopic analysis and the collected fragments. Results show that the fragments of 3 mm thickness shell are much bigger,longer and less than that of 1.5 mm. SEM analysis of fragments section show that their formation is mostly caused by the shear fracture. And jet fracturing process of explosion scattering can be divided into three stages: integral injection,interface appearing in flocculent and breaking,small water droplets forming.
LIANG Hua-qiong , HAN Chao , YONG Lian , CHEN Xue-ping , YANG Yong-lin
2011, 19(3):325-329. DOI: 10.3969/j.issn.1006-9941.2011.03.018
Abstract:The polymer-bonded powder was shaped by rubber isostatic pressing (RIP). The effects of process parameters of RIP on the properties of compact were studied. Results show that the process parameters of RIP have a great effect on the shape of compact and density distribution. The higher the pressure and initial relative density,the better are the properties of compact. At the pressure of 160 MPa and initial relative density of 62%,the axial density difference of compact is less than 0.4%,and the RIP tends to isostatic pressing and becomes a net shaping process.
ZHENG Wen-fang , PAN Ren-ming , LIN Xiang-yang , GUO Chang-ping , FU Xiao-li
2011, 19(3):330-334. DOI: 10.3969/j.issn.1006-9941.2011.03.019
Abstract:By using computational method of minimum free energy,the effects of dibutyl phthalate(DBP) on combustion carbon residue of double-based propellant were studied. Results show that DBP has a remarkable effect on the production of carbon residue in the combustion of double-based propellant. A critical value of DBP content exists in the combustion of the propellant. When the threshold has been exceeded,the combustion of double-based propellant can generate carbon residue,and the concentration of carbon residue will increase with the DBP content. To lower the combustion pressure or increase the nitroglycerine content of the propellant can increase the critical value. In addition,the function of the critical value of DBP content and the nitroglycerine content,combustion pressure is established based on the computational results.
ZHENG Shuang , LIU Bo , LIU shao-wu , WANG Feng , ZHANG Yuan-bo , YU Hiu-fang , HAN Bing , LI Da
2011, 19(3):335-338. DOI: 10.3969/j.issn.1006-9941.2011.03.020
Abstract:In order to reduce the erosion and not affect the characteristic of small caliber weapon,a new organic silicon reducing erosion agent was designed and tested. The static combustion and interior ballistic performances of two charges with new organic silicon reducing erosion and 801# reducing erosion were characterized by the closed-bomb and 5.8 mm rifle firing tests. The ablation and burning completeness were tested by erosion tube and oxygen bomb method. The results show that the decreasing of the ablation in the charge with new organic silicon reducing erosion is 13.8%. The charge with new organic silicon reducing erosion has obvious properties of low ablation,steady and complete combustion and is suitable for the small caliber weapons.
2011, 19(3):339-342. DOI: 10.3969/j.issn.1006-9941.2011.03.021
Abstract:A method for detecting the content of β-polymorph in ε-HNIW by Fourier Transform Raman (FT-Raman) spectroscopy was developed. By analyzing the FT-Raman spectra of the four HNIW polymorphs (α-,β-,γ- and ε-),the peaks within 300~270 cm-1 spectral region were used as the quantitative basis of purity detection for ε-HNIW. A series of different (β-,ε-)HNIW mixtures were prepared. The working curves were plotted by analyzing FT-Raman spectroscopy of the mixtures. There is linear relationship between the relative peak height of (β-,ε-)HNIW mixtures and the content of β-HNIW at 282.60 cm-1. The correlation coefficient was 0.9995 and the standard deviation was 0.0158.
SHENG Tao , PENG Qing-tao , XIA Ben-li , ZHANG Guang-you
2011, 19(3):343-348. DOI: 10.3969/j.issn.1006-9941.2011.03.022
Abstract:Components in rocket kerosene were analyzed by gas chromatography-mass spectrometry. In the condition adopted,159 peaks were detected in total ion current chromatogram (TIC) of rocket kerosene,131 peaks among them were identified. The components identified account for 80.37% of total amount of rocket kerosene. It is found in rocket kerosene that,almost half of all components are bicyclo-paraffins,followed by monocyclo-paraffins and iso-alkanes,still by little n-alkanes,oxygen-containing compounds,alkenes,tricyclo-paraffins and aromatics. Most bicyclo-paraffins are alkyldecalins,alkylspiro[5.5]undecanes,and naphthenic cyclohexanes,which respectively account for 49.04%,19.28% and 16.64% of bicyclo-paraffins. Monocyclo-paraffins are mostly alkylcyclohexanes and alkylcyclopentanes,which respectively account for 66.62% and 31.10% of monocyclo-paraffins.
FAN Yong-hui , ZHAO Tie-zhu , YANG Cai-ning , WANG Qiong-lin , YU Hui-fang
2011, 19(3):349-351. DOI: 10.3969/j.issn.1006-9941.2011.03.023
Abstract:A method to determine the content of polyester in desensitized gun propellant by gas chromatography (GC) was established. The polyester was degraded by sodium hydroxied solution,and the products of degradation were analyzed by GC. Results show that there is good relationship between content of polyester and peak area. The linear range is between 3-6 g·L-1,and the correlation coefficient is 0.996. The average recovery is 100.2%,and the relative standard deviation is 1.51%. The method is characterized by good repertability and accuracy,which shows that the method is promising in the analysis of polyester in desensitized gun propellant.
ZHANG Xian-feng , ZHAO Xiao-ning
2011, 19(3):352-360. DOI: 10.3969/j.issn.1006-9941.2011.03.024
Abstract:Detonation mechanism of high explosives was concerned by researchers all over the world for a long time,and lots of researches were focus on the overdriven detonation (ODD) of double layer charges. The development of ODD in double layer charge was introduced. The theoretical models,numerical simulation and testing and observation results of ODD were reviewed. The application and some experimental techniques of ODD were specially addressed. Some research proposals on experimental techniques and theoretical model are made at the end of the paper.
ZHOU Xiao-qing , MA Qing , ZHANG Xiao-yu , CHENG Bi-bo , HUANG Jing-lun , LIAO Long-yu , WANG Jun
2011, 19(3):361-362. DOI: 10.3969/j.issn.1006-9941.2011.03.025
Abstract:5,5′-Hydrazinebistetrazole (HBT) was synthesized by new process,and its thermal property and sensitivity were measured.
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