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1.
乔琛  梁义  吴金婷  谌思嘉  赵廷兴  张勇  黄明  李鸿波 《含能材料》2022,30(11):1135-1141
高纯度2,4,6-三硝基-5-乙氧基-1,3-苯二胺(DATNEB)可作为内标物,通过高效液相色谱法对含氯法合成的1,3,5-三氨基-2,4,6-三硝基苯(TATB)的纯度进行精确分析。为研究DATNEB的合成及其含能特性,以苦味酸为原料,经4-氨基-1,2,4-三唑(ATA)氨化,原甲酸三乙酯乙基化两步制得高纯DATNEB,总收率为32.5%,纯度≥99.8%。产物经红外(IR)、核磁(1H NMR、13C NMR)、质谱(MS)以及单晶X-射线衍射确证结构。对苦味酸双氨基化机理和中间体二氨基苦味酸羟基乙基化机理进行了探讨,且对DATNEB热性能和爆轰性能进行了研究。结果表明,DATNEB为单斜晶系,空间群为P21/c,晶体学参数为:a=1.21261(7) nm,b=0.89654(4) nm,c=1.12310(6) nm,V=1.17675(11) nm3,Z=4,D=1.62 g·cm-3。吸热峰温为193.9 ℃,放热峰温为236.0 ℃,具有较好的热稳定性。理论爆速为7.05 km·s-1,爆压为21.14 GPa,总体爆轰性能与三硝基甲苯(TNT)相当,但感度远低于TNT和环三亚甲基三硝胺(RDX)。因此合成的高纯DATNEB不仅可作为内标物,用于分析含氯法合成的TATB纯度,还有望作为熔铸炸药的辅助组分。  相似文献   

2.
周诚  李吉祯  李祥志  屈蓓  常佩  王伯周  刘宁 《含能材料》2020,28(12):1163-1169
在甲醇/水溶剂中培养了3,5-二硝氨基-1,2,4-三唑肼盐(HDNAT)单晶,利用X射线单晶衍射仪测定了结构;晶体结构解析表明HDNAT属于正交晶系,空间群为P2(1),晶胞参数a=0.35976(12) nm,b=0.9348(3) nm,c=1.1833(4) nm,V=0.393.9(2) nm3,Z=2,Dc=1.91 g·cm-3,μ=0.170 mm-1,F(000)=230;采用TG-DTG分析了HDNAT的热性能,其分解峰温为193.17 ℃,分解历程为固相直接分解;设计并制备了含HDNAT的改性双基推进剂(CMDB)配方,测试了爆热、比容、密度、特征速度、比冲等能量特性参数和燃烧性能,实测爆热为6042 kJ·kg-1、比容为638 L·kg-1、密度为1.767 g·cm-3、特征速度为1592.3 m·s-1;Φ50 mm发动机燃烧性能实测结果表明,在15 MPa压强下工作稳定,比冲可达到250.91 s,燃速较RDX-CMDB推进剂提高18.8%以上,但推进剂的部分压强指数超过0.4以上。  相似文献   

3.
AEFOX-7的晶体结构和燃烧焓(英)   总被引:2,自引:2,他引:0  
孙倩  李彦峰  徐抗震  宋纪蓉  赵凤起 《含能材料》2015,23(12):1235-1239
制备了1-氨基-1-乙氨基-2,2-二硝基乙烯(AEFOX-7)水合物的单晶并测定了其结构,该晶体属于立方晶系,空间群是Pna2(1)/m,晶体参数为:a=1.3692(3) nm, b=0.71240(16) nm, c=0.9024(2) nm, β =90°, V=0.8802(4) nm3, Z=4,μ=0.133 mm-1, F(000)=408, Dc =1.465 g·cm-3, R1 =0.0306 and wR2 =0.0855。测定了AEFOX-7、 1-氨基-1-甲氨基-2,2-二硝基乙烯(AMFOX-7)和1,1-二氨基-2,2-二硝基乙烯(FOX-7)的燃烧焓,相应的标准摩尔燃烧焓分别是: -(2347.83±4.84),-(1819.96±5.94) kJ·mol-1和-(1159.77±1.30) kJ·mol-1。  相似文献   

4.
以1-叔丁基-3-硝基-3-羟甲基氮杂环丁烷盐酸盐为原料,经氧化-叠氮化、成盐、硝化等反应合成了具有偕叠氮硝基的熔铸炸药3-叠氮基-1,3-二硝基氮杂环丁烷(AzDNAZ),总收率达到58.8%,采用红外光谱、~1H NMR、~(13)C NMR及元素分析等对中间体及最终产物进行了结构表征;培养了新的中间体1-叔丁基-3-叠氮基-3-硝基氮杂环丁烷硝酸盐的单晶,X射线单晶衍射分析表明:1-叔丁基-3-叠氮基-3-硝基氮杂环丁烷硝酸盐晶体结构属单斜晶系,空间群为P2(1)/n,a=0.8281 (314) nm,b=0.8607(2) nm,c=1.7195(2) nm,α=90°,β=95(2)°,γ=90°,V=1.2210(6) nm~3,Z=4,M_r=262,D_c=1.427 g·cm~(-3),μ=0.1 74 mm~(-1),F(000)=552,R=0.041 8,wR_2=0.1 1 68。利用DSC-TG方法分析了热性能,结果表明:AzDNAZ的熔点为78.2℃,分解点为180.7℃。采用Gaussian 09程序和Kamlet-Jacobs方程预估了AzDNAZ的性能,结果表明:AzDNAZ的密度为1.75 g·cm~(-3),生成焓为331.73 kJ-mol~(-1),爆速8460 m·s~(-1)爆压31.83 GPa。表明AzDNAZ可以作为熔铸炸药和含能增塑剂的候选含能材料。  相似文献   

5.
研究了3,6-二硝基吡唑[4,3-c]并吡唑(DNPP)的百克量级合成工艺,总收率由9.3%提高到17.9%。采用IR、1H NMR、13C NMR、元素分析、质谱等方法对中间体及DNPP的结构进行了表征。探讨了环化、还原“一锅法”反应机理及反应安全性;改进了重氮盐中间体的后处理方法: 采用冷冻结晶法代替萃取法,操作简单,避免大量使用有机溶剂,收率从77.0%提高到86.1%; 培养了DNPP·H2O单晶,晶体结构分析表明,DNPP·H2O为单斜晶系,空间群为P2(1)/c,晶体学参数为: a=0.3480(4) nm,b=1.4134(16) nm,c=0.9027(11) nm,α=90°,β=94.327(16)°,γ=90°,V=0.4427(9)nm3, Z=4,Dc=1.756g·cm-3,μ=0.164 mm-1,F(000)=240,R1=0.0503,wR2=0.1391。  相似文献   

6.
为获得3,3-双(叠氮甲基)氧杂环丁烷-四氢呋喃共聚醚(PBT)-甲苯二异氰酸酯(TDI)黏结剂体系固化反应行为规律,采用微热量热法研究了固化温度、固化比以及增塑剂对PBT-TDI体系固化反应的影响,并对PBT-TDI体系的固化反应动力学和热力学进行了研究与分析。实验结果表明:(1)固化反应温度越高、固化剂TDI含量越多,PBT-TDI体系固化反应速度越快;(2)增加增塑剂2,2-二硝基丙醇缩甲醛与2,2-二硝基丙醇缩乙醛混合物(A3)以及癸二酸二辛酯(DOS)用量会降低PBT-TDI体系的固化反应速度;(3)PBT-TDI体系的固化反应符合n级反应动力学模型,其表观活化能Ea为12.81 kJ·mol-1,指前因子A为1.48×10-2 s-1。  相似文献   

7.
黄晓川  王子俊  郭涛  刘敏  邱少君 《含能材料》2015,23(12):1240-1242
以5-氨基-1,2,4三唑基-5-乙酸(1)为原料,经Sandmeyer反应得到一种新型叠氮三唑类化合物5-叠氮基-1,2,4-三唑-5-乙酸(ATAA)。通过1H NMR、13C NMR、IR及元素分析等手段对化合物结构进行表征。TG及DSC的研究表明,ATAA的热行为包括结晶水脱除、熔化及热分解三个过程,每个过程所对应的峰值温度分别为85.6,168.0 ℃和177.9 ℃。基于ATAA设计出一种新型多硝基含能化合物——5-叠氮基-3-硝仿基-1,2,4-三唑(2),并对其爆轰性能进行预估。结果表明其标准生成焓、理论密度及理论爆速分别为449.62 kJ·mol-1、1.91 g·cm-3和9096 m·s-1,整体性能与HMX相当。  相似文献   

8.
马丛明  刘祖亮  姚其正 《含能材料》2015,23(12):1176-1180
以2-氯-4-氨基吡啶(1)为原料,经硝化反应合成出一种新的偶氮桥吡啶衍生物(E)-1,2-双(2-氯-3-硝基吡啶基-4-基)二氮烯(3)和2-氯-4-氨基-3,5-二硝基吡啶(2),随后经胺化反应分别得到(E)-1,2-双(2-氨基-3-硝基吡啶基-4-基)二氮烯(5)和2,4-二氨基-3,5-二硝基吡啶(4),总的得率分别为69%和18%。室温下,用氯仿作溶剂得到化合物3的红色晶体用于X-射线衍射分析。用Kamlet-Jacobs经验方程计算了化合物4和5的爆轰性能。结果表明,化合物3为单斜晶系,空间群P21/N,晶胞参数为:a=9.965(2) , b=6.3190(13) , c=10.737(2) , β= 93.75(3)°, V=674.6(2) 3, Dc=1.689 g·cm-3, C10H4Cl2N6O4,Mr=171.55, F(000)=344, μ(Mo Kα)=0.510 mm-1, Z=4。化合物4的爆轰性能与2,4,6-三硝基甲苯(TNT)相当,而化合物5的爆轰性能不佳。  相似文献   

9.
用3-硝基-1,2,4-三唑-5-酮(NTO)的锂盐水溶液和硫酸锰水溶液反应制得[Mn(H2O)6](NTO)2·2H2O,对它进行了元素分析与红外表征。[Mn(H2O)6](NTO)2·2H2O的结构用单晶分析法测定,其空间群为 C2/C,晶胞参数 a=23.423(3)Å,b=6.5262(9)Å,c=19.412(3)Å,a=90.00(0)°,β=142.713(7)°,γ=90.00(0)°,V=1797.6(4)Å3,Z=4,Dc=1.70 g·cm-3,μ=7.87cm-1,F(000)=947.75。  相似文献   

10.
以乙二醛(40%)和硝基甲烷为原料,通过缩合、硝化两步反应生成了新型硝酸酯类含能增塑剂6b-硝基-1,3,5-三氧环戊烷-并环戊二烯-2,4,6-三硝酸酯(2),总收率为40.90%,并采用红外光谱、核磁共振光谱和元素分析对其进行了表征。首次培养并获得了化合物2的晶体结构,晶体结构分析表明,该化合物属于单斜晶系,晶体空间群为P21/n; 晶胞参数为: a=7.792(9),b=8.534(9), c=19.41(2) , β=117.624(4)°, Mr=370.16, V=1305(2) 3, Z=4, Dc=1.884 g·cm-3, λ=0.71073 ,F(000)=752, μ =0.189 mm-1, S=1.097,最终偏差因子 R1=0.0488,wR2=0.1289。  相似文献   

11.
Tetraacetyldibenzylhitane (TADBIW) was subjected to debenzylation by nitrosating with inorganic materials available commercially to synthesize tetraacetyldinitrosohexaazaisowurtzitane (TADNSIW). TADNSIW was purified, and its structure was determined by FTIR, 1H NMR, MS and element analysis. The debenzylation reaction of TADBIW gave quantitative benzaldehyde as a by-product. This indicates that the reaction produces an imine cation as an intermediate. Hexanitrohexaazaisowurtzitane (HNIW) was prepared from unpurified TADNSIW with the yield over 96.0 % and the purity more than 98.0 %. And the mechanism of the reaction from TADNSIW to HNIW is proposed to be oxidation of nitroso and nitration of acetyl on the molecule of TADNSIW, This reaction system involved is simple, and the reaction can complete within a short time and under mild conditions. The product can be easily to separate and the waste disposed readily.  相似文献   

12.
The technique of watermarking has been introduced into 2D vector maps for many potential applications such as protecting the copyright of important GIS (geographical information system) data and tracing the data source of military maps. In most previous works, although the validity of the map data could be preserved during the embedding procedure, the shape-distortions of the map elements are usually neglected which would tend to degrade the invisibility of the watermarking schemes. A shape-preserving algorithm for watermarking 2D vector maps is presented in this paper. A 1D distance sequence extracted from the original map is adopted as the cover data instead of 2D coordinates. A watermark bit is represented by changing the distributions of the cover data. The embedding procedure induces lower shape-distortions than in former works. Experimental results indicate better invisibility of the proposed scheme, as well as its robustness to certain attacks such as map simplification, interpolation, additive noise and most geometric transforms.  相似文献   

13.
The stability under illumination of transmission-mode GaAs photocathode sealed in the third generation intensifier is investigated by use of spectral response testing instruments. The variations of spectral response with the illumination times under weak and intense illumination are compared. The variations of photoemission performance parameters are also characterized. The results show that during initial several weak illuminations photocathode behaves no evident decay and a maximum sensitivity is achieved, while under intense illumination the sensitivity of photocathode begin to decrease largely at the first illumination. The calculated performance parameters show that the variation of surface escape probability with illumination times is a direct cause of instability of photocathode. It is also found that under intense illumination peak wavelength is moved towards short-wave and peak response is decreased, which shows that the ability of long-wave response of photocathode is decreased.  相似文献   

14.
Open rule-setting method advanced in this paper concentrates on providing designers of engines with a convenient way to express their design innovations and develop the expected prototypes in the early CAD stage, and constitute effective models for the following analysis process of CAE and CAPP. The problems arisen in the process of conceptual design with the traditional experience-based development method are analyzed. Based on those analyses, open rule-setting method is presented and some associated technical problems are discussed. The functional framework of open rule-setting system was built as software engineering methods. The speciality of the engine product as a kind of complex product and the requirement of the engine product based on its structural particularity to rule-setting system are considered carefully. A demonstration is supplied to illustrate how the open rule-setting method enhances the efficiency and quality of the engine conceptual design.  相似文献   

15.
By analyzing the working principle of Linux network device driver, discussing the Linux network driver structure and its key technologies, the general network driver structure and its design methodologies in Linux system are summarized. Through modifying the network device driver of Linux device driver 3rd version snull, c and improving the COW technology, the Zero-Copy technology in Linux (kernel version 2.6.11 ) is implemented. In the end, the success test tells us that the thorough analysis of network device driver is the foundation of many applications, and it also provides a certain improvement to a lot of real applications, even to military application development.  相似文献   

16.
By analyzing the influencing factors of part quality making of sheet alloy of titanium by vibra cutter, the shape of upper reamer is set as cylinder and wedge-shaped form, and the lower reamer as plain and hemicycle form, and its main structural parameters are defined as well. Then it is validated further that such improved vibra cutter reamer can be used to process curve-edged parts of titanium alloy sheet. The experimental result shows that the titanium alloy sheet parts processed by above equipment have no sharpen angles for convex parts and evident crevasse of concave-edged part. In summary, such improvement can eliminate the free-waved edge and improve the manufacture quality of titanium alloy sheet parts greatly.  相似文献   

17.
The initiating behavior of fine-grained explosives by small flyer is studied. The diameter of small flyer in this device is 1 ram. The test results indicate that the granularity of explosives has great effect on its flyer initiating sensitivity.The flyer initiating sensitivity of the fine-grained explosives is higher and the critical initiating energy is lower than that of common explosives. For common explosive, the flyer initiating sensitivity increases as the density is reduced. But for the fine-grained explosive, the test results are exactly opposite.  相似文献   

18.
A Passive Acoustic Radar is presented as a necessary complement to electromagnetic wave radar, which will be expected to be an effective means for detecting cruise missiles. Acoustic characteristics of supersonic flying projectiles with diverse shapes are expounded via experiment. It is pointed out that simulation experiment could be implemented using bullet or shell instead of cruise missile. Based on theoretical analysis and experiment, the ““acoustic fingerprint““ character of cruise missile is illustrated to identify it in a strong noise environment. After establishing a locating mathematical model, the technique of acoustic embattling is utilized to resolve a problem of confirming the time of early-warning, considering the fact that velocity of sound is much slower than that of light. Thereby, a whole system of passive acoustic radar for detecting supersonic cruise missile is formed.  相似文献   

19.
Multi-laser-target tracking is an important subject in the field of signal processing of laser warners. A clustering method is applied to the measurement of laser warner, and the space-time fusion for measurements in the same cluster is accomplished. Real-time tracking of multi-laser-target and real-time picking of multi-laser-signal are introduced using data fusion of the measurements. A prototype device of the algorithm is built up. The results of experiments show that the algorithm is very effective.  相似文献   

20.
The nonlinear dynamic model of spinning ballistic missiles is established during the first boosting phase of the missile. Based on the conventional backstepping sliding mode control and the assumption of a two time-scale separation of missile dynamics, a graded sliding mode controller is designed with two sub-sliding surfaces which have invariability to external disturbances and parameter perturbations, and a matrix which comprises three first order low pass filters is introduced to prevent "explosion of terms". Owing to the upper bounds of the uncertainties are difficult to obtain in advance, adaptive laws are introduced to estimate the values of the uncertainties in real-time. Eventually, the numerical simulation results given to show the proposed controller can ensure the steady flight of missiles.  相似文献   

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