5-氨基四唑合成的反应热和工艺优化研究

利用全自动量热化学反应仪(SIMuLAR)研究了Stolleet法合成5-氨基四唑的化学反应热和各种反应参数的变化过程。结果表明：5-氨基四唑合成反应的摩尔生成热为130．35kJ。mol^-1。最适宜的硝酸用量是等当量的，反应的pH值应控制在2．5—5．5之间，最经济的反应时间是120min。在反应后期有一个剧烈的放热峰，瞬时放热达到65W。     

微波辅助合成1-甲基-2,4,5-三碘基咪唑

在微波加热条件下,以N-甲基咪唑为原料,用I2/HIO3的酸性溶液碘化合成1-甲基-2,4,5-三碘基咪唑（MTII）。采用红外光谱、元素分析和高效液相色谱等方法对合成产物MTII进行了结构表征和纯度分析,讨论了反应温度、反应时间、碘、碘酸用量对碘代反应的影响。结果表明,碘代反应的最佳反应条件为：反应温度80℃,反应时间60min,n （I2）：n （HIO3）∶n （C4H6N2）=2∶3∶1,高效液相色谱分析表明MTII纯度大于98％。     

新法合成5-氨基四唑

以氨基胍硝酸盐为原料,重氮化后,调节反应溶液至弱碱性,加热分子内环化得到5-氨基四唑,并采用红外光谱、核磁共振光谱、质谱等方法,进行了结构表征.探讨了5-氨基四唑合成反应机理,考察了环化反应溶液酸碱性、反应温度及反应时间等关键因素对反应的影响,获得适宜反应条件为:重氮化反应pH=2～3、温度为20～30℃、时间为0.5...     

一种改进的3-氨基-4-硝基呋咱合成方法

以3,4-二氨基呋咱(DAF)为原料,过氧化氢为氧化剂,以钨酸钠-草酸为共催化剂,代替传统合成方法的钨酸钠-浓硫酸共催化剂,合成了3-氨基-4硝基呋咱(ANF)。采用正交设计的方法,考察了反应时间、反应温度和共催化剂用量对产率的影响,最终得到ANF合成的较佳工艺条件:反应时间6h,反应温度30℃,共催化剂与原料摩尔比1∶1,在上述条件下ANF产率可达33.7%。     

5-氨基四唑硝酸盐的合成工艺优化及结构表征

以5-氨基四唑一水化合物(5-AT·H2O)为原料,与硝酸反应一步制得5-氨基四唑硝酸盐(5-ATN)。研究了硝酸用量、反应温度和反应时间对目标物合成的影响。通过正交实验得到最优合成工艺:20℃下,5 g 5-AT·H2O与15 mL浓硝酸(65%)边搅拌边反应15 min,目标物产率达92.6%。和文献报道比较,该工艺反应温度降低、时间缩短、产率提高。表面形貌分析与吸湿性测试结果表明目标产物晶体表面光滑、吸湿性低。     

3,6-二氨基-1,2,4,5-四嗪-1,4-二氧化物的合成与表征

以3，6-对（3，5-二甲基吡唑）-1，2，4，5-四嗪（BT）为起始物，经取代反应合成了3，6-二氨基-1，2，4，5-四嚷（DATZ），产率95．3％，再经过氧蚁酸氧化得到四嗪类高氮低感度炸药——3，6-二氨基-1，2，4，5-四嗪-1，4-二氧化物（DATZO2），产率60．2％；利用IR、NMR、MS、元素分析和DSC等对其结构进行了表征和确认，并对合成反应条件进行了初步探讨，认为最佳反应条件为DATZ1．12g（0．01mol），甲酸20ml，双氧水4ml，25℃反应1h。     

［MIMPS］［HSO4］催化N2O5硝化2,6-二乙酰氨基吡嗪-1-氧化物

制备了1-磺酸丙基-3-甲基咪唑硫酸氢盐[MIMPS][HSO4]离子液体,以[MIMPS][HSO4]作为催化剂,应用于N2O5/有机溶剂硝化2,6-二乙酰氨基吡嗪-1-氧化物合成2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105).通过1 H NMR,IR和MS对LLM-105及其中间体的结构进行了表征.研究了在[MIMPS][HSO4]催化条件下,反应溶剂、催化剂用量、反应温度和反应时间对LLM-105收率的影响,结果表明最佳反应条件为:采用CH3NO2为反应溶剂,反应温度为55 ℃,反应时间为6h,LLM-105的收率为72.2％.研究了[MIMPS][HSO4]的循环使用性能.结果表明,平行实验5次,平均收率71.7％,具有较好的可再生利用性.     

富氮化合物研究进展

富氮化合物是具有良好应用前景的烟火型气体发生剂原料，对具有含氮量高、热稳定性好和生成焓高的一些四唑、四嗪、呋咱类富氮化合物的合成方法及它们的性能进行了综述，重点描述了3，6-(1H-1，2，3，4-四唑-5-氨基)-1，2，4，5-四嗪(BTATZ)、3，3′-偶氮双(6-氨基-1，2，4，5-四嗪)(DAAT)、1，1′-二甲基-5，5′-偶氮四唑(DMATZ)和3，6-(2H-5-四唑基)-1，2，4，5-四嗪(BTT)的合成路线。     

TMPSHSO4催化N2O5/有机溶剂硝化2,6-二乙酰氨基吡啶-1-氧化物

以2,6-二乙酰氨基吡啶-1-氧化物（DAPO）为原料,在Ⅳ,Ⅳ,Ⅳ-三甲基-N-丙磺酸基-硫酸氢铵（TMPSHSO4）催化条件下,采用N2O5／有机溶剂硝化2,6-二乙酰氨基毗啶制得2,6-二氨基-3,5-二硝基吡啶-1-氧化物（ANPyO）。考察了在TMPSHSO4催化条件下反应溶剂、温度和时间对ANPyO产率的影响,结果表明最佳反应条件为：反应溶剂为CH3NO2,反应温度为60℃,反应时间为5h,ANPyO产率为92．5％。用^1HNMR,IR和MS对ANPyO的结构进行了表征。     

3,3′-二(四唑-5-基)二呋咱基醚的合成与表征

以3-氨基-4-氰基呋咱为起始原料,经氧化、醚化、环化三步反应合成了未见文献报道的化合物3,3′-二(四唑-5-基)二呋咱基醚,总收率46.7%,经¹³C NMR、IR、MS、元素分析确认了其结构。确定了环化反应适宜的反应条件： 反应时间4 h,ZnCl₂·2H₂O为催化剂,n(ZnCl₂·2H₂O):n(FOF-2)=1:1,并对锌盐催化的四唑环合成机理进行了探讨。     

Nitrosation and Nitration of Tetraacetyldibenzylhexaazaisowurtzitane

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.     

A Robust Algorithm for Watermarking 2D Vector Maps with Low Shape-Distortions

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.     

Open Rule-setting System Applied to Conceptual Design of Engines

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.     

Research on Linux Network Device Driver

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.     

Improvement and Experiment of the Reamer in Vibra Cutter Against Wave Edge of Titanium Sheet Alloy Parts

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.     

Experimental Study on the Small Flyer Initiating Behavior of Fine-grained Explosives

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.     

Algorithm for Multi-laser-target Tracking Based on Clustering Fusion

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.     

Influence of Installing Error on the Surface Shape Precision of the Axial Symmetry Aspheric Workpiece in Lapping

A method to calculate the surface shape error, which is caused by the installing error between the workpiece and the lapping tool in the process of form lapping, is proposed. The mathematical model which the installing translation error influences on the workpiece surface shape error is established. The changing rule of the error is simulated through the calculating example of the paraboloid workpiece. The results indicate that the surface shape error of the workpiece is increasing with the increase of the installing translation error, it is also increasing gradually along the center point of the curve surface to the edge, and the influence is severer to the curve surface with great curvature than that of the small curvature when the translation error is the same.     

Experimental Research on Output Performances of Giant Magnetostrictive Actuator

The paper introduces the performances of magnetostrictive actuators and its applications, discusses the design methods for the structure and internal magnetic circuit of a giant magnetostrictive actuator, and makes tests on the output displacement and force characteristics for an actuator using homemade magnetostrictive material. The experimental result shows that the actuator has satisfactory output precisions and ranges in transient and stable states, and can be used in lowfrequency vibration control system of precise equipment.     

Robust Graded Sliding Mode Tracking Control for Low Speed Spinning Ballistic Missiles

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.