烯丙基二甲基海因的合成及表征

为了增强复合固体推进剂中粘合剂基体与固体氧化剂之间的界面键合作用,提高推进剂的力学性能,采用盖布瑞尔(Gabriel)合成法合成了具有反应基团的海因类衍生物3-烯丙基-5,5-二甲基海因(ADMH),反应条件为: n(5,5-二甲基海因):n(溴丙烯):n(KOH的醇溶液)=1:1:1,水为溶剂,温度为65 ℃,反应时间为3 h,石油醚两次重结晶后得到结晶形态的产物,产率为50%.通过X射线衍射、热分析、紫外、核磁共振、红外、质谱、元素分析和高效液相色谱对产物进行了全面的分析表征.结果表明,产物为目标物,纯度达到99. 97%,熔点65～66 ℃,初始分解温度为168.3 ℃,目标物有望在复合固体推进剂中得到较好的应用.     

重结晶法级配六硝基茋(HNS)的实验研究

采用溶剂-非溶剂法重结晶级配六硝基茋(HNS),研究在同一系统中同时实现六硝基茋重结晶细化为不同粒径颗粒的粒度级配体系.以二甲基甲酰胺(DMF)为溶剂,水为非溶剂,通过改变溶液温度﹑溶液浓度﹑搅拌速度和滴加速度4个影响因素,研究其与系统中HNS的粒度大小和分布的关系,最终确定了两种粒度(1～2μm,10～15μm)级配的最佳工艺条件,以及对级配产生主要影响的因素为溶液浓度和溶液温度,并从理论上进行了分析.     

偶氮四唑二胍的合成优化与性能表征

以5-氨基四唑(5-AT)为原料,经过氧化和合成两步反应制得偶氮四唑二胍(GZT)。研究了反应温度、反应时间、原料配比和NaOH溶液的浓度对合成该物质的影响,表明该法制备GZT的优化反应条件为:5-AT的用量为0.10 mol时,NaOH溶液的浓度为1.5 mol.L-1,5-AT与KMnO4的摩尔比为3∶3,在80℃下反应60 min。放大实验平均产率在80%以上。并通过元素分析、红外光谱分析、核磁、热重-差热分析,对产物的物性、组成和结构进行了表征。     

2,2,4,4-四硝基金刚烷的合成与表征

以金刚烷酮为原料,经Baeyer-Villiger氧化、内酯重排、缩酮化、氧化和偕硝化等单元反应合成了2,2,4,4-四硝基金刚烷。优化了重要中间体4,4-乙撑二氧基金刚烷-2-酮的合成方法。使用绿色硝化剂五氧化二氮对酮肟进行偕硝化反应,考察了溶剂、温度、反应时间、物料配比对第一步偕硝化反应的影响,确定了最佳反应条件:溶剂为二氯甲烷,n(4,4-乙撑二氧基-2-金刚烷酮肟)∶n(五氧化二氮)=1∶3,反应温度为45℃,反应时间为30 min,收率为52.3%。本路线总收率为14.2%,是文献报道的2.9倍。     

高纯3,3'-二氨基-4,4'-氧化偶氮呋咱(DAOAF)的合成工艺

以乙二醛和盐酸羟胺为原料,经一步法合成中间体3,4-二氨基呋咱(DAF),收率48.0%,纯度99.8%。在NaHCO_3溶液缓冲体系中,DAF经过硫酸氢钾(KHSO_5·0.5KHSO_4·0.5K_2SO_4)氧化制得3,3'-二氨基-4,4'-氧化偶氮呋咱(DAOAF),采用IR、~1H NMR、MS等对其结构进行确证,通过高效液相色谱的面积归一化法测定产品纯度并定性、定量分析产品中所含杂质。考查了氧化反应中反应物投料比、反应时间与温度对收率的影响,获得最佳合成工艺为:n(DAF)∶n(NaHCO_3)∶n(KHSO_5·0.5KHSO_4·0.5K_2SO_4)=1∶6∶4,反应时间5 h,反应温度20~25℃,粗品收率为84.1%,纯度98.2%。粗品DAOAF经HPLC分析确定杂质为DAF、副产物DAAF和ANF。粗品于95℃经DMF重结晶可有效除去杂质,从而制得高纯DAOAF(纯度99.6%),总回收率为86.6%。     

1-甲基-3-氨基-5-硝基-1,2,4-三唑的合成新工艺

以甲基肼为原料,与盐酸反应得到盐酸甲基肼,再与二氰二胺在50℃进行缩合环化反应,调节溶液pH值,经重氮化反应合成含能化合物1-甲基-3-氨基-5-硝基-1,2,4-三唑(DNMT),总收率62.3%,纯度99.4%,并用红外光谱、核磁共振、质谱、元素分析等方法表征了其结构。探讨了缩合环化反应工艺条件,确定适宜的反应条件为:溶剂为乙醇,n(C2H3N4)∶n(NH2NHCH3.2HCl)=1∶1.1,pH=8~9,成盐组分是盐酸,重结晶溶剂为丙酮。     

CL-20重结晶过程中的晶型转变研究进展

介绍了不同晶型六硝基六氮杂异伍兹烷(HNIW,CL-20)(包括α-、β-、γ-、ε-及ζ-)的结构、热稳定性及性能。综述了CL-20的重结晶方法(包括溶剂-非溶剂法和溶剂挥发法)以及在溶液中的晶型转变。认为:ε-CL-20最有应用价值,不能直接合成,它需通过重结晶得到,但结晶时的晶型转变会降低ε-CL-20晶型的纯度,从而影响爆轰性能。讨论了溶剂和温度对CL-20晶型转变的影响。根据Ostwald规则,从热力学和动力学角度解释了CL-20的晶型转变过程。指出了现有研究的不足,提出了通过控制CL-20的晶型转变路径、优化重结晶条件,以获得晶型纯度高的ε-CL-20的新思路。     

DMF-水球形化重结晶HMX工艺研究

为获得球形化效果好的HMX,研究了DMF-水球形化重结晶HMX的工艺影响因素.结果表明:在温度为57℃、搅拌速度为140r/min、V溶剂:V非溶剂=1:3.5和稀释速度为0.153mL/min的条件下,重结晶所得的HMX晶体球形化效果最好,且具有更高的密度和更好的热安定性.     

2,6-二氨基-3,5-二硝基吡啶-1-氧化物的精制

研究了2,6-二氨基-3,5-二硝基吡啶-1-氧化物(ANPyO)经酰化、重结晶和还原的新精制工艺,考察了精制工艺条件对ANPyO纯度、粒径分布、机械感度、摩擦感度和微观结构的影响。对比了新精制工艺样品和三氟乙酸精制样品的酸度、熔点、热安定性和撞击感度。结果表明,精制中间体2,6-二乙酰氨基-3,5-二硝基吡啶-1-氧化物采用DMF作溶剂重结晶,氨气作胺化剂,50 ℃条件下所得ANPyO产物总收率为90.5%,纯度为99.5%,样品的粒度、微观结构和安全性能较理想。新精制工艺所得产物pH为6.3,熔点355 ℃,真空安定性0.01 mL·g-1,撞击感度257 cm,摩擦感度2%,性能显著优于三氟乙酸精制所得ANPyO产物。     

3-硝基-1,2,4-三唑-5-酮(NTO)废酸的循环利用

针对3-硝基-1,2,4-三唑-5-酮(NTO)硝化过程中产生大量废酸导致“三废”综合治理成本高的问题,通过向废酸中补加少量工业浓硝酸制成质量分数为70%的硝酸溶液作为硝化剂,硝化1,2,4-三唑-5-酮(TO),循环合成目标化合物NTO。采用红外光谱、核磁共振光谱、元素分析对其进行了结构表征。考察了硝化剂用量、反应时间、反应温度对产品的影响,优化了硝化反应条件,确定硝化的最佳反应条件为: n(TO)n(HNO₃)=16,反应温度60~65 ℃,反应时间1 h,纯度可达99.9%。废酸循环利用10次以上,平均收率82%,硝酸用量减少了67.6%。      

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.