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1.
以金刚烷为原料,经氧化、肟化,合成了2,6-金刚烷二酮肟,再使用N2O5为硝化剂,直接由2,6-金刚烷二酮肟一步氧化硝化制得了2,2,6,6-四硝基金刚烷,并利用核磁共振(NMR)、红外(IR)、元素分析等对产物进行了表征。研究了物料配比、溶剂、温度、时间对氧化硝化反应收率的影响,确定了最佳反应条件:溶剂为二氯甲烷,摩尔比n(2,6-金刚烷二酮肟)∶n(N2O5)=1∶6,反应温度为50℃,反应时间为30 min,收率为50%。利用热重分析(TG)和差示扫描量热法(DSC)对2,2,6,6-四硝基金刚烷的热性能进行了分析,发现其从275℃开始分解,在298℃时有尖锐放热峰,表明2,2,6,6-四硝基金刚烷具有良好的热稳定性。 相似文献
2.
2,2,4,4-四硝基金刚烷的合成与表征 总被引:2,自引:2,他引:0
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。 相似文献
3.
《含能材料》2020,(7)
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
4.
以3-氰基-4-硝基呋咱为原料,经分子间醚化、加成、重氮化、双肟化得到3,3′-二(N-羟基偕胺肟基)二呋咱基醚(DOFOF),总收率达 51.0%,用IR、1H NMR、13C NMR、元素分析等进行了结构表征。初步优化了双肟化工艺,确定了最佳反应条件: 反应温度 20 ℃,n(DCFOF)n(NH2OH·HCl)n(KOH)= 144。发现了 DOFOF 在碱性条件下易发生歧化反应,分离鉴定了歧化产物 3,3′-二偕胺肟基二呋咱基醚,并从理论上提出了可能的歧化反应机理。 相似文献
5.
以3-氰基~(-1),2,4-三唑为原料,经肟化、重氮化-氯化、硝解、还原、氟化等反应合成了一种含氟偕二硝甲基官能团的新型含能化合物——3-氟偕二硝甲基~(-1),2,4-三唑(FDNMT),利用红外光谱、核磁(~1H NMR、~(13)C NMR)、元素分析和质谱等方法表征了化合物的结构;优化了肟化反应的合成条件:3-氰基~(-1),2,4-三唑和盐酸羟胺摩尔比为1∶1.15,p H值为8,反应时间为2 h,反应温度为60℃,收率为49.0%;获得了FDNMT的单晶并进行了晶体结构解析,该化合物晶体为正交晶系,空间群为Pbcn,晶体学参数为:a=7.4821(11),b=9.8106(15),c=38.683(6),V=2839.5(7)~3,Z=16,μ=0.178 mm~(-1),F(000)=1536;采用Gaussian 09程序中的CBS-4M方法计算了该化合物的生成热,基于密度和计算的生成热,利用Kamlet-Jacobs爆轰方程预估该化合物的爆轰性能:密度1.81 g·cm~(-3),生成热-8.7 k J·mol~(-1),爆速8365.0 m·s~(-1),爆压31.1 GPa,爆热为5614.4 k J·kg~(-1)。 相似文献
6.
3,4-双(3′-硝基苯-1′-基)氧化呋咱的两种合成方法 总被引:1,自引:1,他引:0
分别采用邻二肟氧化脱氢和氧化腈二聚反应两种方法合成了3,4-双(3’-硝基苯-1’-基)氧化呋咱,并利用红外光谱、核磁共振、元素分析、DSC等对其进行了表征。邻二肟氧化脱氢法经苯偶酰硝化反应、羟胺加成、邻二肟氧化关环反应得到目标化合物,总收率为32.4%;氧化腈二聚法经苯甲腈加成、重氮化、氧化腈二聚反应、硝化反应得到了目标产物,总收率为21.0%。DSC结果表明氧化呋咱环开裂放热峰值为280.7℃,放热量为1142J·g^-1。 相似文献
7.
以3,3'-二氰基-4,4'-偶氮呋咱为原料,经加成、重氮化以及硝化等反应得到3,3'-二(偕二硝基甲基)-4,4'-偶氮呋咱(4)及其钾盐(3),四步反应的收率分别为93.3%、91.2%、24.5%和63.1%。在反应过程中分离得到一种未见报道的呋咱化合物——3,3'-二偕氨肟基-4,4'-联氨呋咱(1),推测在羟氨与氰基发生加成反应的过程中,过量羟氨同时将偶氮基还原为联氨基,从而生成1。通过~1H NMR、~(13)C NMR、IR以及质谱等手段对反应中间体及产物结构进行表征。利用差示扫描量热法-热重法研究1、3和4的热分解过程,结果表明:1的热分解包括一个脱结晶水吸热过程和两个热分解放热过程,热失重率分别为5.1%、53.5%和36.3%,吸热峰温为83.7℃,放热分解峰温分别为241.1℃和336.2℃;3的热分解过程仅有一个明显的分解放热阶段,热失重率为86.6%,峰值温度为258.1℃;4的热分解过程也仅有一个明显的分解放热阶段,热失重率为71.8%,其峰值温度为156.0℃。 相似文献
8.
以双环[3.3.1]壬烷-2,6-二酮为原料,经腙化、消除、环氧化、环合、乙酰化、硝化等步骤,合成了一种新型硝基笼形化合物2-硝基-2-氮杂金刚烷-4,8-二醇二硝酸酯,总收率为27%。以硝硫混酸为硝化剂,考察了硫酸与硝酸摩尔比、反应温度、反应时间对硝化反应的影响。确定的最佳反应条件为:摩尔比n(H_2SO_4)∶n(HNO_3)=1∶2,反应温度60℃,反应时间4 h,此时,硝化反应收率达81%。利用热重分析(TG)和差示扫描量热法(DSC)研究了目标化合物的热性能,发现其从170.0℃开始分解,热分解峰温为193.7℃。通过Kamlet-Jacobs公式预估了目标化合物的物化与爆轰性能,其密度为1.71 g·cm~(-3),爆速为5780 m·s~(-1),爆压为11.0GPa。 相似文献
9.
FOX-7合成过程中硝化反应的热危险性 总被引:2,自引:2,他引:0
利用全自动反应量热器(RC1e)测定了1,1-二氨基-2,2-二硝基乙烯(FOX-7)合成过程中的硝化反应热释放速率及传热系数、比热容。结果表明硝化反应加料过程中的平均放热速率约为80 W,保温反应过程中的平均放热速率约为40 W,物料放热量为375.22 kJ·mol-1,理论绝热温升为483.8 K。采用差示扫描量热法(DSC)和热重-微商热重(TG-DTG)法分析了中间体2-(二硝基亚甲基)-5,5-二硝基嘧啶-4,6-二酮的热稳定性,其分解分为两个阶段,起始分解温度为30℃,第一阶段分解峰温为67.01℃,放热量为201.2 J·g-1;第二阶段分解峰温为87.15℃,放热量为1046.6 J·g-1,表明中间体的热稳定性较差。 相似文献
10.
3,5,7-三硝基-1-氮杂金刚烷的合成工艺 总被引:1,自引:1,他引:0
以间二硝基苯(DNB)为原料,经硝化、还原、Henry反应、缩合合成了3,5,7-三硝基-1-氮杂金刚烷,总收率为21.5%。采用熔点测定、IR、NMR对中间体及目标化合物进行了结构表征。研究了硝酸与硫酸摩尔比、混酸用量、加料方式对硝化反应收率的影响。分别采用"分步法"和"一锅法"合成了中间体1,3,5-三羟甲基-1,3,5-三硝基环己烷,并通过提高反应温度缩短了Henry反应时间。研究了酸和碱对缩合反应的影响,并改进了反应工艺。利用热重分析(TG)和差示扫描量热法(DSC)研究了目标化合物的热性能。结果表明,硝化反应的最佳工艺条件为n(HNO_3)∶n(H_2SO_4)=1∶1.5,m(混酸)∶m(DNB)=23,加料方式为先加三分之二的混酸,24 h后再补加三分之一,硝化反应收率达70.7%;提高反应温度后Henry反应的时间缩短12 h,"分步法"的总收率为61.8%,"一锅法"的总收率为83.5%;改进后的缩合反应时间缩短至3天,简化后处理方法依次为过滤、脱色、重结晶,酸和碱都会降低缩合反应的收率;3,5,7-三硝基-1-氮杂金刚烷从225℃左右开始分解,热分解峰温为331℃,表明其热稳定性较好。 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.
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
14.
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
15.
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
16.
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
17.
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
18.
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. 相似文献
19.
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. 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