水悬浮法制备-εHNIW基传爆药的工艺研究

为获得高能低感传爆药,以六硝基六氮杂异伍兹烷为主体炸药,用水悬浮法制备了ε-HNIW为基的传爆药.通过正交试验优化了制备工艺,并对影响包覆效果的主要因素进行了研究.用傅立叶红外光谱(FT-IR)、扫描电子显微镜(SEM)及撞击感度测试等手段对包覆样品进行表征.结果表明,影响包覆效果的因素顺序为:温度＞搅拌速度＞加料速度＞真空度;确定了最佳工艺条件:试验温度70℃、真空度0.05 MPa、搅拌速度700 r/min、加料速度0.725 mL/s.包覆过程中ε-HNIW晶型结构没有发生改变;包覆后样品撞击感度的特性落高H50比原料ε-HNIW提高了27 cm.     

一锅法制备CL–20混合炸药的工艺研究

以CL–20为主体炸药,聚氨酯5702为黏结剂,Span60为表面活性剂,通过一锅造粒法制备了CL–20混合炸药。用单因素实验对影响CL–20混合炸药包覆效果和撞击感度的因素进行了研究,对包覆后的CL–20混合炸药的相关性能进行了测试,得到最佳工艺条件:水浴温度65℃,搅拌器电压为90 V,驱溶时间为1 h,2次加入溶剂的量与高聚物的质量比为4:1。     

水性聚丙烯酸酯顿感包覆CL-20

以CL-20(六硝基六氮杂异伍兹烷)为主体炸药、水性聚丙烯酸酯为胶粘剂,采用泥浆法制备了CL-20基PBX(聚合物粘接炸药)。通过FE-SEM(冷场发射扫描电镜)、XRD(X射线衍射)法对PBX的性能进行了表征。研究结果表明:泥浆法可使水性聚丙烯酸酯成功包覆在CL-20颗粒表面,包覆前后CL-20的晶型没有变化,包覆后CL-20的撞击感度明显降低,其热安定性更好。     

CL-20/RDX共晶炸药的制备与性能测试

为了研究六硝基六氮杂异伍兹烷/环三亚甲基三硝胺(CL-20/RDX)共晶炸药的性能,采用喷雾干燥法制备了质量比为1∶1的CL-20/RDX共晶炸药;通过扫描电镜(SEM)观察了共晶炸药的形貌;采用粉末X-射线衍射法与红外光谱法测试了共晶炸药的结构;采用差示扫描量热法(DSC)测试了共晶炸药的热性能;通过感度实验分别测试了共晶炸药的撞击感度与摩擦感度。结果表明,CL-20/RDX共晶呈球形,粒径在1～5μm; CL-20/RDX共晶的衍射图与CL-20和RDX的衍射图均不完全相同,衍射峰有明显的位移;CL-20/RDX共晶炸药的热分解温度为222.8℃,比CL-20低30℃左右,比RDX低20℃左右,说明共晶的生成对其热性能有较大影响;CL-20/RDX共晶炸药的撞击感度为76%,特性落高为26.9cm,摩擦感度为64%,其机械感度较CL-20有大幅降低,表明共晶炸药的感度显著降低,安全性能得到明显提高,进一步说明共晶在含能材料改性和降感方面的优势。     

喷雾干燥法制备ε-CL-20/EPDM复合炸药及其性能表征

以ε-CL-20(六硝基六氮杂异伍兹烷)为主体炸药,三元乙丙橡胶(EPDM)为胶粘剂,采用喷雾干燥法制备了ε-CL-20基PBX(聚合物粘接炸药)。研究结果表明:通过喷雾干燥法可使EPDM成功包覆在CL-20晶体表面,制得的包覆产物为ε-CL-20/EPDM复合炸药;与细化CL-20相比,ε-CL-20/EPDM的撞击感度明显降低,包覆样品的特性落高(H50)值从25.12 cm升至41.36 cm,表观活化能由182.58 k J/mol增至230.24 k J/mol,热爆炸临界温度由244.18℃增至245.60℃,说明ε-CL-20/EPDM复合炸药的热稳定性更好。     

PVC增塑糊黏度及其经时变化的影响因素

研究了DOP加料方式和加料量、搅拌时间、搅拌速度、搅拌形式、配料温度、配料量、存放温度、测试容器等因素对PVC增塑糊黏度及其经时变化的影响。根据试验结果,建议PVC增塑糊的配制方式为:采用分散盘式搅拌方式,搅拌速度≥1000 r/min,配料与贮存温度为20~30℃,配料罐配备冷却夹套,DOP的加料方式为2次加入。     

一种制备CL-20/LLM-116共晶含能材料的新方法

将直流电通过螺线管产生均匀的磁场,在均匀磁场环境下,以六硝基六氮杂异戊兹烷(CL-20)、4-氨基-3,5-二硝基吡唑(LLM-116)为原料,在匀强磁场环境中,利用溶剂挥发法制备CL-20/LLM-116共晶炸药。采用扫描电子显微镜(SEM)、X射线衍射(XRD)及差式扫描量热仪(DSC)对实验制备的共晶炸药进行表征,结果表明:共晶炸药为块状黄色晶体,与单一CL-20和LLM-116晶体相比形貌有明显变化。共晶炸药的的熔点为148.38℃,分解温度也较单一组分有一定变化,出现2个热分解峰,分解温度分别为244.22℃和251.53℃。综上所述,磁场环境下的溶剂挥发法是一种可行的制备CL-20/LLM-116共晶含能材料的新方法。     

超临界流体反溶剂法制备超细HMX传爆药

为了克服超细炸药在常规包覆过程中易团聚的缺点,采用超临界流体反溶剂法( SAS)制备了以亚微米HMX为主体炸药的超细传爆药,探讨了工艺条件对亚微米HMX包覆效果的影响.结果表明,影响亚微米HMX包覆效果的主要因素有初始浓度、系统温度、系统压力、平均压力升高速率和平均压力下降速率.在加入20 mL的乙酸乙酯、系统压力9....     

CL-20/FOX-7/蜡复合粒子的制备及性能研究

为了提高六硝基六氮杂异伍兹烷(CL-20)的安全性,采用水溶液-悬浮法将FOX-7、微晶蜡包覆在CL-20表面,制备了4种包覆样品;采用扫描电子显微镜法(SEM)、X-射线衍射法(XRD)、傅里叶变换红外光谱法(FTIR)、X射线光电子能谱法(XPS)、差示扫描量热法(DSC)、感度测试法对其微观形貌、晶型、结合方式、包覆效果、耐热性、摩擦感度进行了系统测试分析。结果表明,4种包覆样品均为物理复合,CL-20晶型未发生改变,其中水悬浮法制得的CL-20/FOX-7混合物与机械混合物相比,CL-20表面存在更多的FOX-7粒子,其包覆率为49.83%,热分解峰温为242.79℃,摩擦感度的临界载荷为168N;在混合物中加入微晶蜡后,复合粒子呈类球形,CL-20晶体几乎无外露,但微晶蜡加入的方式对复合粒子性能有较大影响,蜡外包样品的包覆率为64.73%,热分解峰温244.98℃,摩擦感度的临界载荷为360N,较蜡内包样品包覆率提升了5.03%,热分解峰温提升了2.31℃,摩擦感度的临界载荷提升了144N。表明采用FOX-7、微晶蜡可共同对CL-20进行包覆改性,且蜡外包的样品综合性能最好。     

云母钛珠光颜料工艺条件的研究

采用分步加入均相沉淀剂一尿素的方法制备了云母钛珠光颜料。实验主要研究了尿素加入量、反应温度、反应体系pH值、钛液浓度、加料速度和搅拌速度等因素对产品性能的影响,得出了最佳工艺条件。     

CL-20/DNT共晶炸药的制备及其性能研究

以丙酮为溶剂,通过蒸发结晶法制得六硝基六氮杂异伍兹烷(CL-20)/二硝基甲苯(DNT)共晶炸药。利用扫描电镜(SEM)、X射线衍射(XRD)和热重/差示量热法(TGA/DSC)研究了共晶炸药的形貌、结构和热分解特性,测试了CL-20/DNT共晶炸药的机械感度和5s爆发点温度,并计算了其爆轰性能。结果表明,共晶炸药的微观形貌不同于原料CL-20,呈条状晶体;衍射峰明显不同于CL-20/DNT物理混合物的衍射峰,表明有新物相生成。在DSC曲线上,CL-20/DNT共晶几乎没有DNT的熔化吸热峰,而CL-20/DNT物理混合物中有明显的熔化峰,且二者的放热峰峰形和峰位不同;与原料CL-20相比,共晶炸药的分解峰温提前了21℃,放热量(ΔH)和最大热流量(Qmax)分别增加了39%和104%。与CL-20/DNT物理混合物相比,共晶炸药的5s爆发点温度和表观活化能分别增加3.9℃和65.7kJ/mol,撞击感度降低88.9%,摩擦感度降低40%,说明共晶炸药热稳定性增强。CL-20/DNT共晶炸药的理论爆速达到8 340m/s。     

自分层环氧/有机硅丙烯酸酯涂层的影响因素研究

探讨了有机硅添加量、有机硅丙烯酸酯树脂添加量、溶剂、温度等因素对自分层环氧/有机硅丙烯酸酯涂层性能的影响,并采用FTIR-ATR(傅立叶衰减全反射光谱)、SEM(扫描电子显微镜)及表面能等方法对涂层进行了表征。实验结果表明:溶剂用量高于50%,有机硅添加量为0.7%,有机硅丙烯酸酯树脂添加量为树脂总量的40%,固化温度为32℃及颜基比为39.5%时,可获得自分层效果及力学性能最佳的涂层,为自分层涂层的进一步研究和应用提供依据。     

溶剂萃取法回收TNT的安全性研究

为了更好地利用回收的废弃火炸药,以甲苯作为溶剂,利用溶剂萃取法从B炸药中回收TNT组分;采用液相色谱法测定回收TNT的纯度;采用差示扫描量热仪(DSC)和5 s爆发点实验对回收的TNT和对比样品进行了热安定性分析;测定了回收TNT的撞击感度和摩擦感度。结果表明,液相色谱法测得回收TNT纯度为94.19%,对比样品TNT纯度为96.66%;不同升温速率下,回收TNT熔化峰温较对比样品降低了0.9~1.4℃,分解峰温降低了5℃左右,活化能降低3.51 kJ/mol,表明回收TNT的热安定性有所降低;回收TNT的5 s延滞期爆发点为422.7℃,较纯TNT文献值低约53℃,比对比样品TNT高28.5℃;5 s爆发点变化与其所含杂质种类有关,回收TNT中的杂质对热感度的影响较小;回收TNT的撞击感度为8%,摩擦感度为4%,与对比样品相比均下降,表明回收TNT的安全性较好,能满足再利用的要求。     

Coating of Energetic Materials using Crystallization

A sensitive explosive was coated with a less sensitive explosive in order to improve stability while maintaining explosion performance. In this study the sensitive explosive HMX was coated with the less sensitive explosive NTO (3‐nitro‐1, 2, 4‐triazole‐5‐one) by cooling crystallization. The mechanism of coating by crystallization was determined to be an agglomeration and crystal growth phenomenon. The surface morphology and the growth rate of the coating were investigated under various experimental conditions. The surface morphology was predominantly influenced by the solvent type, HMX/NTO ratio, agitation speed, and degree of sub‐cooling. The growth rate of the HMX coating was increased to a certain extent by increasing the concentration ratio of HMX/NTO, but then began to decrease because of high agglomeration. Finally, the optimal conditions to achieve thin and uniform surface coatings on HMX were found experimentally.     

Stabilization of ammonium azide particles through its microencapsulation with some organic coating agents

This work is devoted to reduce spontaneous sublimation of ammonium azide at ambient and elevated temperatures by means of two microencapsulation techniques involving solvent/non-solvent and solvent evaporation methods in which stearic acid, Viton and nitrocellulose (NC) have been tested as coating agents. Scanning electron microscopy (SEM) was employed to examine the coating morphology. The thermal behavior of pure and coated ammonium azide samples have been studied by using simultaneous thermogravimetery-differential thermal analysis (TG-DTA) and differential scanning calorimetry (DSC). The results showed that ammonium azide microparticle could be effectively coated with nitrocellulose through a solvent/non-solvent experiment in which the coating quality depends on some experimental factors such as coating agent to NH₄N₃ weight ratio and volume and addition time of non-solvent. The effect of these factors on coating quality and thermal properties of NH₄N₃ has been revealed by results of SEM and thermal experiments. The most stabilized coated ammonium azide was achieved by using 4.5% (w/w) of NC as stabilizer, and by addition of 30 ml n-hexane as non-solvent within 75 min, where the maximum sublimation temperature increases about 30 °C with respect to uncoated sample and reaches to 145.5 °C. The influence of the heating rate (5, 10, 15 and 20 °C/min) on the DSC behavior of the pure and coated ammonium azide particles at the optimum condition was verified, whereas sublimation temperature of the NH₄N₃ was increased as the heating rate was increased. Also, the kinetic parameters such as the activation energy and frequency factor of the sublimation processes for pure and coated ammonium azide were obtained from the DSC data by non-isothermal methods proposed by Kissinger and Ozawa. The results showed that, activation energy for sublimation of completely coated NH₄N₃ particles is considerably higher than (nearly 1.5 times) that of the pure one. Also, the first order rate constant of sublimation of completely coated sample is noticeably lower than that of pure sample (). The kinetic results led us to conclude that the applied microencapsulation technique caused efficient stabilization of volatile NH₄N_3.     

TATB/HMX共晶炸药的制备及性能研究

采用溶剂/非溶剂法,在超声辅助的情况下,制备了TATB/HMX共晶炸药;探究了TATB/HMX共晶技术的影响因素;计算了TATB/HMX共晶炸药的理论密度和理论爆速;采用扫描电子显微镜(SEM)、X射线衍射仪(XRD)和差示扫描热量法(DSC)对其进行表征和热分析,并测试了其撞击感度。结果表明,制备TATB/HMX共晶的最佳工艺条件为:以[Emim]Ac/DMSO为复合溶剂,TATB和HMX投料比(摩尔比)为3∶7,温度为80℃,搅拌速率为500r/min;与原料相比,TATB/HMX共晶分子在结构上发生改变;TATB/HMX共晶炸药颗粒大小约为2μm,形貌为六边形晶体;共晶炸药的热安定性优于原料HMX,其特性落高比原料HMX高74cm,撞击感度明显降低;理论密度为1.891g/cm~3,理论爆速为8.758km/s,表明其爆炸性能良好。     

Stabilizing of magnesium powder by microencapsulation with azidodeoxy cellulose nitrate

Surface of magnesium particles is highly reactive and may be oxidized easily during storage at ambient conditions. Coating the surface of metal particles with a layer of polymer could be a simple and efficient way to prevent oxidation. In this study, Taguchi robust design was employed as a statistical experiment design for coating of magnesium powder with azidodeoxy cellulose nitrate via solvent/non-solvent technique. FT-IR spectroscopy and scanning electron microscopy techniques were used to evaluate the surface morphology of coated particles. The effect of azidodeoxy cellulose nitrate coating on magnesium powder thermal stability has been investigated by means of thermogravimetry (TG) coupled with differential scanning calorimetry (DSC). The effects of procedure parameters, i.e., type of solvent, percent of polymer as the stabilizer, flow rate of non-solvent addition, and added non-solvent volume in the coating quality and thermal properties of magnesium powder have been studied by thermal analysis methods. Analysis of variance (ANOVA) was employed to evaluate quantitatively the effect of these parameters on thermal stability of coated magnesium particles. Thermal data showed that magnesium powder could be stabilized considerably by controlling coating process parameters including the percent of the stabilizer, flow rate of non-solvent addition, and type of solvent. Based on the ANOVA results, using of 3% stabilizer, 1 ml/min as non-solvent flow rate, and DMF as the solvent are optimum conditions for coating of magnesium particles with azidodeoxy cellulose nitrate leads to producing coated particles with higher thermal stability (567 °C); whereas, TG/DSC analysis results revealed that the main thermal oxidation of the pure magnesium powder starts at lower temperature ranges of 260 °C.     

混凝剂PFS处理焦化废水的研究

采用混凝剂PFS对焦化废水进行处理.分析了混凝剂PFS、助凝剂PAM、初始pH值、搅拌时间、温度等因素对COD、浊度、色度的影响.研究表明,较佳的工艺条件:混凝剂PFS为350mg/L,助凝剂PAM为18mg/L,初始pH值为8,加入PAM后的搅拌时间为8min,温度为40℃,处理后的出水COD去除率达到46％以上.