硝胺炸药的表面包覆及其对推进剂性能的影响研究
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摘要
新型高能固体推进剂中含有大量的硝胺炸药,使得推进剂的机械感度升高、力学和工艺性能变差,这严重制约了这些新型高能推进剂的应用。国内外一些研究表明,采用合适的包覆材料对硝胺炸药进行表面包覆可以改善推进剂安全和力学性能,然而,推进剂的能量性能却会由于这些惰性包覆材料的加入而降低。此外,包覆材料的加入也改变了推进剂的配方组成,对推进剂的相容性、贮运性能和使用性能都产生了不良影响。为消除这种由包覆材料带来的负面影响,本论文以推进剂中组分为包覆材料对硝胺炸药进行了表面包覆,制备了硝胺炸药包覆颗粒,并将其应用到推进剂中。重点考察了表面包覆对硝胺炸药及其推进剂机械感度和热安定性的影响。另外,对采用包覆炸药制成的推进剂的抗拉强度、延伸率和工艺性能也进行了相应地研究。本研究对钝感推进剂的研制及防止硝胺炸药在推进剂中的“脱湿”都具有十分积极的意义。本论文的主要内容如下:
首先,以硝化棉(NC)和中定剂(C-1)为复合包覆剂,采用相分离法和水悬浮—乳液—蒸馏法两种方法对硝胺炸药进行了表面包覆,得出了最佳包覆工艺条件。研究发现两种包覆方法均能使黑索金(RDX)和奥克托金(HMX)的机械感度降低,但水悬浮—乳液—蒸馏法由于具有更加致密的包覆效果,其包覆样品感度降低幅度更大,且该工艺简便、安全。将水悬浮—乳液—蒸馏法制备的RDX包覆颗粒应用到硝胺改性双基推进剂(CMDB)中后,推进剂的安全、力学及工艺等性能较用原料RDX制成的推进剂都得到了一定程度的改善。
其次,以三硝基甲苯(TNT)和一种含能聚合物(HP-1)为复合包覆剂,采用溶剂—非溶剂与水悬浮—熔融相结合的方法对RDX和HMX进行了表面包覆。研究发现,若无HP-1的加入,TNT在硝胺炸药表面的包覆模式为“岛状包覆”,而用TNT/HP-1复合包覆样品的包覆模式转变为“膜状包覆”。这是因为HP-1的加入降低了包覆材料的表面张力,提高了液态包覆材料对炸药颗粒的润湿能力。经表面包覆后,硝胺炸药的撞击和摩擦感度都得到显著降低,热安定性和爆热都没有明显变化。将包覆前后的RDX样品应用到推进剂中后发现,对于表面包覆有2.5%TNT和0.5%HP-1的RDX所制成的推进剂,其撞击和摩擦感度较由原料RDX制成的推进剂有一定程度的降低,且推进剂的延伸率大幅升高、制备时的压延次数明显减少。
第三,以燃烧催化剂(硬脂酸铅和邻苯二甲酸铅)为包覆剂,采用化学沉淀法对硝胺炸药进行了表面包覆。研究发现,硬脂酸铅对硝胺炸药有明显的钝感作用,包覆处理后RDX和HMX的机械感度都大幅度降低。而邻苯二甲酸铅对硝胺炸药没有起到钝感作用,其包覆样品的机械感度不降反升。但如果在邻苯二甲酸铅/硝胺炸药复合粒子表面继续包覆一层聚合物后,其机械感度将得到一定程度的降低。燃烧催化剂的加入方式对推进剂的热分解性能有一定的影响,将硬脂酸铅或邻苯二甲酸铅包覆在硝胺炸药表面可提高其对推进剂组分的催化活性,表现为硝化棉/硝化甘油的热分解峰提前,样品总放热量增加。与直接加入硬脂酸铅的推进剂相比,由硬脂酸铅/RDX包覆粒子制成的推进剂的机械感度、力学性能和能量性能都没有明显变化。
最后,以端羟基聚丁二烯(HTPB)及其助剂为包覆剂,分别采用一步相分离法、两步相分离法和双层包覆技术对硝胺炸药进行了表面包覆。一步相分离法制得样品的性能测试结果表明,尽管包覆后硝胺炸药的机械感度得到明显降低,但样品在进行HTPB的固化工序时极易发生粘连,导致包覆样品流散性差,严重影响了样品的使用性能。为解决该问题,试用两步相分离法对硝胺炸药进行包覆,这种包覆方法能够较有效地防止由HTPB固化产生的粘连,但其缺点为溶剂用量过大、包覆制备效率低。最终,采用双层包覆技术,先后以HTPB/IPDI(异佛尔酮二异氰酸酯)和TNT为包覆剂对RDX进行了表面包覆,成功的制备了外包覆层为TNT,内包覆层为HTPB/IPDI的双层包覆颗粒。外层的TNT有效地阻止了HTPB/IPDI层在固化过程中的相互粘接。当除去TNT后,即得到了分散性良好的固化HTPB包覆RDX复合粉末。这种包覆样品的机械感度较原料RDX有显著降低,特性落高(H_(50))升高了约79%,摩擦爆炸概率(P)降低了约76%。由该包覆颗粒制成的HTPB推进剂浆料和成品的机械感度都比由原料RDX制成的推进剂有明显降低,且推进剂的抗拉强度也得到了显著改善。此外,由于两个推进剂的组份含量完全相同,由包覆RDX制成推进剂的能量性能也没有降低。
Although adding nitroamine explosives can increase the energy of solid propellants, but they also can worsen the safety, the mechanical performances and the processing properties of the propellants, which greatly restricts the application of high energy (HE) propellants. Some researches show that the safety and mechanical performances of propellants can be improved by surface-coating on the nitroamine explosives fillers. However, the energy properties of propellant decrease due to the addition of inert coating materials. Moreover, the formulation composition of propellants can be changed, thus the compatibility, storage transportation properties and service performances of propellants can also be affected by the addition of such coating materials. In order to eliminate the negative effects mentioned above, the ingredients of propellants are selected to coat the nitroamine explosives and the coated explosives are applied into propellants in this paper. The influence of surface coating on mechanical sensitivity and thermal stability of nitroamine explosive are studied. Moreover, the influence of coating of nitroamine explosives on mechanical sensitivity, thermal stability, tensile strength, percentage elongation and processing properties of propellants are also investigated. The research is of great and positive significance to exploit insensitive propellants and prevention of "dewetting" of nitroamine explosives. The details are described as follows:
Firstly, NC (nitrocellulose) and centralite-1 (C-1) are selected to coat niroamine explosives together by phase separation and slurry-emulsion-distillation methods respectively, and the optimum technology conditions are obtained. The mechanical sensitivity of the coated samples prepared by the two methods both decreased. However, the insensitive effect of the sample prepared by slurry-emulsion-distillation is more evident than that prepared by phase separation, due to the denser coating layer. In addition, such coating method has the advantages of facility and safety. Concretely, when [NC+C-1]/RDX composite prepared by slurry-emulsion-distillation is filled in the CMDB propellant as the solid fillers, the safety, mechanical performances and processing technology of propellant are all improved.
Secondly, TNT (2,4,6-trinitrotoluene) and an energetic material (HP-1) are used to coat RDX and HMX (octogen) by means of combining solvent-nonsolvent and aqueous suspension-melting. The research shows that unlike the coating mode of the sample coated with only TNT which belongs to "island coating", the mode of the sample coated with TNT/HP-1 changes to "film coating", in which the TNT/HP-1 capped the surface of RDX tightly. It is attributed to the decrease of surface tension of melted TNT owing to the introducing of HP-1. After coating, the impact and friction sensitivities of RDX decrease obviously, and the thermal stability and of the explosion heat do not vary obviously. In terms of the propellant made with RDX samples coated with 2.5% TNT and 0.5% HP-1, both impact and friction sensitivities are lower than that made with raw RDX. Moreover, the percentage elongation increases and the calendering times decrease distinctly.
Thirdly, the burning catalysts (lead stearate and lead phthalate) of CMDB propellant are used to coat RDX and HMX by chemical precipitation. The insensitive effect of lead stearate on nitroamine explosive is in evidence. By surface coating with lead stearate, the mechanical sensitivity of RDX and HMX both decrease significantly. However, lead phthalate is no insensitive action on nitroamine explosives. The mechanical sensitivity of HMX coated with lead phthalate does not decrease but increase. The thermal decomposition properties of propellants are affected by methods of which way the burning catalysts added into. If the lead stearate and lead phthalate loaded upon the surface of explosive particles are filled into propellants, their catalytic activity are superior beyond the active of catalysts simple mixed in propellants, such as the decreasing of thermal decomposition peak temperatures of NC/NG and the increasing of the thermal decomposition heat. The mechanical sensitivity, mechanical performances and energy properties of propellants do not vary obviously, in despite of which way to add the catalysts into the propellant.
Finally, HTPB (hydroxyl terminated polybutadiene) and its corresponding additives are used to coat nitroamine explosives by one-step phase separation (OSPS), two-step phase separation (TSPS) or double layer coating technology (DLCT), respectively. The performance testing results of samples prepared by OSPS show that the mechanical sensitivity of coated samples reduces greatly. However, lots of severe agglomerations formed during the curing process of HTPB, and the negative result limits its application. To improve the dispersibility of coated samples, TSPS is employed to coat the nitroamine explosive. Such method can effectively prevent the conglutination among the HTPB that attached on the surface of explosive particles. However, there are still some disadvantages in the process, such as high solvent dissipation, low preparation efficiency. As a result, HTPB/IPDI (Isophorone diisocyanate) and TNT are successively coated on RDX (hexogen) particles by DLCT. While HTPB coated on RDX particles cured completely and TNT is removed by solvent dissolution, the well-dispersed RDX particles coated with cured HTPB are obtained successfully. As the outer layer, TNT effectively hinders the adhesion among the inner layer of HTPB. The mechanical sensitivities of RDX decreased significantly by such surface coating. When the covering amount of HTPB is 2wt.%, drop height (H_(50)) of RDX increases by 79% and explosion probability (P) decreases by 76%. Compared with that containing uncoated RDX, the mechanical sensitivities of propellant slurry and products containing coated RDX samples decrease obviously, and the tensile strength also improves obviously. In addition, the energy properties of propellants do not decrease because the propellants filled with HTPB/RDX has the same formulation with the propellant filled with raw RDX.
首先,以硝化棉(NC)和中定剂(C-1)为复合包覆剂,采用相分离法和水悬浮—乳液—蒸馏法两种方法对硝胺炸药进行了表面包覆,得出了最佳包覆工艺条件。研究发现两种包覆方法均能使黑索金(RDX)和奥克托金(HMX)的机械感度降低,但水悬浮—乳液—蒸馏法由于具有更加致密的包覆效果,其包覆样品感度降低幅度更大,且该工艺简便、安全。将水悬浮—乳液—蒸馏法制备的RDX包覆颗粒应用到硝胺改性双基推进剂(CMDB)中后,推进剂的安全、力学及工艺等性能较用原料RDX制成的推进剂都得到了一定程度的改善。
其次,以三硝基甲苯(TNT)和一种含能聚合物(HP-1)为复合包覆剂,采用溶剂—非溶剂与水悬浮—熔融相结合的方法对RDX和HMX进行了表面包覆。研究发现,若无HP-1的加入,TNT在硝胺炸药表面的包覆模式为“岛状包覆”,而用TNT/HP-1复合包覆样品的包覆模式转变为“膜状包覆”。这是因为HP-1的加入降低了包覆材料的表面张力,提高了液态包覆材料对炸药颗粒的润湿能力。经表面包覆后,硝胺炸药的撞击和摩擦感度都得到显著降低,热安定性和爆热都没有明显变化。将包覆前后的RDX样品应用到推进剂中后发现,对于表面包覆有2.5%TNT和0.5%HP-1的RDX所制成的推进剂,其撞击和摩擦感度较由原料RDX制成的推进剂有一定程度的降低,且推进剂的延伸率大幅升高、制备时的压延次数明显减少。
第三,以燃烧催化剂(硬脂酸铅和邻苯二甲酸铅)为包覆剂,采用化学沉淀法对硝胺炸药进行了表面包覆。研究发现,硬脂酸铅对硝胺炸药有明显的钝感作用,包覆处理后RDX和HMX的机械感度都大幅度降低。而邻苯二甲酸铅对硝胺炸药没有起到钝感作用,其包覆样品的机械感度不降反升。但如果在邻苯二甲酸铅/硝胺炸药复合粒子表面继续包覆一层聚合物后,其机械感度将得到一定程度的降低。燃烧催化剂的加入方式对推进剂的热分解性能有一定的影响,将硬脂酸铅或邻苯二甲酸铅包覆在硝胺炸药表面可提高其对推进剂组分的催化活性,表现为硝化棉/硝化甘油的热分解峰提前,样品总放热量增加。与直接加入硬脂酸铅的推进剂相比,由硬脂酸铅/RDX包覆粒子制成的推进剂的机械感度、力学性能和能量性能都没有明显变化。
最后,以端羟基聚丁二烯(HTPB)及其助剂为包覆剂,分别采用一步相分离法、两步相分离法和双层包覆技术对硝胺炸药进行了表面包覆。一步相分离法制得样品的性能测试结果表明,尽管包覆后硝胺炸药的机械感度得到明显降低,但样品在进行HTPB的固化工序时极易发生粘连,导致包覆样品流散性差,严重影响了样品的使用性能。为解决该问题,试用两步相分离法对硝胺炸药进行包覆,这种包覆方法能够较有效地防止由HTPB固化产生的粘连,但其缺点为溶剂用量过大、包覆制备效率低。最终,采用双层包覆技术,先后以HTPB/IPDI(异佛尔酮二异氰酸酯)和TNT为包覆剂对RDX进行了表面包覆,成功的制备了外包覆层为TNT,内包覆层为HTPB/IPDI的双层包覆颗粒。外层的TNT有效地阻止了HTPB/IPDI层在固化过程中的相互粘接。当除去TNT后,即得到了分散性良好的固化HTPB包覆RDX复合粉末。这种包覆样品的机械感度较原料RDX有显著降低,特性落高(H_(50))升高了约79%,摩擦爆炸概率(P)降低了约76%。由该包覆颗粒制成的HTPB推进剂浆料和成品的机械感度都比由原料RDX制成的推进剂有明显降低,且推进剂的抗拉强度也得到了显著改善。此外,由于两个推进剂的组份含量完全相同,由包覆RDX制成推进剂的能量性能也没有降低。
Although adding nitroamine explosives can increase the energy of solid propellants, but they also can worsen the safety, the mechanical performances and the processing properties of the propellants, which greatly restricts the application of high energy (HE) propellants. Some researches show that the safety and mechanical performances of propellants can be improved by surface-coating on the nitroamine explosives fillers. However, the energy properties of propellant decrease due to the addition of inert coating materials. Moreover, the formulation composition of propellants can be changed, thus the compatibility, storage transportation properties and service performances of propellants can also be affected by the addition of such coating materials. In order to eliminate the negative effects mentioned above, the ingredients of propellants are selected to coat the nitroamine explosives and the coated explosives are applied into propellants in this paper. The influence of surface coating on mechanical sensitivity and thermal stability of nitroamine explosive are studied. Moreover, the influence of coating of nitroamine explosives on mechanical sensitivity, thermal stability, tensile strength, percentage elongation and processing properties of propellants are also investigated. The research is of great and positive significance to exploit insensitive propellants and prevention of "dewetting" of nitroamine explosives. The details are described as follows:
Firstly, NC (nitrocellulose) and centralite-1 (C-1) are selected to coat niroamine explosives together by phase separation and slurry-emulsion-distillation methods respectively, and the optimum technology conditions are obtained. The mechanical sensitivity of the coated samples prepared by the two methods both decreased. However, the insensitive effect of the sample prepared by slurry-emulsion-distillation is more evident than that prepared by phase separation, due to the denser coating layer. In addition, such coating method has the advantages of facility and safety. Concretely, when [NC+C-1]/RDX composite prepared by slurry-emulsion-distillation is filled in the CMDB propellant as the solid fillers, the safety, mechanical performances and processing technology of propellant are all improved.
Secondly, TNT (2,4,6-trinitrotoluene) and an energetic material (HP-1) are used to coat RDX and HMX (octogen) by means of combining solvent-nonsolvent and aqueous suspension-melting. The research shows that unlike the coating mode of the sample coated with only TNT which belongs to "island coating", the mode of the sample coated with TNT/HP-1 changes to "film coating", in which the TNT/HP-1 capped the surface of RDX tightly. It is attributed to the decrease of surface tension of melted TNT owing to the introducing of HP-1. After coating, the impact and friction sensitivities of RDX decrease obviously, and the thermal stability and of the explosion heat do not vary obviously. In terms of the propellant made with RDX samples coated with 2.5% TNT and 0.5% HP-1, both impact and friction sensitivities are lower than that made with raw RDX. Moreover, the percentage elongation increases and the calendering times decrease distinctly.
Thirdly, the burning catalysts (lead stearate and lead phthalate) of CMDB propellant are used to coat RDX and HMX by chemical precipitation. The insensitive effect of lead stearate on nitroamine explosive is in evidence. By surface coating with lead stearate, the mechanical sensitivity of RDX and HMX both decrease significantly. However, lead phthalate is no insensitive action on nitroamine explosives. The mechanical sensitivity of HMX coated with lead phthalate does not decrease but increase. The thermal decomposition properties of propellants are affected by methods of which way the burning catalysts added into. If the lead stearate and lead phthalate loaded upon the surface of explosive particles are filled into propellants, their catalytic activity are superior beyond the active of catalysts simple mixed in propellants, such as the decreasing of thermal decomposition peak temperatures of NC/NG and the increasing of the thermal decomposition heat. The mechanical sensitivity, mechanical performances and energy properties of propellants do not vary obviously, in despite of which way to add the catalysts into the propellant.
Finally, HTPB (hydroxyl terminated polybutadiene) and its corresponding additives are used to coat nitroamine explosives by one-step phase separation (OSPS), two-step phase separation (TSPS) or double layer coating technology (DLCT), respectively. The performance testing results of samples prepared by OSPS show that the mechanical sensitivity of coated samples reduces greatly. However, lots of severe agglomerations formed during the curing process of HTPB, and the negative result limits its application. To improve the dispersibility of coated samples, TSPS is employed to coat the nitroamine explosive. Such method can effectively prevent the conglutination among the HTPB that attached on the surface of explosive particles. However, there are still some disadvantages in the process, such as high solvent dissipation, low preparation efficiency. As a result, HTPB/IPDI (Isophorone diisocyanate) and TNT are successively coated on RDX (hexogen) particles by DLCT. While HTPB coated on RDX particles cured completely and TNT is removed by solvent dissolution, the well-dispersed RDX particles coated with cured HTPB are obtained successfully. As the outer layer, TNT effectively hinders the adhesion among the inner layer of HTPB. The mechanical sensitivities of RDX decreased significantly by such surface coating. When the covering amount of HTPB is 2wt.%, drop height (H_(50)) of RDX increases by 79% and explosion probability (P) decreases by 76%. Compared with that containing uncoated RDX, the mechanical sensitivities of propellant slurry and products containing coated RDX samples decrease obviously, and the tensile strength also improves obviously. In addition, the energy properties of propellants do not decrease because the propellants filled with HTPB/RDX has the same formulation with the propellant filled with raw RDX.
引文
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