CN114573632B - 无溶剂含能配合物[Pb3(BTT)2]n及其制备方法和应用 - Google Patents
无溶剂含能配合物[Pb3(BTT)2]n及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种化学式为[Pb3(BTT)2]n的无溶剂含能配合物及其制备方法,以4,5‑二四唑基‑1,2,3‑三唑和硝酸铅为原料,通过溶剂热法制备[Pb3(BTT)2]n,该配合物的稳定性不低于329℃,撞击感度不低于40J,摩擦感度不低于216N。受激光辐照后发生爆轰响应,可作为激光起爆药。具有良好的安全性能和爆轰性能,可作为含能催化剂用于推进剂中,也可作为起爆药用于激光起爆,在含能材料领域具有良好的应用前景。
Description
技术领域
本发明的涉及配合物合成领域含能材料的制备,更具体地,本发明涉及无溶剂含能配合物[Pb3(BTT)2]n及其制备方法和应用。
背景技术
含能配合物作为一类具有强烈爆炸性能的配合物,在含能材料领域显示出良好的发展前景,既可作为起爆药用于各类武器弹药中,也可作为含能催化剂应用于推进剂中。激光起爆技术作为一种安可靠的新型起爆技术,可以避免电磁干扰、静电放电以及杂散电流。我国目前使用的起爆药主要以叠氮化铅、苦味酸和DDNP等为主,这些起爆药多数对外界刺激较为敏,容易发生意外,引起爆炸事故和导致人员伤亡。因此需要寻求更为安全的起爆药和起爆方式显得尤为迫切。近年来以配位化合物为主的起爆药通常被用于激光起爆领域。然而在含能配合物的制备过程中,难以避免溶剂分子参与配位。这些配位的溶剂分子在释放过程中不仅会降低配合物的能量,而且在低温区产生压力,导致配合物的稳定性降低,爆热降低。为充分发挥含能配位化合物的长处,避免溶剂分子参与配位,构建综合性能优异的含能配合物,具有重要的军事意义。
发明内容
本发明的目的在于克服起爆药热稳定性差和能量低的缺点,提供一种新型起爆药,在激光辐射后发生爆轰。
为解决上述的技术问题,本发明的实施方式采用以下技术方案:
无溶剂含能配合物[Pb3(BTT)2]n,所述配合物具有式I所示的化学式为:
所述的配合物[Pb3(BTT)2]n是致密的3D框架结构,属于斜方晶系,Pbca空间群。配合物[Pb3(BTT)2]n的晶体密度达3.344g cm-3。
本发明进一步公开了所述无溶剂含能配合物[Pb3(BTT)2]n的制备方法,以4,5-二四唑基-1,2,3-三唑(H3BTT)和硝酸铅为原料,通过溶剂热法合成得到。H3BTT可通过已知的方法制得。
具体为:
称取Pb(NO3)2(3.3~331mg,0.01~1.0mmol)溶于一定量的DMF与H2O混合溶液中(体积比1:4),随后加入H3BTT·H2O(8.9~896mg,0.04~4mmol),室温搅拌10~60min,呈白色悬浮液,将其转移至反应釜中,升温至120~160℃,恒温10~72h,降至室温,获得黄色块状晶体。
本发明得到的含能配合物的热稳定性不低于329℃,撞击感度不低于40J;摩擦感度不低于216N。
选取适合待测晶体置于Bruker D8 Venture型X射线单晶衍射仪进行单晶测试,测试温度为293K。基于含能配合物[Pb3(BTT)2]n的晶体学参数如表1:
表1
本发明获得的无溶剂含能配合物[Pb3(BTT)2]n受激光辐照后发生爆轰响应,具有良好的安全性能和爆轰性能,可作为激光起爆药。含能配合物[Pb3(BTT)2]n对推进剂的主要氧化剂高氯酸铵(AP)具有良好的催化效果,在含能催化剂领域具有良好的应用前景。
附图说明
图1a为本发明实施例产物的最小不对称单元结构图;
图1b为本发明实施例产物的3D框架结构图;
图2a为本发明实施例产物的DSC曲线;
图2b为本发明实施例产物的TG曲线。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。
H3BTT是指4,5-二四唑基-1,2,3-三唑。
制备H3BTT:(1)称取7.0g亚硝酸钠溶于125mL蒸馏水中待用。称取10.8g二氨基马来腈溶于100mL稀盐酸(1mol L-1)中,严格控制温度0~5℃下,缓慢滴加亚硝酸钠溶液(反应放出大量的热),滴加完毕后,低温反应30min,后缓慢升温至20℃继续反应1h。抽滤得橙色滤液,用乙醚萃取,取乙醚相,蒸馏除去乙醚(温度不超过30℃),真空干燥,得亮黄色粉末,产率90%。IR(KBr,cm-1):3258,2839,2263,1554,1478,1382,1250,1228,1185,1131,1090,999,792,627,521,465.(2)称取1.2g 4,5-二氰基-1,2,3-三唑溶于25mL蒸馏水中,随后加入1.3g叠氮化钠和1.6g氯化锌,加热回流反应3h。后自然冷却至室温,加入12.5mL浓盐酸,随后冷却至0℃,抽滤,用水和乙醇洗涤,真空干燥,得淡黄色粉末,产率80%。13C NMR(100MHz,d6-DMSO)δ/ppm:148.1,131.8;IR(KBr,cm-1):3516,3404,3240,3014,2973,2468,1896,1637,1606,1469,1435,1392,1340,1232,1187,1122,1074,1041,1011,989,964,896,838,748,710,673,576,534,484.制备文献:Chem.Eur.J.2016,22,1768-1778.。
配合物[Pb3(BTT)2]n的溶剂热合成,提供以下三组实施例:
(1)称取Pb(NO3)2(3.3mg,0.01mmol)溶于1mL DMF与H2O的混合溶液中(体积比1:4),随后加入H3BTT·H2O(8.9mg,0.04mmol),室温搅拌60min,转速900r·min-1,得白色悬浮液,将其转移至5mL聚四氟乙烯反应釜中,设定5℃·min-1程序升温至120℃,鼓风恒温24h,后5℃·h-1程序降温至室温,获得黄色块状晶体。
(2)称取Pb(NO3)2(33.1mg,0.1mmol)溶于5mL DMF与H2O的混合溶液中(体积比1:4),随后加入H3BTT·H2O(89.6mg,0.4mmol),室温搅拌60min,转速1200r·min-1,得白色悬浮液,将其转移至10mL聚四氟乙烯反应釜中,设定5℃·min-1程序升温至150℃,鼓风恒温24h,后5℃·h-1程序降温至室温,获得黄色块状晶体。
(3)称取Pb(NO3)2(331mg,1mmol)溶于50mL DMF与H2O的混合溶液中(体积比1:4),随后加入H3BTT·H2O(896mg,4mmol),室温搅拌60min,得白色悬浮液,将其转移至100mL聚四氟乙烯反应釜中,设定5℃·min-1程序升温至160℃,鼓风恒温72h,后5℃·h-1程序降温至室温,获得黄色块状晶体。
配合物[Pb3(BTT)2]n的热稳定性分析
为了评价配合物的热稳定性,采用DSC和TG测试对实施例(1)获得的配合物进行了研究,升温速率均为10℃·min-1,气氛为高纯N2。DSC测定样品质量均小于0.1mg(考虑到实验的安全性),TG测定样品量约1.5mg。配合物[Pb3(BTT)2]n具有良好的热稳定性,起始分解温度为329.1℃,放热峰出现在377.8℃。由于其结构中没有溶剂分子,因此没有出现吸热峰。
图1a为本发明实施例产物的最小不对称单元结构图;图1b为本发明实施例产物的3D框架结构图;图2a为本发明实施例产物的DSC曲线;图2b为本发明实施例产物的TG曲线。
以上所述,仅是本申请的几个实施例,并非对本申请做任何形式的限制,虽然本申请以较佳实施例揭示如上,然而并非用以限制本申请,任何熟悉本专业的技术人员,在不脱离本申请技术方案的范围内,利用上述揭示的技术内容做出些许的变动或修饰均等同于等效实施案例,均属于技术方案范围内。
Claims (5)
2.根据权利要求1所述的无溶剂含能配合物[Pb3(BTT)2]n,其特征在于,所述的配合物为致密的3D框架结构,属于斜方晶系,Pbca空间群,结构中无溶剂分子存在。
3.根据权利要求1所述无溶剂含能配合物[Pb3(BTT)2]n的制备方法,其特征在于,以4,5-二四唑基-1,2,3-三唑H3BTT和硝酸铅为原料,通过溶剂热法合成得到。
4.根据权利要求1所述的无溶剂含能配合物[Pb3(BTT)2]n的应用,其特征在于,用于激光起爆药。
5.根据权利要求1所述的无溶剂含能配合物[Pb3(BTT)2]n的应用,其特征在于,用于推进剂。
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