CN111072708B - 一种石墨烯-席夫碱金属配合物及其制备方法 - Google Patents
一种石墨烯-席夫碱金属配合物及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种石墨烯‑席夫碱金属配合物，其结构式如I所示，M代表催化活性金属铜、钴或镁。其合成过程包括以下步骤：(1)N‑氨乙基‑γ‑氨丙基三甲氧基硅烷改性氧化石墨烯合成氨基化石墨烯；(2)氨基化石墨烯与水杨醛反应合成石墨烯‑席夫碱配合物；(3)石墨烯‑席夫碱配合物分别与硝酸铜、硝酸钴和硝酸镁水溶液反应合成石墨烯‑席夫碱金属配合物。本方法所合成的石墨烯‑席夫碱金属配合物可有效提升含奥克托今(HMX)的改性双基推进剂的燃速，是改性双基推进剂的有效燃烧催化剂。
Description
技术领域
本发明涉及石墨烯-席夫碱金属配合物及其合成方法，该配合物可有效提升改性双基推进剂的燃速，可作为固体推进剂的燃烧催化剂使用。
背景技术
固体推进剂在战术导弹和火箭中具有广泛的应用，其综合性能直接关系到现代武器装备系统的精确打击、高能毁伤及生存能力。通过添加奥克托今(HMX)、黑索今(RDX)和六硝基六氮杂异伍兹烷(CL-20)可有效提升推进剂的能量特性，满足现代战术导弹、火箭武器要求远射程与快速突防的需求。
而固含量的提高会造成改性双基推进剂燃速的降低，通过使用铅-铜-碳复配催化体系可在一定范围内提升改性双基推进剂的燃速，降低压力指数，但仍难以满足现代武器装备系统对于改性双基推进剂高燃速的需求。在铅-铜-碳复配催化体系的基础上外加席夫碱金属配合物可有效提升固体推进剂的燃速，但会造成固体推进剂压力指数提高，难以满足现代武器装备系统对于改性双基推进剂高燃速、低压力指数和宽平台的应用需求。石墨烯等碳材料作为改双配方中有效的燃烧催化剂，与其结合不仅可提升催化活性金属及金属氧化物的分散性，获得更多的催化活性位点，还可赋予推进剂更多的功效性能。
鉴于此，本发明设计、合成了石墨烯-席夫碱铜、钴和镁配合物，结合席夫碱金属配合物和石墨烯载体的优异性能，有效促进催化活性金属及金属氧化物的分散，提供更多的催化活性位点以满足改性双基推进剂的发展需要。
发明内容
为了解决现有催化体系的不足和缺陷，本发明提供石墨烯-席夫碱金属配合物及其合成方法。
本发明的石墨烯-席夫碱金属配合物的结构式如I所示：
本发明的石墨烯-席夫碱金属配合物的合成路线：
为实现上述目的，本发明提供的石墨烯-席夫碱金属配合物的合成方法包括以下步骤：
(1)氨基化石墨烯的合成：
将分散好的氧化石墨烯乙醇分散液置于三颈烧瓶中，滴加适量N-氨乙基-γ-氨丙基三甲氧基硅烷乙醇溶液，于78～85℃反应1～3h，反应结束后冷却至室温，离心收集并用乙醇洗涤得到氨基化石墨烯。其中，N-氨乙基-γ-氨丙基三甲氧基硅烷与氧化石墨烯质量比为10～15:1。
(2)石墨烯-席夫碱配合物的合成：
将步骤(1)合成的氨基化石墨烯乙醇分散液置于三颈烧瓶中，滴加适量水杨醛乙醇溶液，于78～85℃反应2～5h，反应结束后冷却至室温，离心收集并用乙醇洗涤得到石墨烯-席夫碱配合物。其中，水杨醛与氨基化石墨烯质量比为5～10:1。
(3)石墨烯-席夫碱金属配合物的合成
将步骤(2)合成的石墨烯-席夫碱配合物分散于无水乙醇中，与配置好的硝酸铜、硝酸钴或硝酸镁水溶液混合，于55～65℃下反应2～12h，反应结束后冷却至室温，离心收集并用乙醇洗涤得到石墨烯-席夫碱金属配合物。其中，石墨烯-席夫碱配合物与金属硝酸盐的质量比为0.5～1:1，乙醇与水的体积比为2～5:1。
本发明的优点与积极效果：
本发明的石墨烯-席夫碱金属配合物实现了催化活性物质石墨烯、席夫碱配体和活性金属在分子水平上的组装，相较于负载型石墨烯-金属配合物，石墨烯-席夫碱金属配合物可在催化过程中原位生成氧化物等催化活性物质，避免了直接负载金属氧化物易于团聚及与载体间结合力较差等问题，具有更佳的催化效果。
附图说明
图1石墨烯-席夫碱金属配合物的SEM图谱。
图2改性双基推进剂中添加本发明一种石墨烯-席夫碱金属配合物后的燃速-压力曲线。
具体实施方式
形貌采用美国Quantachrome公司的Quanta600型扫描电子显微镜表征。
石墨烯-席夫碱金属配合物的合成
(1)氨基化石墨烯的合成：
将分散好的氧化石墨烯乙醇分散液置于三颈烧瓶中，滴加适量N-氨乙基-γ-氨丙基三甲氧基硅烷乙醇溶液，于78℃反应2h，反应结束后冷却至室温，离心收集并用乙醇洗涤得到氨基化石墨烯。其中，N-氨乙基-γ-氨丙基三甲氧基硅烷与氧化石墨烯质量比为15。
(2)石墨烯-席夫碱配合物的合成：
将步骤(1)合成的氨基化石墨烯乙醇分散液置于三颈烧瓶中，滴加适量水杨醛乙醇溶液，于78℃反应3h，反应结束后冷却至室温，离心收集并用乙醇洗涤得到石墨烯-席夫碱配合物。其中，水杨醛与氨基化石墨烯质量比为10。
(3)石墨烯-席夫碱金属配合物的合成
将步骤(2)合成的石墨烯-席夫碱配合物分散于无水乙醇中，与配置好的硝酸铜、硝酸钴或硝酸镁水溶液混合，于65℃下反应8h，反应结束后冷却至室温，离心收集并用乙醇洗涤得到石墨烯-席夫碱金属配合物。其中，石墨烯-席夫碱配合物与金属硝酸盐的质量比为0.5，乙醇与水的体积比为2。
石墨烯-席夫碱金属配合物的表征
(1)扫描电镜：
制备的石墨烯-席夫碱铜、钴和镁配合物的扫描电镜图如图1(a)、(b)和(c)所示，石墨烯-席夫碱金属配合物保留了石墨烯较好的少层结构，表面结合有席夫碱配体，配位的金属元素作为活性位点具有较好的分散性。
石墨烯-席夫碱金属配合物的应用
实验中采用改性双基推进剂样品的基础配方为：双基黏合剂(NC+NG)63.4％，奥克托今(HMX)26％，功能助剂10.6％。药料按500g配料。催化剂为外加量，Pb-Cu-C复配催化剂为3.9％，石墨烯-席夫碱金属配合物为0.5％，对照组为含3.9％Pb-Cu-C催化体系的配方。
固体推进剂样品采用吸收-驱水-放熟-切成药条的常规无溶剂压伸成型工艺制备。试样的燃速采用靶线法测得。将已处理过的Φ5mm×150mm小药柱侧面用聚乙烯醇溶液包覆6次并晾干，然后在充氮缓动式燃速仪中进行燃速测试。实验温度为20℃，压强范围2～20MPa。
含石墨烯-席夫碱金属配合物的燃速和压力指数如表1和图2所示。其中u为燃速，p为压力，a为3.9％Pb-Cu-C催化体系的配方，b、c和d是在a基础上添加0.5％石墨烯-席夫碱铜、石墨烯-席夫碱钴和石墨烯-席夫碱镁配合物的改性双基推进剂配方。可以看出，本发明中的石墨烯-席夫碱镁配合物对改性双基推进剂的燃速具有较好的提升作用，石墨烯-席夫碱钴对压力指数具有较好的降低作用，在10～20MPa压强范围内n＝0.20。
表1含石墨烯-席夫碱金属配合物的燃速和压力指数
Claims (2)
1.一种石墨烯-席夫碱金属配合物，其特征在于，其结构式如I所示：
式中M＝Cu、Co或Mg。
2.如权利要求1所述的石墨烯-席夫碱金属配合物的合成方法，其特征在于，包括以下步骤：
(1)氨基化石墨烯的合成：
将分散好的氧化石墨烯乙醇分散液置于三颈烧瓶中，滴加适量N-氨乙基-γ-氨丙基三甲氧基硅烷乙醇溶液，于78～85℃反应1～3h，反应结束后冷却至室温，离心收集并用乙醇洗涤得到氨基化石墨烯；其中，N-氨乙基-γ-氨丙基三甲氧基硅烷与氧化石墨烯质量比为10～15:1；
(2)石墨烯-席夫碱配合物的合成：
将步骤(1)合成的氨基化石墨烯乙醇分散液置于三颈烧瓶中，滴加适量水杨醛乙醇溶液，于78～85℃反应2～5h，反应结束后冷却至室温，离心收集并用乙醇洗涤得到石墨烯-席夫碱配合物；其中，水杨醛与氨基化石墨烯质量比为5～10:1；
(3)石墨烯-席夫碱金属配合物的合成
将步骤(2)合成的石墨烯-席夫碱配合物分散于无水乙醇中，与配置好的硝酸铜、硝酸钴或硝酸镁水溶液混合，于55～65℃下反应2～12h，反应结束后冷却至室温，离心收集并用乙醇洗涤得到石墨烯-席夫碱金属配合物；其中，石墨烯-席夫碱配合物与金属硝酸盐的质量比为0.5～1:1，所述的金属为铜、钴或镁；乙醇与水的体积比为2～5:1。
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