全氟磺酸MCM-41分子筛催化合成CL-20  

Synthesis of CL-20 by MCM-41 Molecular Sieve of Perfluorosulfonic Acid

作　　者：石磊[1] 杨超飞 钱华[1,2] 任丽萍 刘大斌 潘仁明[1] SHI Lei;YANG Chao-fei;QIAN Hua;REN Li-ping;LIU Da-bin;PAN Ren-ming(School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China;National Supervision and Inspection Center for Industrial Explosive Materials, Nanjing 210094, China;China Ordnance Industrial Standardization Research Institute, Beijing 100086, China)

机构地区：[1]南京理工大学化工学院,江苏南京210094 [2]国家民用爆破器材质量监督检验中心,江苏南京210094 [3]中国兵器标准化研究所,北京100089

出　　处：《含能材料》2017年第12期1037-1041,共5页Chinese Journal of Energetic Materials

基　　金：国家自然科学基金(21406116);"南京理工大学卓越计划‘紫金之星’"专项基金

摘　　要：为解决N_2O_5/HNO_3硝化四乙酰基六氮杂异伍兹烷(TAIW)合成六硝基六氮杂异伍兹烷(CL-20)收率低以及催化剂难回收的问题,将全氟(1-甲基-乙烷)磺酸接枝到纯硅MCM-41介孔分子筛上,制备全氟磺酸MCM-41分子筛催化剂(SA-MCM-41),并用于N_2O_5/HNO_3硝化TAIW合成CL-20的反应。结果表明,负载了全氟磺酸的MCM-41仍具有MCM-41的典型晶体结构,平均孔径3.13nm,比表面积887.25m^2·g^(-1)。当催化剂用量0.5g,反应温度65~75℃,时间5h时,CL-20收率93.9%,纯度98.4%。该催化剂稳定性好,易与体系分离,重复使用5次,催化性能无明显降低。In order to improve the low yield of CL-20and solve the difficult recovery of the catalyst,perfluorinated(1-methyl-ethane)sulfonic acid was grafted onto pure MCM-41mesoporous molecular sieves to prepare the catalyst of perfluorosulfonic acid MCM-41molecular sieve(SA-MCM-41).The catalyst was applied in the nitration of TAIW to CL-20using N2O5/HNO3.Results show that the catalyst has the typical crystal structure of MCM-41with average pore size of3.13nm and specific surface area of887.25m2·g-1.The optimal reaction condition is catalyst0.5g,reaction temperature65-75℃and reaction time5h with the highest yield and purity of93.9%and98.4%,respectively.The catalyst possesses good stability and is easy to separate from the product.Additionally,it can be reused for five times without any significant loss of catalytic activity under the describe reaction conditions.

关 键 词：六硝基六氮杂异伍兹烷(CL-20) 四乙酰基六氮杂异伍兹烷(TAIW) 分子筛 全氟磺酸 

分 类 号：TQ560.7[化学工程—炸药化工]