摘要
针对工业混酸法制备六硝基六氮杂异伍兹烷(CL-20)废酸污染大及N2O5/HNO3法收率低的现状,制备了酸性季铵盐类、己内酰胺类、咪唑类、吡啶类离子液体,将其用于N2O5/HNO3硝解四乙酰基六氮杂异伍兹烷(TAIW)制备CL-20的反应中。考察了离子液体种类、酸度、用量及反应时间对CL-20收率及纯度的影响。结果表明,离子液体酸强度与催化性能呈正相关关系,[Et3N(CH2)4SO3H][BSO]表现出最佳的催化活性。最佳的反应条件为:反应温度60—80℃,反应时间7h,m([Et3N(CH3)4SO3H][BSO]):m(TAIW):m(N205):V(HNO3)=0.5g:3g:4g:15mL,CL-20收率94.5%,纯度98.1%。离子液体重复使用5次,催化性能无明显降低。
New nitrification systems of N205/HNO3/ ionic liquids( ILs, quaternary ammonium salts, caprolactams, imidazoles, pyridines) were used to nitrify tetraacetyl hexaazaisowurtzitane(TAIW) to prepare hexanitro-hexaazaisowurtzitane(CL-20), instead of the commonly used concentrated nitric and sulfuric acid in industrial scale, which was seriously harmful to the environment. The effects of the type, dosage and acidity of ILs and reaction time on yield and purity of CL-20 were investigated. Results show that acidity of ILs is positively correlated with catalytic performance and the [ Et3 N (CH2 )4 SO3 H ][ BSO ] shows the best catalytic activity. The optimum conditions are as follows: reaction temperature 60-80℃, reaction time 7 h, m ( Et3 N ( CH2 ) 4 SO3 H ] [ BSO 1 ]) : m(TAIW) : m(N2O5) : V(HNO3)=0-5 g : 3 g : 4 g : 15 mL, with the yield and purity of 94.5% and98.1%, respectively. ILs can be reused five times and barely with significant loss of catalytic activity.
出处
《含能材料》
EI
CAS
CSCD
北大核心
2016年第6期571-575,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’"
江苏高校优势学科建设工程资助项目