摘要
为除去直接硝解法合成RDX时生产废酸中的不稳定有机副产物,以正庚烷/正己烷为油相溶剂(O)、十二烷基苯磺酸钠(SDBS)/十二烷基硫酸钠(SDS)为表面活性剂(S)、正丁醇/正戊醇为助表面活性剂(C)与水(W)配制成微乳液,对直接硝解法合成RDX结晶但不氧化产生的废酸用微乳液进行萃取,对萃取后的废酸进行高效液相色谱分析,甲醛吸收液用NaOH溶液滴定,考察了不同微乳液配方、微乳液与废酸的体积比、萃取次数、微乳液循环使用等因素对废酸萃取效果的影响。结果表明,O、S、C和W质量比为13∶2∶8∶1时配制的微乳液萃取与循环使用效果最佳,微乳液与废酸体积比为5∶1时萃取一次可除去废酸中约95%的不稳定副产物,可在被萃取物加热分解后循环使用4次,萃取后的废酸在70℃保持稳定。
In order to extract the unstable organic by-products from the waste acid of RDX production by the direct nitrolysis method, micro-emulsions were prepared using n-heptane/n-hexane as oil phase solvent(O), sodium dodecyl benzene sulfonate (SDBS)/ sodium dodecyl sulfate(SDS) as surfactant(S), n-butanol/n-pentanol as cosurfactant(C) and water(W). The waste acid generated after RDX crystallization but not oxidation was extracted with the micro-emulsions. The extracted waste acid was analyzed by high performance liquid chromatography (HPLC). The formaldehyde absorption solution was titrated by NaOH solution. The effects of different micro-emulsion formulations, volume ratio of micro-emulsion to waste acid, extraction times and recycling of micro-emulsion and other factors on the extraction efficiency of waste acid with micro-emulsion were investigated. The results show that the extraction efficiency and recycling of prepared micro-emulsion is the best when the mass ratio of O∶S∶C∶W is 13∶2∶8∶1. When the volume ratio of micro-emulsion to waste acid is 5∶1, about 95% of the unstable by-products in waste acid can be removed at one time. The micro-emulsion can be recycled for 4 times after the extraction being heated and decomposed, and the extracted acid remains stable at 70℃.
作者
齐秀芳
陈李和
唐杰
QI Xiu-fang;CHEN Li-he;TANG Jie(School of National Defense Science and Technology, Southwest University of Science & Technology, Mianyang Sichuan 621010, China)
出处
《火炸药学报》
EI
CAS
CSCD
北大核心
2019年第3期312-318,I0006,共8页
Chinese Journal of Explosives & Propellants
基金
西南科技大学博士研究基金(No.09zx7101)
关键词
应用化学
RDX
废酸
微乳液法
萃取
循环利用
直接硝解法
applied chemistry
RDX
waste acid
micro-emulsion method
extraction
recycling
direct nitrolysis method
作者简介
齐秀芳(1976-),女,博士,从事含能材料研究。E-mail:qf412@sina.com.
