微乳液法处理RDX的生产废酸
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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(0), sodium dodecyl benzene sulfonate(SDBS)/sodium dodecyl sulfate(SDS) as surfactant(S), n-utanol/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 perform ance liquid chro m atography(HPLC). The formaldehyde absorption solution was titrated by N aOH 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 showthat the extraction efficiency and recycling of prepared micro-emulsion is the best when the mass ratio of O:S : C : Wis 13 : 2 : 8 : 1. When the volume ratio of micro-emusion 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℃.
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(0), sodium dodecyl benzene sulfonate(SDBS)/sodium dodecyl sulfate(SDS) as surfactant(S), n-utanol/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 perform ance liquid chro m atography(HPLC). The formaldehyde absorption solution was titrated by N aOH 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 showthat the extraction efficiency and recycling of prepared micro-emulsion is the best when the mass ratio of O:S : C : Wis 13 : 2 : 8 : 1. When the volume ratio of micro-emusion 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℃.
引文
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[3]Cheng Guang-bin,Li Xia,Qi Xiu-fang,et al.Synthesis of cyclonite(R D X)in the presence of ionic liquids[J].Journal of Energetic Materials,2010,28(1):35-44.
[4]齐秀芳.Brnsted酸性离子液体存在下的硝化(解)反应研究[D].南京:南京理工大学,2008.Q I Xiu-fang.Study on nitration(nitrolysis)in the presence of Br?nsted acidic ionic liquids[D].N anjing:N anjing U niversity of Science and Technology,2008.
[5]冯远.微乳液的应用研究进展[J].中国清洁工业,2016(6):50-56.FEN G Yuan.Progress in application of microemulsion[J].China Cleaning Industry,2016(6):50-56.
[6]路文娟.微乳液及离子液体萃取金和汞的研究[D].济南:山东大学,2013.LU Wen-juan.Extraction of gold(III)and mercury(II)by microemulsion and ionic liquids[D].Jinan:Shandong U niversity,2013.
[7]杨文玉.微乳液膜法处理含高浓度醋酸废水的研究[D].青岛:青岛科技大学,2010.YAN G Wen-yu.Treatment of high acetic acid containing wastewater with microemulsion liquid membrane[D].Q ingdao:Q ingdao U niversity of Science&Technology,2010.
[8]周富荣,杜金萍,万昆.微乳液膜连续处理焦化厂含酚废水的试验研究[J].工业水处理,2007,27(3):49-52.Z HO U Fu-rong,D U Jin-ping,WAN Kun.Study on continuous treatment of phenol-bearing wastewater from coking plant by microemulsion membrane[J].Industrial Water Treatment,2007,27(3):49-52.
[9]毛雪彬,杜志平,台秀梅,等.微乳液的理论及应用研究进展[J].日用化学工业,2016,46(11):648-653,660.MAO Xue-bin,D U Z hi-ping,TAI Xiu-mei,et al.Progress in research work field with respect to theory and application of microemulsion[J].C hina Surfactant Detergent&C osmetics,2016,46(11):648-653,660.
[10]李干佐,郭荣.微乳液理论及其应用[M].北京:石油工业出版社,1995.
[11]郑忠,胡纪华.表面活性剂的物理化学原理[M].广州:华南理工大学出版社,1995.
[12]陆明.表面活性剂及其应用技术[M].北京:兵器工业出版社,2007.