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时间:2020-03-27
《烯丙基二甲基脱氢枞基氯化铵的合成及其条件优化.pdf》由会员上传分享,免费在线阅读,更多相关内容在行业资料-天天文库。
1、第1O期化学世界·6l9·烯丙基二甲基脱氢枞基氯化铵的合成及其条件优化徐大雄。,蔡照胜“,陈智栋,许琦(1.常州大学石油化工学院,江苏常州213164;2.盐城工学院化学与生物工程学院,江苏盐城224051)摘要:在四甲基哌啶基氧(TEMPO)存在下,以脱氢枞胺(DHA)为原料,经Eschweiler—Clarke反应得到N,』\,一二甲基脱氢枞胺(DMDHA)后,再于乙腈溶剂中与氯丙烯进行季铵化反应合成了烯丙基二甲基脱氢枞基氯化铵(ADMDHAC);用FTIR、HNMR和”CNMR袁征了产物结构,两
2、相滴定法测定了产物中ADMDHAC含量,正交试验法优化了ADMDHAC合成条件,表面张力法测定了产物的临界胶束浓度(CMC)。结果表明,ADMDHAC最佳合成条件为:反应温度65℃,TEMPO用量为DMDHA质量的1.25,DMDHA与氯丙烯摩尔比为1:1.6,反应时间为144h;此条件下产物收率为51.11,产物中ADMDHAC含量为97.87;临界胶柬浓度为2.0mmol/L。关键词:烯丙基二甲基脱氢枞基氯化铵;阳离子表面活性剂;合成;临界胶束浓度中图分类号:0621.3文献标志码:A文章编号:0
3、367—6358(2014)1O一0619—05SynthesisofAllylDimethylDehydroabiety1AmmoniumChlorideandOptimizationofItsSyntheticConditionsXUDa—xiong~,CAIZhao—sheng,CHENZhi—dong,XUQi(1.SchoolofPetrochemicalEngineering,ChangzhouUniversity,JiangsuChangzhou213164,China;2.School
4、oJChemicalandBiologicalEngineering,YanchengInstituteofTechnology,JiangsuWancheng224051,China)Abstract:Dehydroabietylamine(DHA)wastransformedintoN,N—dimethyldehydroabietylamine(DM—DHA)throughEschweiler—Clarkereaction,andthenallyldimethyldehydroabietylamm
5、oniumchloride(ADMDHAC)wassynthesizedbythereactionbetweenDMDHAandallylchloridewithacetonitrileassol—ventinthepresenceof2,2,6,6-tetramethyl一1一piperidinyloxy(TEMPO).TheproductwascharacterizedbyFTIR,HNMRandCNMR,andthecontentofADMDHACinproductwasmeasuredbyat
6、wo—phasetitrimetricmethod.ThesyntheticconditionsforpreparingADMDHACwereoptimizedusingorthogonalexperiments.Thecriticalmicelleconcentration(CMC)oftheproductwasinvestigatedbytestingthesur—facetensionofitsaqueoussolution.Experimentalresultsindicatedthatthe
7、optimumconditionsforprepar—ingADMDHACwereasfollows:thereactiontemperaturewas65℃;themassratioofTEMPOversusDMDHAwas1.25;themoleratioofDMDHAversusallylchloridewas1:1.6;andthereactiontimewas144h.TheyieldofADMDHACreached51.11undertheoptimumconditions,andthec
8、ontentofADMDHACinproductwas97.87.TheCMCofADMDHACinaqueoussolutionwas2.0mmol/L.Keywords:ally1dimethyldehydroabietylammoniumchloride(ADMDHAC);cationicsurfactant;synthe—sis:criticalmicelleconcentration收稿日期:2013-l1—25;修回日期:2O13—12—15
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