双烷链阳离子表面活性剂的合成与定量分析

312222(1,2,200237)N,N2,2,GeminiP,;:7Gemini97.5%,,,,2002204214;2002209229(No.200258618)1Gemini1(),,GeminiCMCKraff;;2,Gemini,Gemini,,36,2,Gemini,,Gemini,22.1N,N2N,N2N,N2(,),97%;1,321,421,62(),98%;(),99.9%;(AR,);:pH();(CP,);(AR,);(AR,):0.87g(0.1mg),,1000mL,0.05%(BPB):50mg,100mL:(AR)1%NaOH2,,828410%Na2CO3:10gNa2CO3(AR),100mLNicoletMagna2IR2550,KBr;Brucker2Avance2500,CDCl3,TMS2.2GeminiN,N2460mL(1.6molPL)1,3280mL(0.77molPL)200mL,1000mL,,,80,48h25.8kPa,Gemini1223212,2Br2,3120033(FENXIHUAXUE)ChineseJournalofAnalyticalChemistry3322325234,5060610h,416g(0.663mol)Gemini1223212,2Br2,87%GeminiGemini,2.3[7](BPB),,,,:ROSO3Na+BPB+XQQXpH9.812R-OSO3QQ()+BPB(1):BPB+XQQXpH9.812QQBPB(,)(2)(1)(2)Gemini;X2.4[8]99.5%(wt.)5g(0.1mg),300mL,25mL2molPL,,,,2h,30mL95%(wt.),,100mL,(1%WPV),1molPL,:P=M(V1-V0)CNaOHm100(3)(3):M;m(g);CNaOH(molPL);V1(mL);V0(mL)2.5(1)20mL,10mL10%Na2CO30.5mL1gNaCl70.05%10mL(2)Gemini,,500mL(11510-3molPL),(3)Gemini,(4)Gemini:Conc.%=CaVa2(V1-V0)0.5Mm100(4)(4):MGemini;m(g);Ca,Va(molPL)(mL);V1(mL);V0(mL)33.1Gemini3.1.1IR13Gemini1222212,2Br-,1623216,2Br-,1626216,2Br-IR28503000cm-1,14301500cm-1720730cm-1;CN8701250cm-13233:1610162034103510cm-1H2O1GeminiFig1.InfraredspectraofcationicGeminisurfactants111223212,2Br-;211623216,2Br-;311626216,2Br-2Gemini1223212,2Br-Fig.2ChemicalshiftofnuclearmagnetismresonanceforGemini1223212,2Br-surfactants3.1.22Gemini1223212,2Br-1HNMR,H:CH30.90(6H)CH1.32(36H)NCCH21182(4H)NCH23.54(4H);NCH33.34(12H);NCCH22.73(2H)NCH23.86(4H);4.51Gemini1223212,2Br-Gemini11GeminiTable1ChemicalshiftofnuclearmagnetismresonanceforcationicquaternaryammoniumsaltGeminisurfactantsSurfactantsChemicalshift(10-6)AlkylchainCH3CH2NCCH2NCH2N2CH3AlkanediylspacerNCCCH2NCCH2NCH21223212,2Br-0.90(6H)1.32(36H)1.82(4H)3.54(4H)3.34(12H)2.73(2H)3.86(4H)1226212,2Br-0.89(6H)1.30(36H)1.59(4H)3.46(4H)3.37(12H)1.72(4H)2.0(4H)3.67(4H)1623216,2Br-0.88(6H)1.30(52H)1.80(4H)3.50(4H)3.40(12H)2.70(2H)3.82(4H)1624216,2Br-0.88(6H)1.32(52H)1.77(4H)3.45(4H)3.30(12H)2.14(4H)3.90(4H)1626216,2Br-0.88(6H)1.32(52H)1.52(4H)3.48(4H)3.38(12H)1.71(4H)2.0(4H)3.70(4H)1823218,2Br-0.86(6H)1.27(60H)1.78(4H)3.50(4H)3.38(12H)2.65(2H)3.80(4H)1826218,2Br-0.83(4H)1.26,1.6(60H)1.71(4H)3.45(4H)3.37(12H)1.89(4H)2.03(4H)3.71(4H)3.2Gemini,,(4)Gemini,22,Gemini,Gemini,97.5%42GeminiTable2ThecontainingofcationicGeminisurfactantssynthesizedSurfactantsContent(wt%)1223212,2Br-97.581226212,2Br-98.451623216,2Br-99.121624216,2Br-98.541626216,2Br-99.491823218,2Br-98.871826218,2Br-99.76N,N2,Gemini,P,Gemini,7Gemini97.5%,Gemini42331References1MengerFM,LittauCA.J.Am.Chem.Soc.,1991,113:145114522RosenMJ.Chemtech.,1993,(3):30333ZanaR,BenrraouM,RueffR.Langmuir.,1991,7:107210754ZanaR.Dimeric(Gemini)Surfactants,ed.byKristerHolmberg,NewYork:MarcelDekker,1998:2422785DevinskyF.TensideDetergents.,1985,22:10156WangShengkun(),JiangXingkun().OilChemistry().1998,15(22):2892927CullumDC.IntroductiontoSurfactantAnalysis.BlackieAcademic&Professional,AnImprintofChapman&Hall.1994:1711918ZhongLei(),DingYoudan().AnalysisofSurfactantsandItsAssistants().Hangzhou():ZhejiangScienceandTechnologyPress(),1986:120121SynthesisandQuantitativeDeterminationofAlkanediyl2,2bis(dimethylalkylammoniumbromide)ShiYunhai31,ChenQibin2,TongSi2,LiuHonglai2,HuYing2(ResearchCentreofChemicalEngineering1,DepartmentofChemistry2,EastChinaUniversityofScienceandTechnology,Shanghai200237)AbstractCationicGeminisurfactants,alkanediyl2,2bis(dimethylalkylammoniumbromide)weresynthesizedfromN,N2dimethylalkyltertiaryamineand,2alkyldibromidebyusingethanolassolvent.Thereactantswererecystallizedintheethylacetate2ethanolsolventmixtureandgavethepurifiedproducts.TheGeminiproductswerequalitativelydetectedandverifiedbyinfraredand1Hnuclearmagneticresonanceanalysis,andwerealsoquantitativelydeterminedbythetwo2phasechemicaltitrationbyusingbromophenolblueastheindicatoranddichloroethaneasphasespilttingagent.TheresultsshowedthatthepurityofthesevensynthesizedGeminisaregreaterthan97.5%inweight.KeywordsGeminisurfactant,nucleophilicaddition2saltformingreaction,chemicaltitrationanalysis;N,N2dimethylalkyltertiaryamine,dibromoalkane(Received14April2002;accepted29September2002)2003:82-4311982,,,2003:,,,,,X,19982001,42002CA,,16,112,10,60,82-431,:2,100088:010-82013328,E2mail:[e-mail],http:PP