尼龙_6的合成工艺研究_周诗彪

261Vol.26No.120143JournalofHunanUniversityofArtsandScience(NaturalScienceEdition)Mar.2014doi:10.3969/j.issn.1672-6146.2014.01.005-6,,,,,(,,415000):,,,,(PA6).-6,-6,.,2403.5h100:2100:3,92.0%,6.9×104g/mol.:;;;:TQ323.6:1672-6146(2014)01-0016-06StudyonthesyntheticprocessofNylon-6ZHOUShiBiao,XIAOAnGuo,LUPeng,YANGJin,HUANGXiaoBing,ZHUANGYongBing(DepartmentofChemistryandChemicalEngineering,HunanUniversityofArtsandScience,Changde415000,China)Abstract:Polycaprolactamwassynthesizedviaring-openingpolymerizationusingwaterasinitiator.Inthepolymerizationprocess,oxalicacidwasadoptedforstabilizer.Theinfluencesofpolymerizationconditionontheconversionrateandsofteningtemperatureofresultantpolymerwereinvestigated.Theoptimalpolymerizationconditionsweredeterminedwiththeresultsoftheconversionrate,softeningtemperatureandinfraredspectraofresultantpolycaprolactam.Caprolactamconversionratewasupto92%underthereactiontemperatureof240whentheratiosofthephosphoricacidandoxalicacidtocaprolactamwas0.02and0.03,respectively,viscosityaveragemolecularweightofresultantpolymerwasabout6.9×104g/mol.Keywords:caprolactam;polycaprolactam;polymerizationprocess;ringopeningagent(PA),PA6PA66PA11PA610PA1010,PA6PA66,90%.-6,,.[1][2—8][9],,[10—14].,.-6,-6.11.1,,;,,;email:[e-mail].:2014-01-06:(14JJ2123);2013.1,:-617,,;,,;,,;,,;,,.CL-4A,;Nicolet370,;BS3005-O,;YKKYFM70,;YW-1,;KQ5200B,;,.1.21.2.1,,.,160,1h,.250,,.,-6,45h.1.2.2-6,[15],95%,,,-6,.,NaOH-6PH7,48h.1.2.3-6,1h,,,.V=21100%MM,,V,M1(g),M2-6(g).1.31.3.1-6,,X-5().,80,10/min,-6,.1.3.2KBr-6100:1,,.1.3.3-6,40%,25,3[16].:[]αηKM[]η,K=5.92×102cm3·g1,α=0.69[17],M.22.12.1.120g,3%,1%,220230240250,210220230240250727680848892//%118()2014,,.,1.1,,,240,,,;.3.·,,,;,,,,,,.,,[18].2.1.2,[19]..20g,3%,1%,220230240250,,,,2.2,,.,-6;,,-6.:,;.2.1.3,[20].20g,,0.5%,1%,2%,3%,5%,1%,2403.5h,,3.3,,.,;,,.:,100:1,,100:2,.2.1.4.20g,0.4g,,240,2.533.54.5h,,4.,.,,40%42%,,,..,,.2102202302402505060708090100//%20.000.010.020.030.040.056065707580859095100/%31,:-619,,,.,,.,,.,,.4,,,,,,.2.2-6-6,.,.2.2.1-620g,,3%,1%,220230240250,,,,5.5,;,,,.2.2.2-620g,3%,1%,220230240250,,.,6:6,,-6.-6-6.:,-6,-6,,.2.2.3-620g,0.5%,1%,2%,3%,5%,1%,2403.5h,,7.7,,-6.,;,,.,,100:1,,100:2,.2.2.4-6,240,20g,0.4g,2.533.54.5h,8.8,,,-62.42.83.23.64.0727680848892/%/4-6/210220230240250190200210220230240250/5-620()2014,;,,.,,.2.39.9,3299.1cm12930.0cm11635.9cm11540.6cm1,3299.1cm1,2930.0cm1—CH2—CH2—,1635.9cm1C=O,1540.6cm1N—H.[18].2.4-6,,-6,.,,,.,,,,.,,.,210220230240250190200210220230240250//6-60.000.010.020.030.040.05200210220230240250/7-60246215220225230235240/%/%10-62.53.03.54.04.5200210220230240/h/8-64000300020001000/cm1605040302010R/%961,:-62110.10,,-6,.-6,-6.100:3.3,,:,240,3.5h,100:2,100:3,,92.0%,6.9×104g/mol.:[1]W,RJH.ε--6[P].CN:99814711,2002-01-16.[2]DanielCrespy,KatharinaLandfester.Anionicpolymerizationofε-Caprolactaminminiemulsion:synthesisandcharacterizationofpolyamide-6nanoparticles[J].Macromolecules,2005,38:68826887.[3]DemicheliA,RussoS,MarianibA.Synthesisandcharacterizationofε-caprolactam-L-phenylalaninecopolymers[J].Polymer,2000,41:14811486.[4]LauraRicco,OriettaMonticelli,SaverioRusso,etal.Fast-ActivatedAnionicPolymerizationofε-caprolactaminsuspension.Macromol[J].ChemPhys,2002,203:14361444.[5]MatevaR,PetrovP,RoussevaS,etal.Onthestructureofpoly-ε-caprolactams,obtainedwithbifunctionalN-carbamylderivativesoflactams[J].EuropeanPolymerJournal,2000,36:813821.[6]LauraRicco,SaverioRusso.Caprolactam-laurolactamcopolymers:fastactivatedanionicsynthesis,thermalpropertiesandstructuralinvestigations[J].MacromolChemPhys,2001,202:21142121.[7]LauraRicco,SaverioRusso,OriettaMonticelli,etal.ε-Caprolactampolymerizationinpresenceofpolyhedraloligomericsilsesquisoxanes(POSS)[J].Polymer,2005,46:68106819.[8].PA6[J].,1996,19(2):3542.[9],.PA6[J].,2000,(34),19.[10].[J].,2004(2):1618.[11],,.[J].,2003,26(4):2223.[12].[J].,1999,13(4):2127.[13].[P].CN:1374333A,2002-10-16.[14],.[J].,2007,25(2):2023.[15][]B..,.()[M].:,1980:7779.[16].PA6[J].,1999,22(5):5052.[17],,,.[M].2.:,2009:431446.[18],,,.[M].:,2003:2028.[19],,,.[M].:,1982:9293.[20].[J].,2006(2):3334.(:)