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Nylon 6.6

Nylon 6.6

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Vol.12No.1CHINESEJOURNALOFPOLYMERSCIENCE1994
STUDYONTHEMECHANISMOFNYLON6,6DISSOLVINGPROCESSUSINGCaCb/MeOHASTHESOLVENT*
(ResearchInstituteofPolymerMaterials,BeijingInstituteofChemicalTechnology,Beijing100029)
ABSTRACT
Adiscussionofthemechanismofnylon6,6dissolvingprocessusingCaC1
2
/MeOHasthesol-ventispresented.Thecalciumchlorideformsacomplexcompoundwithnylonfi,6bybreakingthehydrogenbonds.ThemeltingpointoftheCael
2
-nylon6,6complexwasfoundtobereducedby
91K
relativetothepurenylon6,6polymer.Theroleofmethanolissomewhatsimilartoacatalyst.TheresultsdemonstratethatthecomplexationofaLewisacid(CaCl,)andaLewisbase(nylon6,6)canbeusedtoprobeintermolecularinteractionssuchashydrogenbondinginpolymers,tomodifythepolymerpropertiesandmediateitssolubilityandprocessing.
INTRODUCTION
Asymmetricnylon
6,6
membranescanbemadebyastandardwetphaseinversionprocessprovidedasuitablesolventcanbefound.Asnylon
6,6
hasastructureinwhichtheN-HgroupsinthechainarehydrogenbondedtotheC=Ogroupsinadjacentchains(Figure
1),
ithashighcrystallinity,ahighmeltingpoint(523-545K)[lJ,goodmechanicalproperties,andchemicalstability.Consequently,itisimpossibletodissolvenylon
6,6
beforeitshydrogenbondsaresevered,anditisdifficulttofindasuitablesolventtodissolvenylon
6,6.
Inrecentyears,twokindsofsolventsfornylon
6,6
weredeveloped.Oneisformicacid[2,3,4J.However,formicacidisunpleasanttoworkwithandcausessomedegradationofthepolyamide[S,6J.Theotherisanalcohol!saltsolution.Thissolventsystemcanbeusedtoformporousmembranesheetsofhighmolecularweightpolymerwithoutdegradationandstrengthreductionasassociatedwiththeformic-acid-basedmembranes.Forexample,a
methanolz'Ce.Cl,
solutionisadesirablesolventfornylon
6,6.
Nylon
6,6
wasobservedtobeinsolubleinmethanol,butsolubleinamethanol/CaC12solution.Thisshowsthatthesaltisimportantinthe
*
ReceivedAugust7,
1992
 
58
CHINESEJOURNALOFPOLYMERSCIENCE
1994
polymerdissolvingprocess.
It
isknownthatcalciumchlorideisaLewisacid,anditcancomplexwithamides(Lewisbases).Forexample
.it
cancomplexwithacetamideandthecomplexnumber
x
maybe1,3,4or6dependingonthe
temperaturel'",
CaCl
2
+nCH
3
CONH
2
---CaCI
2
xCH
3
CONH
2
Robertsetal.
[8J
reportedtheconceptofusingaLewisacid(galliumchloride)complexationofapolymer(nylon6)tomodifypolymerproperties.Theaimofthispaper,therefore,istoreportthefindingsofourstudyontheroleofthesaltandthemechanismofthenylon6,6dissolvingprOCeSS.
EXPERIMENTAL
Materials
-,
NH.··
"
,
OC~H"ocfHOC?
/<
co-..
("COOH<
H/OH~<H
~,
,
?
NH..·
oc
NH...
oc"
J"
"·oc
-,
Fig.1Hydrogenbondedstructure
ofnylon6,6
TheNylon6,6studiedwasCelanese
1200-1
with
Mwof
120,000
and
M;
of
50,300.
ThecalciumchloridewasFisherCertifiedACSgrade.Themethanolwas
J.
T.BakerAnalyzedReagentgrade.
Solutionpreparation
Twodifferentkindsofsolutionswereprepared.SolutionA:nylonpolymerwasaddedtomethanolandheatedtorefluxforseveralhours,thenCaCl
2
wasaddedandtheresultingmixturewasheatedtorefluxforseveralhoursmore.SolutionB:nylonpolymerwasaddedtoasolutionofcalciumchlorideinmethanolandheatedtorefluxuntilthenylondissolved.
Membranesamplepreparation
CaClrnylon6,6membrane:MembranesamplesofCaCl
2-
nylon6,6forFouriertransforminfrared(FTIR)andmeltingpointmeasurementwerepreparedbycastingthenylon6,6/CaCI
2
/methanolsolutionontoaglasssub-stratesfollowedbyaslowevaporationofthesolventinafumehoodandtheninavacuumovenatroomtemperaturefor48hours.Nylon6,6membrane:Acastingsolutionwaspreparedbydissolving
 
Vol.12No.1
MECHANISMOFNYLON6,6DISSOLVINGPROCESS59
nylon6,6informicacidatabout400K.Thesolutionwasthencastontoaglasssubstratefollowedbyaslowevaporationoftheformicacidinafumehood,theninavacuumovenatroomtemperaturefor48hours.
Testforfree
Ca2+
insolution
CarbondioxidegaswaspassedthroughsolutionAandsolutionBseparatelytotestfortheexistenceoffreecalciumcations.
AnalysisofpermeateofsolutionB
SolutionBwasseparatedbypermeatingthroughaPVCultrafiltrationmembraneunderthepressureof18psiandatroomtemperature.Theper-meate;apuremethanolsample,andamethanbl/CaClzcomplexsolutionsamplewerecastseparatelyontoaKBrsubstrateforinfraredspectroscopy.MethanolsamplewerecastseparatelyontoaKBrsubstrateforinfraredspectroscopy.InfraredspectrawerecollectedonaBeckmanInfraredSpectrometer.
Meltingpointmeasurement
ThemeltingpointsoftheCaCl~-nylon6,6membranesampleandthenylon6,6sampleweremeasuredwithaPERKIN-ELMERDSC-2Differen-tialScanningCalorimeterusingflowingnitrogen.Indium(rn.p.156.6°C)DSCStandardwasusedtocalibratethemeasuredtransitionpoints.Samplesintherangeof
1.
7to4.4mgweresealedinDSCpans.Thescanratewas10K/min.
FTIRmeasurementofmembranesamples
TheinfraredspectraoftheCaCh-nylon6,6membranesampleandthenylon6,6membranesamplewerecollectedonaBIORADFTS-15/90FourierTransformInfraredSpectrometeratroomtemperature(22°C)undernitrogenpurge.
RESULTS
Experimentalphenonmenaofthedissolvingprocess
Threedifferentexperimentalphenomenaofthedissolvingprocesswereobserved.First,nylon6,6wouldnotdissolveinmethanol.Second,thenylon6,6insolutionApartiallydissolved.Third,whencalciumchloridewasdissolvedinmethanol,muchheatwasreleased.Finally,nylon6,6dissolvedcompletelyintheresultingMeOH/CaClzsolution.

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