羟丙基纤维素接枝改性研究Study on graft modification of hydroxypropyl cellulose.docx
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羟丙基纤维素接枝改性研究Study on graft modification of hydroxypropyl cellulose.docx
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羟丙基纤维素接枝改性研究Studyongraftmodificationofhydroxypropylcellulose
羟丙基纤维素接枝改性研究(Studyongraftmodificationofhydroxypropylcellulose)
Articlenumber:
10044736(2000)04000604
Studyongraftmodificationofhydroxypropylcellulose
YangJiamo,LiShirong,YuFaquan,BiYafan,ChenXiaoyan
(Departmentofchemicalengineering,WuhanInstituteofchemistry,Hubei,Wuhan430073,China)
Abstract:
thegraftcopolymerizationofhydroxypropylcellulosewithmethylmethacrylatewascarriedoutbyusingUVandceriumsaltsastwoinitiators
Theeffectsofreactiontime,temperature,monomerconcentration,photosensitizerorinitiatordosageontheviscosityoftheproductwereinvestigated.Twokindsofinitiationwerecompared
Theoptimumoperationconditionofthereactionisobtained
Keywords:
hydroxypropylcellulose;graftcopolymerization;modification;viscosity
CLCnumber:
TQ361.6,documentidentifiercode:
A
Receiveddate:
20000509
Biography:
YangJiamo(1949),male,ProfessorofZhangshuCity,Jiangxi.LongtermteachingandresearchworkinchemicalengineeringandChemicalTechnology
0Introduction
Themolecularformulaforcottoncelluloseis(C6H10O5)n,whichisformed
Thechiefconstituentoftheplantcellmembrane.Celluloseinthemacromolecularstructure
Consistingofrepeatedglucoseunitslinkedtothe1,4betaglycosidicbond
Thereactioncharacteristicofcelluloseismainlythatitsproductisinhomogeneous
Sexandcomplexity,themolecularstructureoftherawmaterialhasanimpactonthereactionprocess
Thereactionactivityisaffectedbytheneighboringfunctionalgroupandthereactionstripatthesametime
Thetypeofreactionisrelatedtothereaction
Stepprocessingproductstomeetthequalityrequirementsofusersmoredifficult,big
Manyofthemneedtoberemodifiedtoimprovetheirperformance
Graftcopolymerizationisoneofthemostcommonandhasbeenprovedbypractice
Themodificationmethodwithremarkableeffectisthroughtwokindsofmacromolecularbackbone
Chemicallylinkedwithabranchedchaintoproduceaproduct
Withthecomprehensivepropertiesofthesetwomolecules,idealresultscanbeobtained
Improveitsphysicalandchemicalpropertiesoruseperformance
Thenewproductcanbesynthesizedbythefollowingways
Thepurposeofimprovingitsqualityorperformance:
(1)introducingactivegroupsonmacromolecularbackbone
Theinitiationofamonomer,copolymerization,andgrowthofapolymer
Branchedchain;
(2)bymeansof"grafting"(chemicalcombination),akindof
Themolecularchainoftheadductactsasabranchedchainattachedtotheparentmacromolecularbackbone;
(3)intheprocessofpreparingapolymer,makeanotherkind
Polymersareformedsimultaneouslyandareusedasbranchedchainswiththefirstpolymer
Toobtainmacromolecularproducts
Theabovereactionscanbeperformedindifferentways,suchaschaintransferandactivity
Groupmethod,radiationmethod,additionpolymerizationmethodandringopeningpolymerizationmethod,etc.
Etc.,thisworkistousehydroxypropylcellulose,methylmethacrylate
Thelipidwasthemainrawmaterial,whichwascausedbycericammoniumnitrateandultravioletlightrespectively,
Graftcopolymerizationwascarriedouttoimprovecelluloseviscosity
Objectiveandcomparetheadvantagesanddisadvantagesoftwodifferentmethods
Optimumoperatingconditions
1mainrawmaterials,drugsandinstruments
Hydroxypropylcellulose(HEC):
whitepowder,Hubeibell
Cheungcellulosecompanyproducesanaqueoussolutionof.W2%withaviscosityof
20000mPa.s(20DEGC).Dry24h.beforeuse
Methylmethacrylate(C5H8O2)molecularweight:
100.12
Analytical,pure,HubeiUniversitychemicalplantproduction
Cericammoniumnitrate[(NH4)2Ce(NO3)6]referredtoasceriumsalt
Themolecularweightis548.32,purityanalysis,ShanghaiYuelongDayeNon-FerrousMetalsCostudents
Production.
PyrogallicacidC6H3(OH)3:
amolecularweightof126.
11,theanalysisofpure,Guizhou,Zunyisecondchemicalplantproduction
Rotaryviscosimeter:
modelNDJ-1,Shanghaibalanceinstrumentfactory
Production
UVinitiatedgraftcopolymerizationdevice:
Homemade
2experimentprocedureandexperimentscheme
2.1experimentalsteps
Inordernottooxidizethereactionprocess,nitrogenisneeded
Protection.First,anitrogenpurgeunitisassembledtodissolveitthroughcopperammonia
Liquid,pyrogallicacidsolutionandphosphatesolution,andchecktheseals
Acertainamountofdriedhydroxypropylcelluloseisplacedinthereactor,
Addproperamountofdistilledwaterandmixwith2hforconsistency
Aftertheentry,thenitrogenisinjected30min,andthemixtureisstirredatthesametime
Thesaltheatsorturnsontheultravioletlight.Whenthetemperatureisreached,themeterisadded
Theamountofmonomermethylmethacrylate,stirringuntilapredeterminedreactiontime
Theproductisremovedandcooledtoroomtemperature
Determinationofviscosityoftheproduct
Twenty-secondvolumefourthJournalofWuhanInstituteofChemicalTechnologyVol.22No.4
December2000J.WuhanInst.Chem.Tech.Dec.20002.2experimentalprogram
Becauseoftheinfluencefactorsofgraftcopolymerization,more
Theorthogonalexperimentwasusedtoanalyzetheeffectsofvariousfactorsonthepropertiesoftheproducts
Theoptimumreactionconditionswereobtainedandtheleveloforthogonalexperimentwasinvestigated
SeeTable1,table2.
Table1Table1levelfactorofceriumsalt
Table1,Levels,and,factors,of,reaction,initiated,by,Ce4+
Factor
Factors
Horizontal
Levels
123
Reactiontime/h
Reactiontime123
Initiatordosage/mL=L-L
Initiatoramount123
Monomerdosage/mL=L-L
Monomeramount101520
Reactiontemperature/temperature
Reactiontemperature405060
Table2horizontalfactortablesofultravioletlight
Table2,Levels,and,factors,of
Reaction,initiated,by,UV,light
Factor
Factors
Horizontal
Levels
123
Reactiontime/h
Reactiontime123
Photosensitizerdosage/mL=L-L
Photosonsiticeramount304050
Monomerdosage/mL=L-L
Monomeramount579
Reactiontemperature/temperature
Reactiontemperature405060
Aftertheorthogonalexperiment,inordertoinvestigatetheinfluenceofvariousfactorsontheviscosityoftheproduct
Theinfluenceofdegreewasanalyzedbysinglefactor
3experimentalresultsanddiscussion
Analysisoftheresultsof3.1orthogonalexperiments
AccordingtothetableoflevelfactorsshowninTable1andtable2,accordingtotheorthogonalreal
TheruleofexperimentistotaketheorthogonalexperimentofeachfactorindependentofeachotherL9(34)
Theresultsofthetwosetsofexperimentsarelistedintables3and4
Itcanbeseenfromtable3andtable4thatUVinducedgraftreaction
Themostinfluentialfactorwasthereactiontime,whereasceriumsaltswerethemostinfluential
Thebigfactoristheamountofinitiator,whichisthesameasbefore
Theresultsofthestudyareidentical
Theoptimumreactionofcericsaltwasobtainedbyorthogonalexperiment
Theconditionis:
A3B2C3D2,thatis,thereactiontimeis3h,andtheinitiatorisused
Theamountis2mL/L,themonomerdosageis20mL/L,andthereactiontemperatureis
Table3schemeandresultoforthogonalexperimentinitiatedbyceriumsalt
Table3,Orthogonal,experiment,plan,and,effect,of
ReactioninitiatedbyCe4+
Experiment
Serialnumber
TestNo.
Item
Item
ABCD
viscosity
MPa-S
Viscosity
111104026500
212155048200
313206046500
421156032000
522204047200
623105044500
731205043600
832106042800
933154046600
Yi140400.034033.3,37933.3,40100/
Yi241233.346066.7,42266.7,45433.3/
Yi344333.345866.7,45766.7,40433.3/
range
Limite
Rreur
3933.3,12033.4,7833.3,5333.3/
Table4schemeandresultofUVinducedorthogonaldesign
Table4,Orthogonal,experiment,plan,and,effect,of
Reaction,initiated,BG,UV,lighe
Experiment
Serialnumber
TestNo.
Item
Item
ABCD
viscosity
MPa-S
Viscosity
113054028600
214075051500
315096046300
423076046500
524094060600
625055058400
733095051600
834056052200
935074055600
Yi142133.342233.3,46433.3,48266.7/
Yi255166.754800,51200,53833.3/
Yi352500.053433.3,52833.3,48366.7/
range
Limite
Rreur
13033.3,12566.7,6400,5566.6/
50.TheoptimumoperatingconditionsforUVinducedreactionsare:
A2B2C3D2,thatis,thereactiontimeis2handthephotosensitizerdosageis40
ML/L,theamountofmonomeris9mL/L,thereactiontemperatureis50DEGC
Fromtheresultsoftheviscosityoftwosetsofreactionproducts,theeffectofUVirradiationwasobserved
Theeffectisclearlysuperiortothatcausedbyceriumsalts,i.e.,UVinduced
Thegraftingratioshouldbehigherthantherateofgraftinginitiatedbyceriumsalts
Theworkwasconsistentwithpreviousstudies
7,fourth,YangJiamoetal.Studyongraftmodificationofhydroxypropylcellulose3.2singlefactoranalysis
AscanbeseenfromFigure1andFigure2,thereactiontimeisrelativetothetwokindsofgrafting
Fig.1Effectofreactiontimeofceriumsaltonviscosity
Fig1,Viscosity,of,graft,copolymer,initiated,by,Ce4+
Was,influenced,by,reaction,time
Fig.2EffectofUVirradiationreactiontimeonviscosity
Fig2,Viscosity,of,graft,copolymer,initiated,by
UV,light,was,influenced,by,reaction,time
Thereisanoptimumvalueforthepolymerizationreaction,whentheproductviscosityexceedsthisvalue
Instead,thismaybethemainchainatthebeginningofthereaction
Theinitiationandchaincontinue,whilethereactiontimeistoolong,whichwillleadtograftcopolymerization
Thechainterminationreactionacceleratedandthegraftingratedecreased
Theoptimumoperationtimeofthegraftcopolymeriza
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