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Information to Users INFORMATION TO USERS Thil manulCl'ipt 1181 been reproduced from the microfilm mater. UMI films the text directly tram the originll or capy 1Ubmitted. Thuit sorne thelil and diuertmion COpiel are in typewriter face, whi.. oth8rI .".y be from any type cl computer primer. The quallty of thla Nproductlon la .pendent upon the quallty of the capy submitted. Broken or indistinct prim. coIored or poor quality illustr8tions .nd photographl, print bleeclthraugh t lubltandard m8rginlt and improper alignment can &dversely 8ffect reproduction. ln the ""'ikely event th8t the author did not send UMI • complete msnuscript and there are misling pages, the.. will be noted. AllO. if unauthorized copyright mat.rial Nid ta be removed, 8 note will indic8t the deletion. Overlize materiall (e.g., mapl, dl'8Wing.. chlrtl) .,. reproduced by sectioning the original, begiming 8t the upper Ieft-hn:l corner and continuing from 18ft ta right in equal sec:tions with small overtaps. Photographs incIucIed in the original manuscrfpt NIve been repraduced xerognlphically in thil copy. Higher ~Iity S- x 9" black and white photog_ic prints are aVlilibie for ~y photogrlphl or illultnltionl appe8ring in thil capy for an .ciditional chlrge. Contact UMI directly to arder. Bell &HoweIllnrorm.tion and Lening 300 North 2Mb ROId. Ann Arbor, MI .108-1348 USA 800-521-œoo • THE PRESSURE-VOLUME-TEMPERATURE BEHAVIOR AND THE EFFECT OF PREsSURE ON CRYSTALLIZATION KlNETiCS OF POLYETHYLENE REsINS by • Ludovic CAPT A Thesis Submittecl to the FICUIty orGraduate 5tudies and Research in Partial Fulfillment orthe Requirements for the Degree ofMuterorEnpneering Department ofCbemical EnlÏDeering McGiIl University Montreal Ianuary, 1999 National Ubrary BibliothèQue nationale 1+1 of Canada du Canada Acquisitions and Acquisitions et Bibliographie Services services bibliographiques 385 wellington Street 395. rue WelUngtan OtIawaON K1A0N4 Ottawa ON K1A 0N4 C8nIda c.n.dII The author bas granted a oon­ L'auteur a accordé une licence non exclusive licence allowing the exclusive permettant à la National Library ofCanada to Bibliothèque nationale du Canada de reproduce, loan, distnbute or seU reproduire, prêter, distribuer ou copies ofthis tbesis in microform, vendre des copies de cette thèse sous paper or electronic formats. la fonne de microfiche/~ de reproduction sur papier ou sur format électronique. The author retains ownership ofthe L'auteur conserve la propriété du copyright in this thesis. Neither the droit d'auteur qui protège cette thèse. thesis nor substantial extracts ftom it Ni la thèse ni des extraits substantiels may he printed or otherwise de celle-ci ne doivent être imprimés reproduced without the author' s ou autrement reproduits sans son penmSSlon. autorisation. 0-612-50594-4 • ABSTRACT In plastics manufàeturing. the morphology and crystallinity are important in the determination ofthe properties ofthe final product. They are influencecl by seven1 parameters, in particular the pressure and the temperature history during solidification. Therefore, the study of the influence of pressure and temperature on crystaUization kinetics is important. In tbis study~ the crystaIlization Idnetics and the PVT behavior of various grades ofpolyethylene resins were evaluated and compared using a bigh-pressure dilatometer under bath isothermal and isobaric conditions. A1so, the PVT behavior wu compared to the predictions ofthe Tait equation ofate. It wu round that polyethylene chain structure, u determined by branching and branching uniformity, int1uences nucleation, crysta1lization kinetics, and the effeet of pressure on these processes. In addition, the mults confirm the decrease ofthe surface ftee energy ofthe crystal nucleus • with increasing pressure. • ü • RtsUMt Dans la fabrication d'articles en plastique, les propriétés du produit fini SOlit principalement déterminées par la morpholoaie et la cristaUinité. Ces demims sont controlées par plusieurs paramètres. en particulier par la pression et la température. pendant la solidification. En collléquence, il est intéreuant d'étudier l'éffet de la pression et de la température sur la cinétique de cristallisation. Dans le cadre de cette étude, la cinétique de cristallisation et les diqrammes de Pression-Volume-Température d'une variété de résines de polyéthylene ont été investisué. et comparés en utilisant un dilatomètre à haute pression. De plus, le comportement de l'état fondu a été comparé avec les prédictions de l'équation d'état de Tait. D a été découvert que les propriétés structurelles de la chaine moléculaire du polyéthylene, en particulier les branches et leur distribution, influencent 1& nucléation, la cristallisation et l'efret de la pression sur ces deux phénomènes. Les résultats ont aussi confirmé la diminution de l'énergie libre de • surface du nucleus avec l'augmentation de la pression. • üi • A la mémoire de mon grand-père PierroL • • iv • ACKNOWLEDGEMENTS 1 wish ta express my deepest Appreciation and utmost sratitude for the guidance and encouragement received trom my research supervilOr, Prof M. R. ICamaI, who stimulatecl my initial interest in the field ofpolymer science and engineering_ 1 alsa would like to express my sincere appreciation to Mf. M. Samara for his invaluable comments anclsugestïons duriDg this investiption, IJICI to my colleapes for their belp in various upects. 1am indebted to Nova Cbemicals for supplying the materials used in this study. 1 alsa extend my gratetùlness 10 the financial support receiveel Û'om the National Science and Engineering, Research Council ofCanada. the Ministère de l'Education du Québec, and the department of Chemical Engineerins in the fonn of teaching and research assistantships. 1 am especially sratetùl to Miss Gloria Vendrell for her encouragement and ber SUl8estions. Finally, 1 would like to express my love to my parents for their patience and • constant encourqemenl • v • TABLE OF CONTENTS ABStRAcr ---------------------ii AcxNOWLEDGEMENT ------------------v TABLB OF CONlENTS vi LIST OF FIGURBS De LIST OF TABLBS xiii 1 IN'I'aOOUcnON 2 TllEOUTICALBACKGROOND 2.1) U••r Law Deult)' Potyetll,.e., 2 2.1.1) Catalysts Cor LLDPE Production 3 2.1.1.1) Ziegler Catalysts 3 2.1.1.2) Metalloœne Cattllysts 3 2.1.1.3) ClroIIIhmI Dnde-BasedCatalysts 4 2.1.2) Polymerization Processes S 2.1.2.1) Gas-phtlse Polymerization 5 2.1.2.2) Solution Polymerization 6 2.1.3) Properties ofLLDPE 6 • 2.1.3.1) Type 01COIIfOIIOIIIer 6 2.1.3.2) Branching lJniformity 1 2.1.3.3) Cryata/linity anddensity 1 2.1.3.4) Mo/eCliIar Weight 7 2.1.3.5) PhysictdProperttes 8 2.2) PoIy.er Cry.....iado. 10 2.2.1) Polymer morphololY 10 2.2.1.1) Po/ytIIer Crystllllograplry Il 2.2.1.2) CItain Folding and iœIIellar erystals 12 2.2.1.3) SpIJenIlites 15 1.2.1) Nucleation and growth 17 2.2.2.1) Nucl«ltion 17 2.2.2.2) Crystal Growth 19 2.2.2.3) Secondtry Crystlll/iZlltion and Crystal Perfection 23 2.2.3) CrystalliJation lCinetics 24 2.2.3..1) TIte Kinetic Equations 25 2.2..3.2) FtlCtors ilflluencingcrystG1/iZlltiOll ii_tics 29 2.2.. 3.3) Otlters .,ecuolCrpltlllimtionKinetics 31 2.3) ........Vol••e-Te.pen..re Pnperdel.Ip.a,.en 34 • 2.3.1) Pressure-Volume-Temperature Apparatus 34 vi 2.3.2) Equations ofState 34 2.3.2.1) The TlJsoretical Si",1ta-Somcyruky .quation 35 2.3.2.2) The Modified Tait equation 36 • 2.3.2.3) TIte Inverse-Vo"'" Eqwztion 37 2.3.3) Compreuibility and Thermal Expansion Coefficient 38 2.3.4) Literature Review for VariOUI Polyethylenes 39 3 SCOPE AND OBlECl1.VD 4 ExPEIuMENTAL 4.1) Potyedlyleae Relia Propertia .... 4.2) PftlIUn-Volume-Te.perature Apparatul 41 4.3) PVT M..ure••t Technlqu. 43 4.3.1) Sample Preparation 43 4.3.2) Calibration 44 4.3.3) Experiment Description 44 4.3.3.1) lsothel7lltll 1IIelISIUeme"ts 45 4.3.3.2) lsoborlc IlleQSlll'e,.nts 46 4. 3.J.3) lsothermaVIsobaric M.QSllr,,,,,,,ts 46 5 DATAANALYSIS 5.1) lIothermal Masure.eau 50 S.1.1) Determination orthe Additional Volume SO S.1.2) Determination ortheMelt and Solid State Regiona 51 • S.1.3) Determination orthe Parameters ofthe Tait Equation SI 5.1.4) Determination ofthe Parameters ofthe Inverse-Volume Equation 53 S.1.S) Isotbermal Measurement Limitations 53 5.2) IIobarie Meuun.eatl 54 5.3) IIotilenullllobaric Masuremeau 5f S.].I) Crysta1lization durinl Pressurization 56 S.3.2) Induction Time and BeginnÎDI ofCrystallization S8 S.3.3) End ofCrystl1IiRtion S9 S.3.4) Crystallization Temperature ofthe Experiment 60 6 REsULTS AND DISCUSSION 6.1) PVT Propertiel '2 6.1.1) General PVT Behavior 63 6.1.2) PVT Melt Bebavior 66 6.1.2.1) Tait EquDlion 67 6.1.2.2) Inverse-VobIMe EqwztiOll 70 6.1.3) Isothermal Compreuibility and Thermal Expansion Coeflicient 73 6.1.3.1) IsotItmrtal COIIIpI'esri61/ity 73 6.1.3.2) 1'ItmIItIlErponsiOll CœJficient 7$ • 6.1.4) Summary 78 vii 6.2) Preslure Depe.d.ee 01 Crystalizatioa ud Meltia. '9 6.2.1) General Bebavior in Isobaric Experimenta 79 6.2.2) Pressure Dependenc:e ofT. and Tc: 82 • 6.2.3) Me1tina and Crystal1izatiOD curvel und..Pressure 85 6.2.4) Summary 81 6.3) Cry"I'lado. Xûleda .9 6.3.1) SecondaryCrystallization Eftèct 90 6.3.2) Crystallization Kinetic data 92 6.3.3) Effect ofPressure 011 Crysta1lization Kinetics 96 6.3.4) FurtherInterpretation 101 6.3.S) Summary lOS 7 SUMMARY, CONCLUSIONS, AND FURnIER WORIC 7.1) Sam.ary aad C.ad.iou 106 7.2) 1leeo••eadatioa 'orPurther Work 10. REFERENCES 110 APPENDICES APPENDIXI: PVT SAMPLER.UNS A-t LI) sa.pIe Rua Pnpantioa A-I • U)Callbntioa or"pieRua A'" U) Reca•••datiou A·5 APPENDIX U: ERROR ANALYSIS A-6 8.1) Ernria die VoI••e CIIu.eM...,..eDt A-6 lU) Repeatability .1iIoda..aI ••••n.... A-I APPENDIX m: IsoBARIC ExPERIMENT DATA A-9 DLI) IIobarie Esperi••t Oata A-' ID.2) Cry......tio.
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