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  • Post-Consumer Poly(ethylene terephthalate) – Properties,

    Problems during Reprocessing, and Modification by

    Reactive Extrusion

    Von der Fakultät für Mathematik, Informatik und Naturwissenschaften der RWTH

    Aachen University zur Erlangung des akademischen Grades eines Doktors der

    Naturwissenschaften genehmigte Dissertation

    vorgelegt von

    Dennis Berg, M.Sc.

    aus Adenau, Deutschland

    Berichter: Universitätsprofessor Dr. rer. nat. Martin Möller

    Universitätsprofessor Dr. rer. nat. Andrij Pich

    Tag der mündlichen Prüfung: 17.12.2018

    Diese Dissertation ist auf den Internetseiten der Universitätsbibliothek verfügbar.

  • Für Karen…

  • „Suche nicht andere, sondern dich selbst zu übertreffen.“

    Marcus Tullius Cicero (106 - 43 v. Chr.)

  • II

    Eidesstattliche Erklärung

    Hiermit versichere ich, Dennis Berg, dass ich die vorliegende Dissertation

    selbständig verfasst und keine anderen als die angegebenen Quellen und Hilfsmittel

    benutzt habe.

    Ferner erkläre ich, dass ich nicht anderweitig mit oder ohne Erfolg versucht habe,

    eine Dissertation einzureichen oder mich einer Doktorprüfung zu unterziehen.

    Köln, den 26. Dezember 2018

    ………………………………………….

    Dennis Berg

  • III

    Table of Content:

    List of Abbreviations: ................................................................................................. VI

    Acknowledgment ...................................................................................................... XII

    List of Publications................................................................................................... XIV

    Summary ................................................................................................................. XVI

    Zusammenfassung .................................................................................................. XIX

    Chapter 1: Introduction ................................................................................................ 1

    1.1 Introduction and Motivation .......................................................................................... 1

    1.2 Content of this Thesis .................................................................................................. 2

    1.3 Reference .................................................................................................................... 4

    Chapter 2: State-of-the-Art .......................................................................................... 5

    2.1 PET-Production............................................................................................................ 6

    2.1.1 Catalysts ............................................................................................................... 7

    2.1.2 Solid State Polycondensation Process .................................................................. 9

    2.1.3 Liquid State Polycondensation Process ................................................................13

    2.2 Recycling of Poly(ethylene terephthalate) ...................................................................14

    2.2.1 Thermal Recycling ................................................................................................14

    2.2.2 Chemical Recycling ..............................................................................................15

    2.2.3 Mechanical Recycling ...........................................................................................17

    2.3 Importance of the Molecular Weight of PET for its Application ....................................19

    2.4 Chain Extenders .........................................................................................................20

    2.4.1 1,3-Phenylene-bis-oxazoline (1,3-PBO) ................................................................21

    2.4.2 N,N’-Carbonylbiscaprolactam (CBC) ....................................................................23

    2.5 References .................................................................................................................24

    Chapter 3: Reasons for the Discoloration of Post-Consumer Poly(ethylene

    terephthalate) during Reprocessing ..................................................... 33

    3.1 Introduction .................................................................................................................34

    3.2 Experimental Section ..................................................................................................36

    3.2.1 Materials ...............................................................................................................36

    3.2.2 Heating of Antimony Oxide in Ethylene Glycol ......................................................37

    3.2.3 Sample Preparation ..............................................................................................37

    3.2.4 Characterization of PET Materials ........................................................................37

    3.3. Results and Discussion ..............................................................................................40

  • IV

    3.3.1 On the Graying of Poly(ethylene terephthalate) during Reprocessing ...................40

    3.3.2 Yellowing of Poly(ethylene terephthalate) during Reprocessing ............................46

    3.4 Conclusions ................................................................................................................59

    3.5 References .................................................................................................................60

    3.6 Supporting Information ................................................................................................63

    3.6.1 On the Graying of Poly(ethylene terephthalate) during Reprocessing ...................63

    3.6.2 Detection of Polyamides in Post-Consumer Poly(ethylene terephthalate) .............63

    3.6.3 MALDI-ToF-MS Analysis of Poly(ethylene terephthalate) Oligomers ....................68

    Chapter 4: Zinc Peroxide Particles as Bleaching Agents to Improve the Color of Post-

    Consumer Poly(ethylene terephthalate) .................................................. 69

    4.1 Introduction .................................................................................................................70

    4.2 Experimental Section ..................................................................................................73

    4.2.1 Materials ...............................................................................................................73

    4.2.2 Sample Preparation ..............................................................................................73

    4.2.3 Grinding of Commercial Zinc Peroxide .................................................................73

    4.2.4 Characterization of Zinc Peroxide Particles ..........................................................74

    4.2.5 Extrusion ..............................................................................................................74

    4.2.6 Characterization of PET Materials ........................................................................75

    4.3 Results and Discussion ...............................................................................................78

    4.3.1 Characterization of the Zinc Peroxide Particles ....................................................78

    4.3.2 Bleaching of Post-Consumer Poly(ethylene terephthalate) with Zinc Peroxide in the

    Extrusion Process .........................................................................................................81

    4.4 Conclusions ................................................................................................................99

    4.5 References ............................................................................................................... 100

    Chapter 5: Impact of the Chain Extension of Poly(ethylene terephthalate) with

    1,3-Phenylene-bis-oxazoline and N,N’-Carbonylbiscaprolactam by

    Reactive Extrusion on its Properties .................................................. 103

    5.1 Introduction ............................................................................................................... 104

    5.2 Experimental Section ................................................................................................ 107

    5.2.1 Materials ............................................................................................................. 107

    5.2.2 Extrusion ............................................................................................................ 108

    5.2.3 Viscosimetry ....................................................................................................... 108

    5.2.4 Size Exclusion Chromatography ......................................................................... 109

    5.2.5 Rheology ............................................................................................................ 109

    5.2.6 Differential Scanning Calorimetry .......................................