Differences of zirconocenes and hafnocenes: from low isotactic, elastic - to high isotacticity, high melting polypropylene
Gespeichert in:
| 1. Verfasser: | |
|---|---|
| Format: | Abschlussarbeit Buch |
| Sprache: | English |
| Veröffentlicht: |
München
Verl. Dr. Hut
2012
|
| Ausgabe: | 1. Aufl. |
| Schriftenreihe: | Makromolekulare Chemie
|
| Schlagworte: | |
| Online-Zugang: | Volltext https://nbn-resolving.org/urn:nbn:de:bvb:91-diss-20121106-1107885-0-8 Inhaltsverzeichnis |
| Beschreibung: | V, 197 S. Ill., graph. Darst. |
| ISBN: | 9783843907613 |
Internformat
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| 100 | 1 | |a Schöbel, Alexander |e Verfasser |4 aut | |
| 245 | 1 | 0 | |a Differences of zirconocenes and hafnocenes |b from low isotactic, elastic - to high isotacticity, high melting polypropylene |c Alexander Schöbel |
| 250 | |a 1. Aufl. | ||
| 264 | 1 | |a München |b Verl. Dr. Hut |c 2012 | |
| 300 | |a V, 197 S. |b Ill., graph. Darst. | ||
| 336 | |b txt |2 rdacontent | ||
| 337 | |b n |2 rdamedia | ||
| 338 | |b nc |2 rdacarrier | ||
| 490 | 0 | |a Makromolekulare Chemie | |
| 502 | |a München, Techn. Univ., Diss., 2012 | ||
| 650 | 0 | 7 | |a Zirkonocen |0 (DE-588)4190962-8 |2 gnd |9 rswk-swf |
| 650 | 0 | 7 | |a Hafnocen |0 (DE-588)4319832-6 |2 gnd |9 rswk-swf |
| 650 | 0 | 7 | |a Propen |0 (DE-588)4175940-0 |2 gnd |9 rswk-swf |
| 650 | 0 | 7 | |a Temperaturverhalten |0 (DE-588)4457534-8 |2 gnd |9 rswk-swf |
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Datensatz im Suchindex
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|---|---|
| adam_text | IMAGE 1
TABLE O F CONTENTS
1 INTRODUCTION 1
2 THEORETICAL BACKGROUND 3
2.1 DEFINITION OF METALLOCENES 3
2.2 A BRIEF HISTORY OF HOMOGENEOUS OLEFIN POLYMERIZATION CATALYSTS 3
2.3 IMPORTANT STRUCTURAL PARAMETERS OF ANSA- METALLOCENE COMPLEXES 4
2.4 ACTIVATION OF METALLOCENES 7
2.4.1 GENERAL ASPECTS 7
2.4.2 MAO ACTIVATION 7
2.4.3 BORON-BASED ACTIVATION 8
2.4.4 ACTIVATION INVESTIGATIONS VIA UV-VIS SPECTROSCOPY 10
2.4.5 H F AND ZR. THE DIFFERENCE IN ACTIVATION/ACTIVITY 11
2.5 CHAIN PROPAGATION MECHANISM IN THE COORDINATION-INSERTION
POLYMERIZATION OF
A-OLEFINS WITH METALLOCENES 13
2.6 STEREO AND REGIOCHEMISTRY IN METALLOCENE-BASED A-OLEFIN
POLYMERIZATION 14
2.6.1 STEREO AND REGIOCONTROL IN THE HOMOGENEOUS POLYMERIZATION O F
PROPENE TO IPP. 14 2.6.2 H F AND ZR: THE DIFFERENCE IN REGIO- AND
STEREOCONTROL 18
2.7 CHAIN RELEASE REACTIONS 18
2.7.1 P-HYDRIDE TRANSFER 18
2.7.1.1 P-HYDRIDE TRANSFER TO THE METAL 19
2.7.1.2 P-HYDRIDE TRANSFER TO THE MONOMER 19
2.7.2 P-METHYL TRANSFER 21
2.7.3 CHAIN TRANSFER TO ALUMINUM AND OTHER TRANSFER AGENTS 22
2.7.4 H F AND ZR: THE DIFFERENCE IN TRANSFER REACTIONS 23
2.8 COMPLEX- AND POLYMER STRUCTURE CORRELATION 24
2.9 ELASTIC POLYPROPYLENE 26
2.9.1 DIFFERENT WAYS FOR THE PRODUCTION O F ELASTIC PP 27
2.9.2 RIEGER S CI-SYMMETRIC METALLOCENES AND THE INFLUENCE O F THE
CO-CATALYST ON THE MICROSTRUCTURE 31
2.9.3 H F AND ZR: THE DIFFERENCE IN THE FORMATION O F EPP 32
2.10 HIGH MELTING ISOTACTIC POLYPROPYLENE 33
2.10.1 STATE O F THE ART ZIEGLER-NATTA CATALYSTS 34
2.10.2 STATE O F THE ART HOMOGENEOUS METALLOCENES 36
2.10.2.1 INDENYL-BASED METALLOCENES WITH 2-SUBSTITUTION PATTERN 36
2.10.2.2 INDENYL-BASED METALLOCENES WITH 2,4-SUBSTITUTION PATTERN 37
2.10.2.3 INDENYL-BASED METALLOCENES WITH 2,4,7-SUBSTITUTION PATTERN 40
2.10.2.1 HETEROATOM-SUBSTITUTED INDENYL-BASED METALLOCENES 43
III
HTTP://D-NB.INFO/1028927711
IMAGE 2
TABLE OF CONTENTS
3 CONCEPT OF THIS WORK 45
4 RESULTS AND DISCUSSION 49
4.1 CI-SYMMETRIC METALLOCENES FOR THE FORMATION OF EPP 49
4.1.1 TEMPERATURE STABILITY O F THE CATALYST 49
4.1.2 PREACTIVATION WITH TIBA: UV-VIS AND NMR MEASUREMENTS 52
4.1.3 INFLUENCE O F POLYMERIZATION TEMPERATURE ON MOLECULAR WEIGHTS O F
PRODUCED EPPS 62
4.1.4 CHAIN TRANSFER REACTIONS TO THE CO-CATALYST 63
4.1.5 TRANSFER REACTIONS: THE DIFFERENCE BETWEEN ZR AND H F 65
4.1.6 POSTULATED TRANSFER MECHANISM: THE DIFFERENCE BETWEEN ZR AND H F
71 4.1.7 MODIFICATION O F LIGAND STRUCTURE O F THE CI-SYMMETRIC
COMPLEXES FOR A SUPPRESSION O F TRANSFER REACTIONS 73
4.1.8 LONG-CHAIN-BRANCHED (LCB) EPP 76
4.1.9 FORMATION O F PP MACROMONOMERS AND THEIR COPOLYMERIZATION WITH
ETHENE 80
4.2 C 2-SYMMETRIC METALLOCENES FOR THE FORMATION OF EPP 83
4.3 C2-SYMMETRIC METALLOCENES FOR THE FORMATION OF IPP 86
4.3.1 SYNTHESIS O F BIS(7-ALKOXY-4-ARYL-2-METHYLINDENYL)DIMETHYL SILANE
FROM 4-ARYLPHENOL AND METHACRYLOYLCHLORIDE 86
4.3.1.1 7-HYDROXY-2-METHYL-4-PHENY!INDANONE (13) 87
4.3.1.2 4-METHOXY-2-METHYL-7-PHENYLINDENE (15) 88
4.3.1.3 BIS(7-METHOXY-2-METHYL-4-PHENYLINDENE)DIMETHYL SILANE (16) 89
4.3.2 SYNTHESIS O F BIS(7-ALKOXY-4-ARYL-2-METHYLINDENYL)DIMETHYL SILANE
FROM 4-BROMOPHENOL AND METHACRYLOYLCHLORIDE 91
4.3.2.1 4-BROMO-7-HYDROXY-2-METHYLINDANONE (19) 92
4.3.2.2 7-BROMO-4-METHOXY-2-METHYLINDE (21) 93
4.3.2.3 4-AIYL-7-METHOXY-2-METHYLINDENES VIA C-C COUPLING REACTION 93
4.3.2.4 SYNTHESIS O F SIME2 -BRIDGED LIGANDS 95
4.3.3 SYNTHESIS O F
BIS[4-(3 ,5 -DI-TERT-BUTYLPHENYL)-2-METHYLINDENYL)DIMETHYL SILANE (33)
FROM L-BROMO-2-(BROMOMETHYL)BENZENE 96
4.3.4 COMPLEX SYNTHESIS AND CRYSTAL STRUCTURES 97
4.3.4.1 SYNTHESIS O F ZIRCONOCENE 34 AND HAFTIOCENE 35 FROM
BIS[4-(3 ,5 -DI-/ERTBUTYLPHENYL)-7-METHOXY-2-METHYLINDENYL]DIMETHYL
SILANE 97 4.3.4.2 SYNTHESIS O F HAFNOCENE 36 FROM
BIS[4-(3 ,5 -DI-/ERT-BUTYLPHENYL)-2METHYLINDENYL]DIMETHYL SILANE 98
4.3.4.3 COMPARISON O F CRYSTAL STRUCTURES O F RAC-34-36 98
4.3.5 SOLUTION POLYMERIZATION O F PROPENE WITH RAC-34-36 101
4.3.5.1 PRODUCTIVITY O F COMPLEXES RAC-34-36 104
4.3.5.2 DETERMINATION O F STEREO- AND REGIOREGULARITY VIA 13C NMR
SPECTROSCOPY 105
IV
IMAGE 3
TABLE O F CONTENTS
4.3.5.3 COMPARISON O F STEREO- AND REGIOREGULARITY O F IPP PRODUCED WITH
COMPLEXES
RAC-34-36 AND LITERATURE-KNOWN CATALYSTS 106
4.3.5.4 INFLUENCE O F PROPENE CONCENTRATION ON MOLECULAR WEIGHT AND
MICROSTRUCTURE O F IPP PRODUCED BY METALLOCENES RAC-34-36 109
4.3.6 STABILITY, MELTING, CRYSTALLIZATION, AND MECHANICAL PROPERTIES O F
THE HIGHLY REGIO- AND ISOSPECIFIC PP 112
4.3.6.1 STABILITY O F THE HIGHLY REGIO- AND ISOSPECIFIC PP 112
4.3.6.2 ANNEALING EXPERIMENTS 114
4.3.6.3 MECHANICAL INVESTIGATIONS 116
5 SUMMARY 119
6 ZUSAMMENFASSUNG... .... ....... 12S
7 EXPERIMENTAL PART 131
7.1 GENERAL PROCEDURES 131
7.2 UV-VIS INVESTIGATIONS 139
7 3 NMR INVESTIGATIONS 140
7.4 POLYMERIZATION PROCEDURE 140
7.5 LIGAND SYNTHESIS 143
7.5.1 L-(9-FLUORENYL)-2-(5,6-CYCLOPENTYL-2-PHENYL-L-INDENDYL)-ETHANE 143
7.5.2 BIS(7-AIKOXY-4-ARYL-2-METHYLINDENYL)DIMETHYL SILANE 149
7.5.3 BIS(4-ARYL-2-METHYLINDENYL)DIMETHYL SILANE 171
7.6 COMPLEX SYNTHESIS 174
7.6.1 I?AC-DIINETHYLSILANEDIYLBIS(2-METHYL-L-BENZ[E]INDENYL) HAFNIUM
DICHLORIDE (10) 174 7.6.2 /?AC-DIMETHYLSILANEDIYLBIS[4-(3 ,5
-DI-FERT-BUTYLPHENYL) -7-METHOXY-2METHYLINDENYL]ZIRCOMUM DICHLORIDE
(34) 175
7.6.3 /?AC-DIMETHYLSILANEDIYLBIS[4-(3 ,5 -DI-FERT-BUTYLPHENYL)-
7-METHOXY-2METHYLINDENYL]HAFHIUM DICHLORIDE (35) 176
7.6.4 /?AC-DIMETHYLSILANEDIYLBIS[4-(3 ,5
-DI-/ER/-BUTYLPHENYL)-2-METHYLINDENYL]HAFNIUM DICHLORIDE (36) 178
8 LITERATURE 183
V
|
| any_adam_object | 1 |
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| edition | 1. Aufl. |
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| record_format | marc |
| series2 | Makromolekulare Chemie |
| spelling | Schöbel, Alexander Verfasser aut Differences of zirconocenes and hafnocenes from low isotactic, elastic - to high isotacticity, high melting polypropylene Alexander Schöbel 1. Aufl. München Verl. Dr. Hut 2012 V, 197 S. Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier Makromolekulare Chemie München, Techn. Univ., Diss., 2012 Zirkonocen (DE-588)4190962-8 gnd rswk-swf Hafnocen (DE-588)4319832-6 gnd rswk-swf Propen (DE-588)4175940-0 gnd rswk-swf Temperaturverhalten (DE-588)4457534-8 gnd rswk-swf Katalysator (DE-588)4029919-3 gnd rswk-swf Polymerisation (DE-588)4046704-1 gnd rswk-swf (DE-588)4113937-9 Hochschulschrift gnd-content Zirkonocen (DE-588)4190962-8 s Hafnocen (DE-588)4319832-6 s Katalysator (DE-588)4029919-3 s Polymerisation (DE-588)4046704-1 s Propen (DE-588)4175940-0 s Temperaturverhalten (DE-588)4457534-8 s DE-604 Erscheint auch als Online-Ausgabe urn:nbn:de:bvb:91-diss-20121106-1107885-0-8 http://mediatum.ub.tum.de/node?id=1107885 Verlag kostenfrei Volltext https://nbn-resolving.org/urn:nbn:de:bvb:91-diss-20121106-1107885-0-8 Resolving-System DNB Datenaustausch application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=025692130&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
| spellingShingle | Schöbel, Alexander Differences of zirconocenes and hafnocenes from low isotactic, elastic - to high isotacticity, high melting polypropylene Zirkonocen (DE-588)4190962-8 gnd Hafnocen (DE-588)4319832-6 gnd Propen (DE-588)4175940-0 gnd Temperaturverhalten (DE-588)4457534-8 gnd Katalysator (DE-588)4029919-3 gnd Polymerisation (DE-588)4046704-1 gnd |
| subject_GND | (DE-588)4190962-8 (DE-588)4319832-6 (DE-588)4175940-0 (DE-588)4457534-8 (DE-588)4029919-3 (DE-588)4046704-1 (DE-588)4113937-9 |
| title | Differences of zirconocenes and hafnocenes from low isotactic, elastic - to high isotacticity, high melting polypropylene |
| title_auth | Differences of zirconocenes and hafnocenes from low isotactic, elastic - to high isotacticity, high melting polypropylene |
| title_exact_search | Differences of zirconocenes and hafnocenes from low isotactic, elastic - to high isotacticity, high melting polypropylene |
| title_full | Differences of zirconocenes and hafnocenes from low isotactic, elastic - to high isotacticity, high melting polypropylene Alexander Schöbel |
| title_fullStr | Differences of zirconocenes and hafnocenes from low isotactic, elastic - to high isotacticity, high melting polypropylene Alexander Schöbel |
| title_full_unstemmed | Differences of zirconocenes and hafnocenes from low isotactic, elastic - to high isotacticity, high melting polypropylene Alexander Schöbel |
| title_short | Differences of zirconocenes and hafnocenes |
| title_sort | differences of zirconocenes and hafnocenes from low isotactic elastic to high isotacticity high melting polypropylene |
| title_sub | from low isotactic, elastic - to high isotacticity, high melting polypropylene |
| topic | Zirkonocen (DE-588)4190962-8 gnd Hafnocen (DE-588)4319832-6 gnd Propen (DE-588)4175940-0 gnd Temperaturverhalten (DE-588)4457534-8 gnd Katalysator (DE-588)4029919-3 gnd Polymerisation (DE-588)4046704-1 gnd |
| topic_facet | Zirkonocen Hafnocen Propen Temperaturverhalten Katalysator Polymerisation Hochschulschrift |
| url | http://mediatum.ub.tum.de/node?id=1107885 https://nbn-resolving.org/urn:nbn:de:bvb:91-diss-20121106-1107885-0-8 http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=025692130&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| work_keys_str_mv | AT schobelalexander differencesofzirconocenesandhafnocenesfromlowisotacticelastictohighisotacticityhighmeltingpolypropylene |