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Block copolymers by combination of LAP and RAFT polymerization

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Title: Block copolymers by combination of LAP and RAFT polymerization


1
Block copolymers by combination of LAP and RAFT
polymerization
  • Wang Hui Fudan Univ. China
  • Ellen Donkers Lab of Polymer
    Chemistry, TU/e
  • Bert Klumperman the Netherlands

2
Background
  • Living anionic polymerization
  • ? Excellent control
  • ? Pure reactants
  • ? Strict reaction conditions
  • ? Limited range of monomers
  • (styrene, diene)
  • Elastomer PB, PI
  • Thermoplastic elastomer SBS

3
  • RAFT polymerization
  • ? Rather good control
  • ? Wide range of monomers
  • ? Wide range of operating conditions

4
Combination of LAP and RAFT
5
Model reaction with low MW RAFT agent
Styrenemaleic anhydride1M Reaction
temperature 85 ?C Initiator Vazo
88 RAFT/Vazo 8810 Solvent MEK/Toluene (1/2)
Linear increase of Mn with conversion Final
PDI1.16 Final conversion95
6
Chain extension of P(EB)-macro-RAFT
MWmacro-RAFT4000 g/mol Styrenemaleic
anhydride1M Reaction temperature 85
?C Initiator Vazo 88 RAFT/Vazo
8810 Solvent MEK/Toluene (2/1)
Predictable MW and linear increase of Mn with
conversion Final conversion93 PDI
macro-RAFT1.03 PDI final product1.15
7
Chain extension of P(B)-macro-RAFT
MWmacro-RAFT3500 g/mol Styrenemaleic
anhydride1M Reaction temperature 85
?C Initiator Vazo 88 RAFT/Vazo
8810 Solvent MEK/Toluene (2/1)
linear increase of Mn with conversion Final
conversion48 PDI macro-RAFT1.03 PDI final
product1.37 Cross-linking after long reaction
time
8
Chain extension of P(SB)-macro-RAFT
MWmacro-RAFT4000 g/mol MW styrene block2000
g/mol Styrenemaleic anhydride1M Reaction
temperature 85 ?C Initiator Vazo
88 RAFT/Vazo 8810 Solvent MEK/Toluene (2/1)
Linear increase of Mn with conversion Final
conversion89 PDI macro-RAFT1.07 PDI final
product1.57
9
Chain extension of P(SB)-macro-RAFT with rather
high MW
MWmacro-RAFT70000 g/mol MW styrene block60000
g/mol Styrenemaleic anhydride0.3M Reaction
temperature 85 ?C Initiator Vazo
88 RAFT/Vazo 885 Solvent MEK/Toluene
(1/1)
If MW of butadiene block is 60000, reaction was
stopped in 2 hours, due to the intensive
gelation.
10
Chain extension of P(SEP)-macro-RAFT with rather
high MW
DRI
UV-305nm
MWmacro-RAFT70000 g/mol, MW styrene block10000
g/mol Styrenemaleic anhydride1M Reaction
temperature 85 ?C Initiator Vazo 88,
RAFT/Vazo 885 Solvent MEK/Toluene (1/1)
11
Conclusion and discussion
  • ? Block copolymers were prepared by combination
    of LAP and RAFT polymerization, starting from
    different macro-RAFT agents without too high MW.
  • ? Double bonds had some influences on the
    polymerization in RAFT process. The higher
    content of PB block is, the sooner cross-linking
    will take place.

12
Conclusion and discussion
  • ? High viscosity does not effect the RAFT
    polymerization.

MWmacro-RAFT70000 g/mol MW styrene block60000
g/mol styrenemaleic anhydride1M RAFT/vazo
8810 Solvent MEK/toluene1 Reaction
temperature 85 ?C
13
Conclusion and discussion
  • ? Macro-RAFT agents with too high MW may act as
    inhibitor in RAFT polymerization.

14
Conclusion and discussion
  • ? Styrene homopolymerizatio gives less inhibition
    in chain extension of P(SEP)-RAFT agent with
    rather high MW.

DRI
UV-305nm
15
Conclusion and discussion
  • ? Reactive center-tertiary carbon radical may not
    work well in the RAFT polymerization.
  • New RAFT agent with a secondary living group
    has been synthesized and tested in the same way.

16
Future work and recommendations
  • ? The reaction conditions to be optimized.
  • ? Alternative way to be proposed.
  • Click Chemistry?

17
Acknowledgement
  • Prof. Daoyong Chen
  • Prof. Ming Jiang
  • Prof. Zhengzhong Shao
  • Department of Macromolecular Science
  • Fudan University
  • Ellen Donkers
  • Dr. Bert Klumperman
  • Prof. Cor Koning
  • Prof. P.J. Lemstra
  • Edgar Karssenberg
  • Eindhoven University of Technology
  • Dutch Polymer Institute

18
  • Thanks for your attention and time!

19
  • Questions???

20
A typical Route
21
Proposed Mechanism of RAFT
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