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Reverse atom transfer radical polymerisation (RATRP) of methacrylates using copper(I)/pyridinimine catalysts in conjunction with AIBN
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UNSPECIFIED (2006) Reverse atom transfer radical polymerisation (RATRP) of methacrylates using copper(I)/pyridinimine catalysts in conjunction with AIBN. EUROPEAN POLYMER JOURNAL, 42 (1). pp. 61-68. doi:10.1016/j.eurpolymj.2005.08.011 ISSN 0014-3057.
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Official URL: http://dx.doi.org/10.1016/j.eurpolymj.2005.08.011
Abstract
N-n-Propyl-2-pyridylmethanimine, 1, N-n-octyl-2-pyridylmethanimine, 2, N-n-lauryl-2-pyridylmethanimine, 3, and N-n-octadecyl-2-pyridlmethanimine, 4 have been used in conjunction with copper(II) bromide and azo initiators for the reverse atom transfer radical polymerisation of a range of methacrylates. AIBN to (CuBr2)-Br-II ratios of 0.5:1, 0.75:1 and 1:1 give PMMA with M-n 11500 g mol(-1) (PDi = 1.24) (at 22% conversion), 12 500 g mol(-1) (PDi = 1.06) (at 83% conversion) and 10 900 g mol(-1) (PDi = 1.11) (at 84% conversion), respectively. A (CuBr2)-Br-II complex is demonstrated to be needed at the start of the reaction for good control over molecular weight and polydispersity as reactions using Cu(I)Br as catalyst yielded PMMA of M-n 31000 g mol(-1) (PDi = 2.90), reactions with no copper yield PMMA of M-n 33 000 g mol(-1) (PDi = 2.95). The RATRP of styrene was carried out using (CuBr2)-Br-II as catalyst. AIBN to (CuBr2)-Br-II ratio of 0.5:1, 0.75:1 and 1:1 gave PS with M-n = 12400 g mol(-1) (PDi = 1.27) at low conversion, M-n = 15500 g mol(-1) (PDi = 1.11) and 12400 g mol(-1) (PDi = 1.38), respectively at similar to 85% conversion. A series of block copolymers of MMA with BMA, BzMA and DMEAMA (15600 g mol(-1) (PDi = 1.18), 13300 g mol(-1) (PDi = 1.14) 15300 g mol(-1) (PDi) = 1.16), using a PMMA macroinitiator were prepared. Emulsion polymerisation of MMA using [initiator]: [(CuBr2)-Br-(II)] ratio = 0.5:1 with Brij surfactant gave a linear increase of Mn with respect to conversion, final M,, = 112800 g mol(-1) (PDi = 1.42). Further reactions were carried out with [initiator]:[(CuBr)-Br-(II),] ratio = 0.75:1 and 1:1. Both giving PMMA with M-n similar to 32000 g mol(-1) (PDi similar to 2.4). These reactions exhibit no control, this is because the azo initiator is present in excess and all of the monomer is consumed by a free radical polymerisation as opposed to a controlled reaction. Particle size analysis (DLS) showed the particle size between 160 and 170 nm in all cases. (c) 2005 Published by Elsevier Ltd.
Item Type: | Journal Article | ||||
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Subjects: | Q Science > QD Chemistry | ||||
Journal or Publication Title: | EUROPEAN POLYMER JOURNAL | ||||
Publisher: | PERGAMON-ELSEVIER SCIENCE LTD | ||||
ISSN: | 0014-3057 | ||||
Official Date: | January 2006 | ||||
Dates: |
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Volume: | 42 | ||||
Number: | 1 | ||||
Number of Pages: | 8 | ||||
Page Range: | pp. 61-68 | ||||
DOI: | 10.1016/j.eurpolymj.2005.08.011 | ||||
Publication Status: | Published |
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