Quantitative determination of threading in rotaxanated polymers by diffusion-ordered NMR spectroscopy

被引:38
作者
Zhao, TJ
Beckham, HW [1 ]
Gibson, HW
机构
[1] Georgia Inst Technol, Sch Text & Fiber Engn, Polymer Educ & Res Ctr, Atlanta, GA 30332 USA
[2] Virginia Polytech Inst & State Univ, Dept Chem, Blacksburg, VA 24061 USA
关键词
D O I
10.1021/ma025959g
中图分类号
O63 [高分子化学(高聚物)];
学科分类号
070305 ; 080501 ; 081704 ;
摘要
Two-dimensional diffusion-ordered NMR spectroscopy (DOSY) was used to examine a rotaxanated polymer and its blends with unthreaded macrocycles. The threaded macrocycles exhibit self-diffusion coefficients similar to those of the polymer, while the diffusion coefficients for the unthreaded macrocycles are much larger. For poly[(styrene)-rotaxa-(30-crown-10)], the method provided definitive proof that the 30-crown-10 is threaded; for blends, the method allowed quantitative determination of the threaded-macrocycle fraction. The DOSY technique is particularly useful for those rotaxanated polymers in which weakly interacting macrocycle and polymer offer no other detectable spectroscopic signature. Threading can be proven, and the fraction of threaded macrocycles can be determined.
引用
收藏
页码:4833 / 4837
页数:5
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[11]   POLYROTAXANES - MOLECULAR COMPOSITES DERIVED BY PHYSICAL LINKAGE OF CYCLIC AND LINEAR SPECIES [J].
GIBSON, HW ;
MARAND, H .
ADVANCED MATERIALS, 1993, 5 (01) :11-21
[12]  
Gibson HW, 1996, LARGE RING MOLECULES, P191
[13]   Studies of the formation of poly(ester rotaxane)s from diacid chlorides, diols, and crown ethers and their properties [J].
Gibson, HW ;
Liu, S ;
Gong, CG ;
Ji, Q ;
Joseph, E .
MACROMOLECULES, 1997, 30 (13) :3711-3727
[14]   Polyrotaxanes by free-radical polymerization of acrylate and methacrylate monomers in the presence of a crown ether [J].
Gibson, HW ;
Bryant, WS ;
Lee, SH .
JOURNAL OF POLYMER SCIENCE PART A-POLYMER CHEMISTRY, 2001, 39 (12) :1978-1993
[15]   ROTAXANES, CATENANES, POLYROTAXANES, POLYCATENANES AND RELATED MATERIALS [J].
GIBSON, HW ;
BHEDA, MC ;
ENGEN, PT .
PROGRESS IN POLYMER SCIENCE, 1994, 19 (05) :843-945
[16]  
GOGN C, 1999, MOL CATENANES ROTAXE, P277
[17]   A strategy to eliminate dethreading during the preparation of poly(ester/crown ether rotaxane)s: Use of difunctional blocking groups [J].
Gong, CG ;
Ji, Q ;
Glass, TE ;
Gibson, HW .
MACROMOLECULES, 1997, 30 (17) :4807-4813
[18]   Main chain polyrotaxanes by threading crown ethers onto a preformed polyurethane: Preparation and properties [J].
Gong, CG ;
Ji, Q ;
Subramaniam, C ;
Gibson, HW .
MACROMOLECULES, 1998, 31 (06) :1814-1818
[19]   Synthesis and characterization of a polyester/crown ether rotaxane derived from a difunctional blocking group [J].
Gong, CG ;
Gibson, HW .
MACROMOLECULES, 1996, 29 (22) :7029-7033
[20]   The influence of polymer molecular-weight distributions on pulsed field gradient nuclear magnetic resonance self-diffusion experiments [J].
Håkansson, B ;
Nydén, M ;
Söderman, O .
COLLOID AND POLYMER SCIENCE, 2000, 278 (05) :399-405