C-13 AND N-15 CP/MAS NMR CHARACTERIZATION OF MDI-POLYISOCYANURATE RESIN SYSTEMS

被引:33
作者
DUFF, DW [1 ]
MACIEL, GE [1 ]
机构
[1] COLORADO STATE UNIV,DEPT CHEM,FT COLLINS,CO 80523
关键词
D O I
10.1021/ma00214a008
中图分类号
O63 [高分子化学(高聚物)];
学科分类号
070305 ; 080501 ; 081704 ;
摘要
A series of MDI-polyisocyanurate resins were prepared under a variety of reaction conditions from 4,4′-methylenebis(phenylisocyanate) (MDI) and from15N-enriched MDI, using stannous octoate as catalyst. The formation of cross-links via isocyanurate ring formation and the fate of the unreacted isocyanate were monitored by both13C and15N CP/MAS NMR methods, and an optimal cure temperature of ca. 120 °C was determined for this particular system. Urea linkages and other less predominant structures such as amine, biuret, and uretidione were clearly identified by15N CP/MAS. The ability of15N CP/MAS to yield quantitative results on the extent of cross-linking is demonstrated.15N CP/MAS proves to be a powerful technique for structure elucidation in these complex macromolecular systems. © 1990, American Chemical Society. All rights reserved.
引用
收藏
页码:3069 / 3079
页数:11
相关论文
共 46 条
[1]  
ALLA M, 1978, JETP LETT, V27, P208
[2]   RECENT ADVANCES IN ISOCYANATE CHEMISTRY [J].
ARNOLD, RG ;
NELSON, JA ;
VERBANC, JJ .
CHEMICAL REVIEWS, 1957, 57 (01) :47-76
[3]  
BARIKANI M, 1986, CELL POLYM, V5, P169
[4]   A MAGIC-ANGLE SPINNING SYSTEM FOR BULLET-TYPE ROTORS IN ELECTROMAGNETS [J].
BARTUSKA, VJ ;
MACIEL, GE .
JOURNAL OF MAGNETIC RESONANCE, 1981, 42 (02) :312-321
[5]  
Britain J. W., 1960, J APPL POLYM SCI, V4, P207
[6]  
BRYSON RL, 1983, MACROMOLECULES, V16, P1669, DOI 10.1021/ma00244a021
[7]   CHARACTERIZATION OF POLYURETHANE ELASTOMERS BY C-13 NMR-SPECTROSCOPY [J].
DELIDES, C ;
PETHRICK, RA ;
CUNLIFFE, AV ;
KLEIN, PG .
POLYMER, 1981, 22 (09) :1205-1210
[8]  
DIXON WT, 1981, J MAGN RESON, V44, P220, DOI 10.1016/0022-2364(81)90206-7
[9]  
EDWARDS KN, 1981, URETHANE CHEM APPLIC
[10]   C-13 SUBSTITUENT EFFECTS IN MONOSUBSTITUTED BENZENES [J].
EWING, DF .
ORGANIC MAGNETIC RESONANCE, 1979, 12 (09) :499-524