Taking advantage of the DSC method, general procedures were presented for qualitative and quantitative evaluation of the phase separation degree and the crystalline phase content in polyurethane elastomers with well-defined structures. Those elastomers were obtained not only in a typical one-step method but also in the prepolymer method with the use of urethane oligomers with controlled molecular weight distribution (MWD). Prepolymers with well defined chain structures and narrow distributions of their molecular weights (MWD) M w /M n ¼ 1.1-1.3 were produced in a multistage method, i.e., in step-by-step polyaddition of 2,4-and 2,6-TDI with polyoxyethylenediols or with polycaprolactonediols of varied molecular weights. Isocyanate oligomers obtained at individual stages were then crosslinked with triethanolamine, whereas hydroxyl-terminated oligomers were crosslinked with 4,4 0 ,4 00 -triphenylmethane triisocyanate (Desmodur RE). The obtained polyurethane elastomers were found to be characterized by the presence of five phases: soft phase consisted of flexible polyol-type segments, crystalline phase made of soft segments, crystalline and amorphous hard phase made of hard segments, and intermediate phase, which was a composition of the soft and hard segments. The polyurethanes obtained out of prepolymers with defined MWD were characterized by better phase separation of the soft segments and increased structural order inside the hard phase as well as by better thermal stability than polyurethanes obtained from the typical one-step method. The structural effects were also discussed on the thermal properties of the synthesized elastomers as analyzed by the TG and DTA methods.
Using alicyclic diisocyanates (HDI, TMDI, IPDI, H 12 MDI), aliphatic unfluorinated and fluorinated alcohols, dibutyltin dilaurate as well as triethylamine as catalysts, blocked polyisocyanate crosslinkers for powder lacquers were synthesized. The chemical structure of these compounds was characterized by means of IR, 1 H-NMR, 13 C-NMR, and 19 F-NMR spectroscopy. Their molecular weight distribution parameters were determined by gel permeation chromatography. These blocked polyisocyanates were used for the production of powder lacquer compositions and coatings. The three-dimensional surface topography and surface chemical structure of the resulting powder lacquers were investigated by means of confocal microscope and ATR FT-IR. The values of surface roughness parameters were calculated.
With the use of alicyclic diisocyanates, aliphatic alcohols and dibutyltin dilaurate as well as triethylamine as a catalysts internally-blocked polyisocyanate crosslinkers which contained allophanate bonds were synthesized. The chemical structure of those compounds were characterized by IR, 1 H-NMR, and 13 C-NMR spectroscopy. Their molecular weight distribution (MWD) parameters were determined by gel permeation chromatography (GPC). Those blocked polyisocyanates were used for the production of ecological lacquer compositions and coatings. The unblocking and curing reactions were investigated on the DTA, TG, and DSC thermograms. The resulting powder lacquers exhibit an excellent appearance; they are transparent, smooth, and nonyellowing. V C 2010 Wiley Periodicals, Inc. J Appl Polym Sci 116: [3613][3614][3615][3616][3617][3618][3619][3620] 2010
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