Rf. Harris et al., SYNTHESIS AND CHARACTERIZATION OF UREA-BASED POLYUREAS .2. MORPHOLOGYCONTROL IN UREA-TERMINATED POLY(1,6-HEXAMETHYLENEUREA) PARTICLES, Polymer, 36(24), 1995, pp. 4683-4693
The effects of reaction parameters on the synthesis of urea-terminated
poly(1,6-hexamethyleneurea) particles dispersed in a polyol continuou
s phase have been studied. Oligomeric units are held together by hydro
gen bonding into a macrostructure which separates as a stable disperse
d phase during synthesis. Monomer addition rate, synthesis temperature
and stirring rate are important factors in morphology control of the
particles. High aspect ratio (10-20) particles having a spiral fibre b
undle morphology (by scanning electron microscopy) are produced at syn
thesis temperature between 140 and 175 degrees C; spherical particles
are produced at 185 degrees C. Particles produced at 140 degrees C hav
e a different crystalline structure from particles produced at higher
temperatures. Molecular weight, particle size and the extent of hydrog
en bonding increase with increasing synthesis temperature. The structu
re of these highly crystalline particles is established at an early st
age in the reaction, Annealing up to 185 degrees C has little effect o
n particle morphology. Annealing near the melting point (270 degrees C
) results in loss of crystallinity; particle macrostructure is destroy
ed by melting or dissolution.