The preparation of 2-aminoethanol salt of dehydroabietic acid from disproportionated rosin by reaction-crystallization coupled with ultrasound wave was studied by using disproportionated rosin and 2-aminoethanol as raw materials
ethanol as reaction solvent
and pure dehydroabietic acid could be obtained by extraction
crystallization
recrystallization and acidification.The effects of concentration of ethanol
reaction temperature
reaction time
ultrasound intensity and agitating velocity on the yield of dehydroabietic acid were investigated by orthogonal experiment
and the optimal conditions for isolation were obtained as follows: reaction time 50 min
reaction temperature 35℃
ultrasound power 500 W
concentration of ethanol 50%
agitating velocity 400 r8226;min-1.Under these conditions
the yield of dehydroabietic acid was 55.37%
and the purity was 99.53%.At the same time
the effect of the conversion of phase state during the aminating reaction-crystallization on the chemical equilibrium and selectivity was investigated.When reaction temperatures were 35℃ and 70℃
respectively
the reaction was heterogeneous and homogeneous
and the purities of dehydroabietic acid prepared were 99.53% and 95.66%.The dehydroabietic acid prepared was analyzed and confirmed with GC
GC-MS
elemental analysis
UV
FT-IR
melting point instrument and polarimeter as well
and the results were in good agreement with the values in literature.