【摘要】 以歧化松香和2-乙醇胺为原料,采用超声波强化的方法进行反应-结晶耦合单离脱氢枞酸过程研究。考察了反应时间、反应温度、超声波强度、溶剂浓度、搅拌转速、胺盐结晶溶剂浓度、重结晶次数及结晶方式对脱氢枞酸收率的影响,实验结果表明,超声波可以有效地强化歧化松香胺化反应-结晶过程,适宜的反应时间为40min、反应温度为35℃、超声波功率为300W、溶剂浓度为40%、搅拌转速为300r·min-1、胺盐结晶溶剂浓度为40%、胺盐重结晶次数为2~3次、结晶方式为自然结晶,所制得的脱氢枞酸收率为48.59%,纯度为99.28%。并对脱氢枞酸单离过程的收率、纯度和损失率进行了跟踪分析,其中胺化反应-结晶过程脱氢枞酸产品的损失率最大,其次是溶剂萃取过程,二者损失率分别为36.12%和10.94%。更多还原

【Abstract】 Using disproportionated rosin and 2-aminoethanol as raw material and ethanol as reaction solvent, the isolation of dehydroabietic acid from disproportionated rosin by the reaction-crystallization strengthened by ultrasonic wave was studied. The effects of reaction time, reaction temperature, ultrasound intensity, concentration of reaction solvent, agitating speed, concentration of solvent for amine salt crystallization, times of recrystallization and means of crystallization on the yield of dehydroabietic acid were investigated. The experimental results show that the ultrasound wave can effectively strengthen aminating reaction-crystallization of disproportionated rosin, and the appropriate operation conditions found are reaction time of 40 min, reaction temperature of 35℃, ultrasound power of 300 W, reaction solvent concentration of 40%, agitating speed of 300 r·min-1, crystallization solvent concentration of 40%, using spontaneous nucleation crystallization and recrystallization of 2~3 times. The yield of dehydroabietic acid prepared can reach 48.59% with purity of 99.28%. Moreover, the tracking analysis of the yield, purity and loss ratio of dehydroabietic acid was carried out for each process which composing the whole isolation process of dehydroabietic acid, such as the processes of aminating reaction-crystallization, solvent liquid-liquid extraction, first time recrystallization, second time recrystallization and third time recrystallization, and it was found that the aminating reaction-crystallization process has the biggest loss ratio of dehydroabietic acid, which is 36.12%, and the solvent extraction process has the next biggest loss ratio of 10.94%.更多还原