以松香、乙醇胺为原料,盐酸为催化剂,乙醇为溶剂进行超声波强化胺盐法单离枞酸的研究。在胺化反应过程中,采用五因素四水平正交实验考察了反应温度、反应时间、超声功率、搅拌转速、溶剂浓度对枞酸单离收率和纯度的影响。实验结果表明,影响枞酸质量收率因素按显著程度依次为反应温度〉超声功率〉溶剂浓度〉搅拌转速〉反应时间。确定优化的胺化条件为:反应温度30℃、超声功率300W、溶剂浓度40%、搅拌转速400r·min^-1和反应时间40min,枞酸产品的收率和纯度分别为49.73%和98.42%。经气相色谱和圆盘旋光仪进行产品分析鉴定,实验值与文献值吻合。
The isolation of abietic acid by amine salt in combination with ultrasound wave was studied; during which, the rosin and ethanolamine, the HCI and the ethanol were used as raw materials, catalyst and solvent, respectively. The effects of reaction temperature, reaction time, ultrasound intensity used, agitating speed and solvent concentration on the yield and purity of abietic acid obtained in the process of aminating reaction were investigated by the orthogonal experiment L16 (4^5). The experimental results show that the significant degree sequences of the influential factors affecting the yield of abietic acid are as follows: reaction temperature 〉 ultrasound intensity 〉 solvent concentration 〉 agitating speed 〉 reaction time. The optimized aminating conditions obtained are as follows: reaction temperature of 30℃, ultrasound intensity of 300 W, solvent concentration of 40%, agitating speed of 400 r·min^-1 and reaction time of 40 min. Under above optimized reaction conditions, the yield and purity of the abietic acid obtained are 49.73% and 98.42%, respectively. The isolated abietic acid products were analyzed and identified with gas chromatography and disc polarimeter; the experimental values are in good agreement with the values in literatures.