CAJ | 학술논문

为提高枞酸的纯度和收率,以松香为原料,乙醇为溶剂,利用微波强化松香异构和胺化反应-结晶耦合的方法单离枞酸,通过单因素和正交试验考察酸种类、微波功率、温度、时间和原料配比对枞酸提纯的影响。结果表明,微波强化松香异构反应的最优条件是：异构反应催化剂为盐酸、微波功率为500 W、反应温度为40℃、反应时间为30 min；胺化反应的温度为35℃、反应时间为25 min、原料配比( n松香：n乙醇胺)为1：1,此条件下单离得到枞酸的纯度和收率分别为98.60%及57.47%。微波强化胺盐法降低了反应温度,实现反应与结晶分离的耦合,提高了枞酸纯度和收率。
위제고종산적순도화수솔,이송향위원료,을순위용제,이용미파강화송향이구화알화반응-결정우합적방법단리종산,통과단인소화정교시험고찰산충류、미파공솔、온도、시간화원료배비대종산제순적영향。결과표명,미파강화송향이구반응적최우조건시：이구반응최화제위염산、미파공솔위500 W、반응온도위40℃、반응시간위30 min；알화반응적온도위35℃、반응시간위25 min、원료배비( n송향：n을순알)위1：1,차조건하단리득도종산적순도화수솔분별위98.60%급57.47%。미파강화알염법강저료반응온도,실현반응여결정분리적우합,제고료종산순도화수솔。
In order to obtain abietic acid with high purity and high yield , abietic acid isolation was studied using rosin isomerization coupling amination reaction and crystallization with rosin as raw ma-terial and ethanol as solvent under mircrowave irradiation. The effects of acids, power of microwave, reaction temperature and time, and material proportion on the purification of abietic acid were inves-tigated by single factor and orthogonal experiments. The result showed that the optimal reaction con-ditions of rosin isomerization under mircrowave irradiation were as follows:hydrochloric acid as cata-lyst, microwave power 500 W, reaction temperature 40 ℃, and reaction time 30min. The optimal reaction conditions of amination were obtained as follows:reaction temperature 35 ℃, reaction time 25min and material proportion 1:1. Under above reaction conditions, the purity of abietic acid ob-tained could reach 98.60% with a yield of 57.47%. The isolation of abietic acid by microwave-as-sisted amine salt method is benefited by reducing the reaction temperature, achieving the coupling of reaction and crystallization separation, and increasing the purity and yield of abietic acid.