CAJ | 학술논문

为开发多级逆流微萃取系统，实现稳定逆流操作，研究液-液两相在此系统中的传质规律，以及探索传质性能的最优化操作条件。以双向四缸往复泵和四个缓冲室通过单向阀与料液罐相连，构成脉冲进料出料系统，以单向阀控制两相单向流动，实现微萃取系统的逆流操作；以30%(v/v)TBP-煤油/水体系为研究对象，选择硝酸为待萃取物，以平行并列微通道为微萃取设备，进行单级微萃取实验，研究脉冲频率、脉冲体积、浓度等操作条件对传质性能的影响；在此基础上，进行四级逆流微萃取的研究，总结出最优化操作条件。结果表明，在两相脉冲冲程均为80μL，脉冲频率为0.13 Hz时，单级微萃取的萃取级效率达到最大；在四级逆流微萃取系统中，总萃取效率超过90%。
위개발다급역류미췌취계통，실현은정역류조작，연구액-액량상재차계통중적전질규률，이급탐색전질성능적최우화조작조건。이쌍향사항왕복빙화사개완충실통과단향벌여료액관상련，구성맥충진료출료계통，이단향벌공제량상단향류동，실현미췌취계통적역류조작；이30%(v/v)TBP-매유/수체계위연구대상，선택초산위대췌취물，이평행병렬미통도위미췌취설비，진행단급미췌취실험，연구맥충빈솔、맥충체적、농도등조작조건대전질성능적영향；재차기출상，진행사급역류미췌취적연구，총결출최우화조작조건。결과표명，재량상맥충충정균위80μL，맥충빈솔위0.13 Hz시，단급미췌취적췌취급효솔체도최대；재사급역류미췌취계통중，총췌취효솔초과90%。
The purpose of this work is to develop a multi-stage countercurrent micro-extraction system to achieve stable operation of countercurrent flow, and investigate liquid-liquid mass transfer performance. The countercurrent flow was achieved by using a pulse feeding discharging system and a one-way control system. The pulse feeding discharging system was composed of a reciprocating pump with four pistons moving at opposite directions, and four chambers connected with the material vessels by check valves. The single-stage extraction performance was first investigated in a multi-channel micro-extraction device with 30%TBP-kerosene / water- nitric acid as the liquid-liquid extraction system. The effect of operation conditions including pulse frequency, pulse volume and concentration on the mass transfer performance was investigated, and then the extraction performance of the four-stage micro-extraction system was tested. Optimal operation conditions were finally obtained. The highest extraction efficiency of the single-stage extraction is achieved when the pulse frequency is at 0.13Hz, with the pulse stroke of both phases at 80μL. The total extraction efficiency of the four-stage micro-extraction system is higher than 90%in all experiments.