重结晶-柱色谱联用法分离C_(60)研究

Efficient separation of fullerene C_(60) with the recrystallization-column chromatography method

为了提高粗富勒烯中C_(60)的分离效果,采用重结晶～柱色谱联用法从粗富勒烯中分离C_(60)。结果表明,以邻二甲苯为溶剂,80℃时重结晶分离1次,可得纯度为90%的C_(60),再以活性炭作单一固定相、甲苯为流动相,对结晶分离得到的、90%C_(60)进行柱色谱分离,当活性炭与富勒烯的质量比为9:1,色谱柱的高径比为10:1时,所得C_(60)的纯度和总回收率分别为99.9%、81%。

The paper is aimed at introducing the recrystallization-column chromatography method to the heightening of the performance of the purification between C60 and C70- We have done a series of efforts trying to separate C60 from the crude fullerenes by means of recrystal-lization-column chromatography combined technique in our study. In prnceeding with our research, the crude fullerenes soot extract samples were first of all put into a Stoppard Erlenmeyer flask with pure oxylene and then heat the whole solution to 80℃, while maintaining the state for four hours. Keep stirring the solution electromagnetically in the heating process, the deposit would be filtrated from the supernatant quickly with the solution kept warm. The obtained C6o could be enriched in the solid deposit by centrifugation and then sent for its purification of fullerenes to be tested by HPLC. The parity of the said C60 obtained as a result of the sedimentation can be made to reach 90% . And, then, it is possible to let the resulted highly purified C60 be treated by column chromatography, which can then use activated carbon as a single stationary phase and toluene as the mobile phase. Under the given condition, the C60 was made dissolved with the toluene under ultrasound again. The solution gained in this case could be let to pass through the column quickly with the final purple fraction collected and concentrated by evaporation. Thus, the pure C6o can be finally obtained. The experimental results from our research indicate that high purity and total recovery with the application of this method proves to be closely related with the mass of activated carbon and the dimension of the column. When the activated carbon and fullerene mass ratio reached a ration of 9 ： 1 with the ratio of height to diameter of the column up to 10：1, it would be possible to increase the final purity of C60 to 99.9 % while the total recovering rate could reach 81%. Compared with the simple recrystallization or column chromatography and any other methods, the method we have proposed enjoys its advantage in operation and nice splitting effect with a promising future in the mass separation.