Abstract

For extraction of higher fullerenes and endohedral metallofullerenes (EMF) with yttrium from fullerene-containing carbon soot (soot) obtained by combined spraying of graphite and yttrium oxide powders in an arc plasma, we developed a device (Extractor*) that provides mechanical activation effects on agents combined with filtration. It has been shown that the soot recovery percentage of a mixture of higher fullerenes and EMF with different solvents (carbon disulfide, o-xylene, pyridine) and the EMF mass fraction in the mixture is significantly higher than in the extraction with a Soxhlet apparatus traditionally used for these purposes. The time spent on the extraction process is reduced significantly. Due to a known reaction with titanium chloride (TiCl4) and removal of a solution of empty fullerenes, subsequent bonding of EMF with yttrium into an insoluble complex directly in the extractor allows the product to be significantly enriched with EMF. In general, we were able to significantly reduce both the duration of extraction of the fullerenes mixture and EMF and the production of EMF separately.

1. Highlights

2. A mechanical extractor (Extractor*) developed by us, which allows processing a larger amount of carbon black and, accordingly, extracting more fullerenes per unit of time, has been applied.

3. The percentage of extraction from the soot of a mixture of higher fullerenes and EMF with various solvents was significantly higher than with extraction using the Soxhlet apparatus.

4. It has been shown that mechanical extractor using makes it possible to increase the coefficient of mass transfer from the surface of the particles to the extracting agents.

5. The Extractor* was first used for the non-HPLC separation of endohedral metallofullerenes with TiCl4. The use of the new device made it possible to isolate a product significantly enriched in endohedral metallofullerenes.

摘要

为了从通过在电弧等离子体中组合喷涂石墨和氧化钇粉末获得的含富勒烯的碳烟灰（烟灰）中用钇萃取高级富勒烯和内嵌金属富勒烯 (EMF)，我们开发了一种设备（Extractor*），它提供机械活化效果上剂结合过滤。已经表明，高级富勒烯和 EMF 与不同溶剂（二硫化碳、邻二甲苯、吡啶）的混合物的碳烟回收率和混合物中的 EMF 质量分数显着高于传统的索氏装置萃取用于这些目的。提取过程所花费的时间显着减少。由于与氯化钛 (TiCl4) 的已知反应和空富勒烯溶液的去除，随后 EMF 与钇直接在萃取器中键合成不溶性复合物，使产品显着富含 EMF。一般来说，我们能够显着减少富勒烯混合物和 EMF 的提取持续时间以及 EMF 的产生。

1. 强调

2. 我们开发的机械萃取器（Extractor*）已被应用，它可以处理更多的炭黑，因此每单位时间可以萃取更多的富勒烯。

3. 用各种溶剂从高级富勒烯和 EMF 混合物的烟灰中提取的百分比显着高于使用索氏装置提取的百分比。

4. 已经表明，使用机械萃取器可以增加从颗粒表面到萃取剂的传质系数。

5. Extractor* 首次用于使用 TiCl4 对内嵌金属富勒烯进行非 HPLC 分离。新设备的使用使得分离富含内嵌金属富勒烯的产品成为可能。