PURIFICATION OF C-60 AND C-70 BY SELECTIVE COMPLEXATION WITH CALIXARENES

PURIFICATION OF C-60 AND C-70 BY SELECTIVE COMPLEXATION WITH CALIXARENES
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DOI:
10.1038/368229a0
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发表时间:
1994-03-17
期刊:
影响因子:
64.8
通讯作者:
RASTON, CL
RASTON, CL
中科院分区:
综合性期刊1区
文献类型:
--
作者:
ATWOOD, JL;KOUTSANTONIS, GA;RASTON, CL

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富勒烯在主客体复合物中的分子络合具有提供富勒烯的有效大规模纯化的潜力(1)。这种方法将避免目前使用的色谱技术中固有的损失,这些损失是由固定相上的不可逆吸收引起的(2)。已经报道了C-60的几种主体-客体相互作用,包括与1,4-氢醌(3,4)、氮杂冠化合物(5)、某些水溶性大环如γ-环糊精(6-8)形成络合物,以及C-60与铱膦之间的络合,其中连接到磷原子的侧基形成相邻C-60分子的摇篮(9)。其他相关研究包括将C-60纳入微孔磷酸铝(10)和在C-60和硫富瓦烯之间形成电荷转移络合物(11)。在这里,我们表明,C-60和C-70将与杯芳烃形成离散的复合物,具有疏水空腔的Howl-shaped大环。p-Bu '-杯[8]芳烃与“粗”富勒烯烟灰的甲苯提取物的混合物的络合,随后进行一系列重结晶,得到>99.5%纯度的C-60。我们的方法可以大大降低纯化C-60和C-70的成本。
MOLECULAR complexation of fullerenes in host-guest complexes has the potential to afford efficient large-scale purification of fullerenes(1). This method would avoid the losses inherent in the chromatographic techniques currently in use, which arise from irreversible absorption on the stationary phase(2). Several host-guest interactions have been reported for C-60, including the formation of complexes with 1,4-hydroquinone(3,4), azacrown compounds(5), certain water-soluble macrocycles such as gamma-cyclodextrin(6-8), and complexation between C-60 and an iridium phosphine in which pendant groups attached to a phosphorus atom form a cradle for an adjacent C-60 molecule(9). Other relevant studies are the inclusion of C-60 into a microporous aluminophosphate(10) and the formation of a charge-transfer complex between C-60 and a thiafulvalene(11). Here we show that both C-60 and C-70 Will form discrete complexes with calixarenes, howl-shaped macrocycles with hydrophobic cavities. Complexation of p-Bu'-calix[8]arene with a mixture of the toluene extract of 'crude' fullerene soot, followed by a series of recrystallizations, affords >99.5% pure C-60. Our approach could lead to a substantial reduction in the cost of purifying C-60 and C-70.