PREPARATION OF FULLERENES BY INCOMPLETE

该项目的目的是改进通过烃类不完全燃烧制造富勒烯，特别是巴克敏斯特富勒烯C60的方法，以便在不久的将来可以通过连续方案大规模生产富勒烯。在项目的第一年，我们集中分析了商业烟灰产品中的富勒烯，希望获得燃料、燃烧温度、净化等条件。在检查了一些传统和现代的煤烟产品后，我们发现中国的墨棒和一些木炭不断地分析出巴克敏斯特富勒烯，有时也分析出C70。新的墨棒通常含有约0.1ppm的C60。这种水平的C60可以通过苯、环己烷和其他碳氢化合物在空气中的小火焰中的简单燃烧产生，并且也与在古老的地质物体中检测到的水平一致，例如来自K-T layr的黑色粘土，其被认为是来自野火 ...更多信息 是由火流星撞击造成的有趣的是，我们发现中国墨棒中C60的含量在几百年的时间内随时间减少，符合一级速率定律。我们解释的减少，而不是自发分解，但布朗型运动的球形和光滑的C60分子的微观结构中的墨棒。在第二年，我们进行了大量的燃烧试验，使用简单的自由燃烧装置，同时改变燃料和催化剂。尽管它们是初步的，但我们通过使用茂金属催化剂获得了两个令人鼓舞的结果：（1）添加催化量的二茂铁导致C60的产率增加高达500%，和（2）添加催化量的二茂镍和二茂钛降低了C60的产率，但在提取物的HPLC分析中产生了一个新的强峰，相对于C60的Rf值为0.65，其被认为是类似于霍华德等人曾经报道的中间体。作为这些初步实验的结果，我们设计了一个实验燃烧装置，其安全性高，可方便地用于寻找各种燃烧条件的催化剂。少

The purpose of this project is to improve the method of manufacturing fullerenes, especially buckminsterfullerene C60, by incomplete combustion of hydrocarbons, so that fullerenes can be produced in large scale by continuous scheme in the near future.In the first year of the project, we concentrated on the analysis of fullerenes in commercial soot products with the hope of obtaining clues for fuel, burning temperatures, purification and other conditions. After examining a number of traditional as well as modern products from soots, we found that Chinese ink sticks and some charcoals constantly analyzed positively for buckminsterfullerene and sometimes C70 as well. New ink sticks usually contain about 0.1ppm of C60. This level of C60 can be produced by simple burning of benzene, cyclohexane and other hydrocarbons in small flames in air and also agrees with the level detected in ancient geological objects like the black clay from K-T layr, which has been considered to arise from wildfire … More caused by bolide impact. Interestingly enough we found that the C60 contents in Chinese ink sticks decrease with time over a period of several hundred years conforming to the rate law of the first order. We interpret the decrease not by spontaneous decomposition but by Brownian type movements of spherical and smooth C60 molecules in the microstructure of ink sticks.In the second year, we performed numerous burning tests using simple free burning apparatus, while changing fuels and catalysts. Preliminary as they are, we obtained two encouraging results by using metallocene catalysts : (1) addition of catalytic amounts of ferrocence led to up to 500% increase in the yield of C60, and (2) addition of catalytic amounts of nickellocene and titanocene decreased the yields of 60, but produced a new intense peak in the HPLC analysis of the extract with Rf value of 0.65 relative to C60, which is supposed to be an intermediate similar to what was once reported by Howard et al.As the results of these preliminary experiments, we have designed an experimental burning apparatus, which is safe and can be conveniently used for seeking various burning conditions for searching catalysts. Less