柱色谱法批量分离N-甲基-2-(3-硝基苯基)吡咯烷[3’,4’:1,2][60]富勒烯研究

经C60、N-甲基甘氨酸和间硝基苯甲醛反应得到N-甲基-2-(3-硝基苯基)吡咯烷[3′,4′∶1,2][60]富勒烯(MNPF)反应液,旋转蒸发干燥得质量分数为23%的MNPF粗品,采用柱色谱法批量分离其中的MNPF。确定了柱色谱法批量分离MNPF的最佳工艺条件:二硫化碳为流动相,柱层析用硅胶(37~48μm)为固定相,色谱柱直径5cm,高径比为6∶1,最大上样量为23 g。此时分离所得MNPF纯度达99%,回收率为92.3%。

A new approach to the large-scale separation and isolation of N-methyl-2-(3-the nitro phenyl) pyrrolidine fullerenes by using column chromatography

This present paper attempts to introduce a new approach to the problem of large-scaled separation of MNPF and in turn to reduce the cost of its preparation.In order to study the effects and regulations of the MNPF separation used as the combustion catalyst of modified double-based propellant in the solid-rockets,we need large amounts of MNPF products.But it was impossible for the traditional processing methods to supply or prepare enough MNPF.In this research,we have implemented a series of separation and isolation experiments on the derivatives of fullerenes in quantity by chromatography.First of all,we have gained the liquid of N-methyl-2-(3-the nitro phenyl) polymerization of silane [3′,4′: 1,2] fullerenes(MNPF) though C60,N-methyl glycine and m-nitrobenzaldehyde in turn.Secondly,we have obtained crude products containing 23% of the crude products of MNPF by rotating and removing the dissolvent and succeeded in isolating MNPF by column chromatography.In so doing,this paper has studied respective factors affecting the separation process,such as eluant,stationary phases,thus,allowing us to develop enough number of samples,with the greatest length of chromatographic column,and so on.Along with the research work in separation and isolation,we have worked out the optimal conditions for isolation,that is, using carbon disulfide as mobile phase,gel column chromatography(300-400 mesh) as stationary phase,chromatography in diameter of 5 cm and the ratio of height and diameter of 6 cm,with the biggest sample size being 23 g.In addition,we have purified crude products needed by recrystallization with carbon disulfide as solvent.Meanwhile,we have refined the products to make it thinner with the ether and acetone.Next,we have done analysis of the products by High Performance Liquid Chromatography(HPLC),to make the efficiency of MNPF separation as high as about 99% and the recovery ratio getting to 92.3%.In so doing,we have successfully solved the time-consuming problem of MNPF separation,and overcome the difficulty in preparing MNPF.Thus,it can be concluded that this paper helps to offer a theoretic basis and technical support for large-scale separation of MNPF.