工业级卡托辛成分分析及其双核二茂铁制备工艺

2,2-双(乙基二茂铁)丙烷（卡托辛）因其优异的催化活性和制药工艺性，成为当前复合固体推进剂中主要的燃速催化剂之一。由于卡托辛合成工艺复杂，工业级产品成分也很复杂，使得其相关产品的性能难以得到保证。利用气相色谱-质谱联用技术和高效液相色谱技术，对工业级卡托辛的成分进行了分析；依据各成分结构特性及其极性、溶解度差异，通过柱层析法、溶解-析出法对其进行了分离提纯，得到了含量高且分子结构中含有两个二茂铁单元结构的双核二茂铁。结果发现：工业级卡托辛成分中双核二茂铁的总含量为84.82 %，单核二茂铁的总含量为15.18 %。柱层析法可得到含量大于99.0%的双核二茂铁；溶解-析出法可得到含量大于96.5%的双核二茂铁，且该法具有可宏量制备、操作工艺简便、成本低等特点。

Component Analysis of Industrial Grade Catocene and Preparation of Binuclear Ferrocene

2,2-bis (ethylferrocenyl) propane (catocene) has become one of the main burning rate catalysts in composite solid propellant because of its excellent catalytic activity and pharmaceutical technology. The composition of industrial grade products is also very complicated due to the complex synthesis process of catocene, which makes the performance of related products difficult to be guaranteed. The composition of industrial grade catocene is analyzed by using gas chromatography-mass spectrometry and high performance liquid chromatography. According to the structural characteristics of the components and the differences in their polarities and solubilities, the components of catocene were separated and purified by using column chromatography and dissolution-precipitation method, and the binuclear ferrocene containing two ferrocene units in the molecular structure with high content was obtained. It is found that the total contents of binuclear ferrocene and mononuclear ferrocene in the industrial grade catocene are 84.82% and 15.18%, respectively. The results show that column chromatography can be used to obtain binuclear ferrocene with a content greater than 99.0%; the dissolution-precipitation method can be used to obtain binuclear ferrocene with a content greater than 96.5%, and the proposed method has the characteristics of large-scale preparation, simple operation and low cost, etc.