环糊精包结分离制备高纯度辛基二茂铁同分异构体

以辛基二茂铁工业品与本实验室前期分离得到的三种一元辛基二茂铁混合制剂(C8-Fc)为原料,以β-环糊精包结硅胶得到包结分离柱Immo-CD-1,确定了包结分离制备高纯度辛基二茂铁同分异构体的原料;在此基础上,利用正交实验的方法,确定了包结分离的主要影响因素与最佳条件,发现水分含量对于分离效果的影响最为显著,经Immo-CD-1柱分离得到纯度为97.2%的(4-辛基)-二茂铁、纯度大于96%的(3-辛基)-二茂铁以及(2-辛基)-二茂铁和(3-辛基)-二茂铁的混合物;利用类似的方法,以羟丙基-β-环糊精为主体材料制备包结分离柱Immo-CD-2,并对上述所得到的(2-辛基)-二茂铁和(3-辛基)-二茂铁混合物进行包结分离,经优化分离后,得到纯度大于95%的(2-辛基)-二茂铁。

Inclusion separation of cyclodextrin for preparation of octylferrocene isomers in high purity

Octylferrocene is one of the most widely used rocket fuel catalyst.However the current commercial octylferrocene is a mixture of (2-octyl)-ferrocene, (3-octyl)-ferrocene,(4-octyl)-ferrocene (C8-Fc) and multi-substituted ferrocene. The separation and purification of the commercial octylferrocene compounds is crucial for achieving their maximum catalytic efficiency. The C8-Fc was chosen as the raw material for preparation of octylferrocene isomers in high purity with β-cyclodextrin coated silicone as the packing agent ( Immo-CD-1) . When the C8-Fc was used as the raw material and Immo-CD-1 was the stationary phase, the influen-cing factors including the content of water, the particle size of supporter and the loading ratio of the silicone coated with cyclodex-trins were optimized by orthogonal experiments. The main innovation of this research is that the content of water in the Immo-CD-1 has greatest effect on the separation. A positive column chromatography separation with Immo-CD-1 as the stationary phase, n-hex-ane as the eluent, C8-Fc as raw material could get the relative content of 97.2% (4-octyl)-ferrocene and relative content of 96.1%( 3-octyl)-ferrocene,as well as a mixture of ( 3-octyl)-ferrocene and ( 2-octyl)-ferrocene. The separation column of Immo-CD-2 was prepared with hydroxypropyl-β-cyclodextrin coated silicone as the packing and separation of the mixture of ( 3-octyl)-ferrocene and (2-octyl)-ferrocene was carried out. The relative purity of (2-octyl)-ferrocene can reach 95.3 %.