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本文提出了一种简便的吸附柱色谱-两步结晶的实验室测定渣油中微晶蜡潜含量的方法。先用无水氧化铝柱,以石油醚为冲洗剂,在溶剂循环色谱柱上脱去沥青质、胶质和多环芳烃,然后在—20℃的酮-苯溶剂中结晶脱去油,再升温,二次结晶得到各熔点牌号的精制衡晶蜡。溶剂组成为甲苯:丁酮=60:40;溶剂比为30mL/g。测得南阳轻脱沥青油中80号、85号和90号徽晶蜡的潜含量分别为40.6%、22.7%和9.5%,南阳重脱沥青油中则分别为30.7%、14.7%和7.2%。采用密度法计算了各精制微晶蜡的结构族组成的结构参数;用氢核磁共振测得其支化度均小于0.106,用尿素络合法测得正构烷烃含量均大于39.2%。结构族组成在折光指数-熔点图上分别都位于异构烷和单环环烷区。
In this paper, a simple method for the determination of latent volume of microcrystalline wax in residual oil by two-step crystallization in a laboratory is proposed. First remove the asphaltenes, gums and polycyclic aromatic hydrocarbons (PAHs) on a solvent-circulating column with petroleum ether as a solvent on an anhydrous alumina column, and then de-oil the oil in a ketone-benzene solvent at -20 ° C Heating, secondary crystallization of the melting point of the refined wax grades. The solvent composition is toluene: butanone = 60: 40; the solvent ratio is 30 mL / g. Measured Nanyang light deasphalted asphalt oil 80, 85 and 90, the latent content of wax 40.6%, 22.7% and 9.5%, respectively, Nanyang re-asphalts in the oil were 30. 7%, 14.7% and 7.2%. Density method was used to calculate the structure parameters of each refined microcrystalline wax. The degree of branching was less than 0.106 by hydrogen nuclear magnetic resonance, and the content of n-alkanes was greater than 39.2 %. Structural family composition in the refractive index - the melting point diagram were located in the isoparaffins and monocyclic naphthenic area.