【作者】 刘勇；

【导师】 杨景昌；

【作者基本信息】 四川大学 ， 化学工艺， 2006， 硕士

【摘要】 研究了以粗羊毛脂为原料提取胆甾醇的工艺过程,重点研究了从羊毛脂醇中提取胆甾醇的工艺过程。将原来的一次皂化过程改为二次皂化过程;将配合试剂由原来的六水氯化钙改为含40%水的氯化钙;将原来的直接在乙醇中配合,改为先用石油醚和水对羊毛脂醇进行萃取除杂,接着使羊毛脂醇在石油醚和少量乙醇中配合。通过研究,得出了各相关因素对胆甾醇纯度及收率的影响规律和相应的适宜工艺条件。得出的适宜工艺条件如下:对于羊毛脂皂化过程,第一次皂化碱用量为1.8倍理论碱量,时间为8h;第二次皂化碱用量也为1.8倍理论碱量,时间为6h。对于皂化产物分离过程,氯化钙用量为理论用量的1.3倍,反应温度为25℃左右;对羊毛脂醇的萃取过程,第一次萃取,乙醇:粗羊毛脂(v:w)=4:1,萃取30min;第二次萃取,乙醇:粗羊毛脂(v:w)=2:1,萃取20min;第二次皂化转化只需一次萃取,乙醇:粗羊毛脂(v:w)=1.5:1,萃取20min。对于胆甾醇的配合及其配合物提纯过程,萃取除杂时,石油醚:水:粗羊毛脂(v:w:w)=3:2:1;配合时,氯化钙:胆甾醇(mol:mol)=6:1,其中水:氯化钙(w:w)=2:3,配合温度为77~78℃,配合反应时间1h;提纯时,乙醇:石油醚(v:v)=3:50,降温速度为10℃/h,最终冷却温度为10℃。对于配合物水解过程,水:粗羊毛脂(w:w)=10:1,温度为15℃左右,时间为1h。对于胆甾醇的精制过程,乙醇:粗胆甾醇(v:w)=6:1,最终冷却温度为5℃。在上述适宜工艺条件下,得到的羊毛脂醇皂化值约为10mg/g,所得胆甾醇产品的纯度达90%以上,总收率可望达到60%以上,其质量基本符合美国更多还原

【Abstract】 In the paper, the process of extraction of cholesterol from crude lanolin was studied, and the one from lanolin alcohol which is one of saponification production of lanolin were focused on. The once saponification was changed to the twain saponification. Change of complexing reagent from CaCl2·6H2O to hydrated CaCl2 with 40% water, and change of complexing solvent from ethanol to petroleum ether and a little ethanol were done, and the impurity in lanolin alcohol was extracted by petroleum ether and water before the complexing, so that the adduct yield was improved. On the base of study, the effects of every correlative factor on yield and purity of cholesterol, and the suited process conditions were presented.The suited conditions of process were determined as follows:For the process of crude lanolin saponification,NaOH dosage is 1.8 times to theoretic dosage, and reaction time is 8h in the first saponification, and NaOH dosage is the same multiple to first saponification, and the time is 6h in the second saponification.For the separation of saponification results, CaCl2 dosage is 1.3 times to theretical dosage, and reaction temperature is 25℃. For the extractions of lanolin alcohol from calcium lanolin acid, the ratio of ethanol to lanolin is 4:1, 2:1 and 1.5:1 respectively, and the extraction time is 30min, 20min and 20min respectively.For the complexing of cholesterol and purification of adduct, the ratio of petroleum ether to water and crude lanolin is 3:2:1 in the of romoving impurity, and the rate of CaCl2 to cholesterol is 6 by molecule, the rate of CaCl2 to water is 1.5更多还原