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作 者:郭庆 赵露 李凯 徐宾朋 赵厚发 GUO Qing;ZHAO Lu;LI Kai;XV Bin-peng;ZHAO Hou-fa(Anhui Chem-Bright Bioengineering Co.,Ltd.,Huaibei Anhui 235000,China)
机构地区:[1]安徽科宝生物工程有限公司,安徽淮北235000
出 处:《辽宁化工》2023年第12期1768-1770,1774,共4页Liaoning Chemical Industry
基 金:淮北市科技计划重大专项(项目编号:Z2020014);安徽省三重一创重大专项(项目编号:HB-2017-ZX2)。
摘 要:以羊毛醇为原料,通过皂化、萃取、浓缩结晶及重结晶等工序,建立了胆固醇的产业化工艺路线,研究了各工艺条件的影响。确定最佳工艺条件为:乙醇用量为羊毛醇质量的2倍,10%碱液用量为羊毛醇质量的1倍,时间为7h;萃取剂为环己烷,用量为皂化液总质量的5倍,时间为60min,重复萃取2次;结晶试剂为乙酸乙酯,用量为浓缩物质量的8倍,加热回流时间为1h;重结晶试剂为无水乙醇,用量为胆固醇质量的8倍,pH值为10.5,回流时间为2h,结晶温度为5~10℃。在上述工艺条件下,所得胆固醇产品的收率≥90%,含量(质量分数)≥95%,熔点≥147℃。The industrialization process of cholesterol was established by saponification,extraction,concentration,crystallization and recrystalization with lanolin as raw material,and the influence of each process condition was studied.The optimum conditions were as follows:the amount of ethanol was 2 times the mass of lanolin alcohol,the amount of 10%lye was 1 times the mass of lanolin alcohol,and the time was 7 h.The extraction agent was cyclohexane,and the amount was 5 times of the total mass of saponification solution.The extraction time was 60 min,and the extraction was repeated twice.The crystallization reagent was ethyl acetate,the dosage was 8 times the mass of concentrate,and the reflux time was 1 h.The recrystallization reagent was anhydrous ethanol,the dosage was 8 times the weight of cholesterol,the pH value was 10.5,the reflux time was 2 h,and the crystallization temperature was 5~10℃.Under the above conditions,the yield of cholesterol products was more than 90%,the mass fraction was more than 95%,and the melting point was more than 147℃.
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