四氢嘧啶溶析结晶工艺的研究  

Study on elution crystallization process of tetrahydropyrimidine

作　　者：李珍爱 李海军 胡红涛 张英华 郑德强 唐双焱[4] LI Zhen-ai;LI Hai-jun;HU Hong-tao;ZHANG Ying-hua;ZHENG De-qiang;TANG Shuang-yan(Shandong Freda Biotechnology Co.,Ltd.,Linyi 276700,China;Shandong Freda Pharmaceutical Group Company,Jinan 250000,China;Shandong Academy of Pharmaceutical Sciences,Jinan 250000,China;CAS Key Laboratory of Microbial Physiology and Metabolic Engineering,Institute of Microbiology,Chinese Academy of Sciences,Beijing 100101,China)

机构地区：[1]山东福瑞达生物科技有限公司,山东临沂276700 [2]山东福瑞达医药集团有限公司,山东济南250000 [3]山东省药学科学院,山东济南250000 [4]中国科学院微生物研究所,中国科学院微生物生理与代谢工程重点实验室,北京100101

出　　处：《现代化工》2022年第11期207-210,共4页Modern Chemical Industry

摘　　要：为提高四氢嘧啶的结晶收率,提出了有机试剂溶析结晶四氢嘧啶浓缩液方案,考察了溶析剂的选择、料液浓度、溶析剂的添加量及搅拌速率对收率的影响。结果表明,利用6倍料液体积的丙酮从300 g/L的四氢嘧啶浓缩液中溶析结晶出晶体,搅拌速率为300 r/min,一次结晶收率可达到94%以上,相比降温结晶提高40%以上,且晶体经重结晶、干燥后纯度可达99%以上。A technical solution is proposed for the elution crystallization of tetrahydropyrimidine concentrate by organic reagent to improve the crystallization yield of tetrahydropyrimidine.The influences of the selection of eluent,the concentration of the tetrahydropyrimidine concentrate,the amount of the eluent and the stirring rate on the yield of tetrahydropyrimidine are explored.It is indicated that the primary crystallization yield can reach 94%,40%higher than that by the cooling crystallization when acetone with a volume 6 times that of the feed liquid is used to elute and crystal the 300 g·L^(-1) tetrahydropyrimidine concentrate,and the stirring rate is 300 rpm.Moreover,the purity of the crystal after recrystallization and drying can exceed 99%.

关 键 词：四氢嘧啶 有机试剂 丙酮 结晶 干燥 

分 类 号：TQ026.5[化学工程]