【作者】 吴卫彦；

【导师】 赵广荣； 王清格；

【作者基本信息】 天津大学 ， 制药工程， 2009， 硕士

【摘要】 2-酮基-L-古龙酸又叫古龙酸,是维生素C生产中重要的中间体,古龙酸的收率高低直接影响到维生素C成本,本文研究了吸附法预处理古龙酸母液,母液转型盐析结晶回收古龙酸钠,古龙酸钠用阳离子树脂交换回收古龙酸的工艺。在实验中,吸附法预处理古龙酸母液与本厂目前工艺进行了比较;通过对四种转型剂、析出剂研究对比,筛选出较为理想的Na2CO3作为转型剂、CH3OH为析出剂。研究了影响古龙酸钠盐析结晶的主要操作条件:加入晶种温度、晶种的用量、析出温度、保温时间对产品收率的影响,筛选出最佳的盐析结晶回收工艺条件,即加入晶种的温度为23～24℃,晶种用量为0.8～1.0g,析出温度为0～﹣2℃,保温时间为1h;研究并筛选出古龙酸钠交换成古龙酸采用X型树脂交换时最佳工艺条件为:15%的古龙酸钠溶液,用床层高径比为10的X型树脂进行交换,出料速度控制3倍柱体积收集PH﹤1.7的溶液,溶液浓缩降温结晶,得到古龙酸。结果表明,采用此回收工艺古龙酸的回收收率可达到77.63%以上,比原工艺提高了二十个百分点,古龙酸干品质量明显提高,含量达到了88.54%,提高了3%;由回收古龙酸经酯化、转化的维生素C钠含量、收率也较目前工艺分别提高1.27%和1.95%。研究结果表明,采用吸附法处理古龙酸母液、母液转型盐析结晶和X型树脂交换法回收古龙酸工艺与原工艺相比,无论从产品收率及中间体的质量方面都有明显提高。而又具有易分离、无污染、无腐蚀性的优点,是一种极具潜力的绿色环保型回收工艺。更多还原

【Abstract】 2 -Keto-L-gulonic acid is the important intermediate during producing Vitamin C, and its receiving rate influences the cost of Vitamin C directly. In this article, the salting out crystallization law to recycle gulong sodium, Gulong sodium dissolves and cation exchange resin recovering gulonic acid recovery process has been studied.Through the transformation of four different agents, precipitation contrast agent research, selected a more ideal agent Na2CO3 as a transition, CH3OH as precipitation agent. In this experiment, the main operating condition which affecting the 2 - keto-L-gulonic sodium salt out and crystal has been studied: Adding crystal seeds of temperature, the amount of seed, precipitation temperature, holding time on the yield of products, Selected the best salt analysis of the crystallization of the recovery process conditions, namely by adding crystal seeds of the temperature of 23 ~ 24℃, the amount of seeds for the 0.8g ~ 1.0g, precipitation temperature of 0 ~ -2℃, holding time for 1h.At the same time, research on using of X-resin exchange to translate sodium gulong sodium into gulonic acid has been done, and the best conditions were as follows: 15% sodium gulong with bed height to diameter ratio of 10 X-exchange resin, the material speed control 3 times the size of the collection of columns PH <1.7 of the solution, the solution concentrated cooling crystallization recovered gulonic acid goods.The results showed that the introduction of new recycling technology of vitamin C intermediates of 2 - Keto-L-gulonic acid recovery yield of 77.63% to reach more than the original 20.00%, The dry goods quality of 2 - Keto-L-gulonic acid was significantly improved and the content has achieved 88.54%, the present craft enhanced 3%.The Vc-Na,s making by gulonic acid recovery content and yield is enhanced1.27% and 1.95%.The results show that the use of salting-out crystallization transition and X-type exchange resin recycling 2-Keto-L-gulonic acid new technology has markedly improved in terms of product yield and quality of intermediate, comparing with the original process. Easy separation and pollution-free, non-corrosive non-corrosiveness, is one kind of a potential type of green environment-friendly recycling processes.更多还原