摘要
用正交法考察了温度、NaOH用量、溶剂A和溶剂B的体积比,以及溶剂总体积(ml)和糊状叶绿素重量(g)比等四因素对叶绿素铜酸制备过程中的皂化工序的影响;对铜代过程中硫酸铜用量和铜代条件进行试验;探索了酸化结晶工序的工艺条件;采用了反萃结晶法精制叶绿素铜酸;测定了叶绿素铜酸在溶剂中的溶解度;研究了反萃结晶过程的工艺条件;考察了蒸发干燥过程中温度和时间的影响.在对叶绿素铜钠盐制备过程的总结和分析的基础上,提出了优化的工艺流程和条件,并对其进行了实验验证.全过程叶绿素铜钠盐的收率可达59.8%.
The process technology of production of sodium copper chlorophyllin was studied.The orthogonal cross test method with four elements and three levels was used to evaluate the effects of reaction temperature,quantity of NaOH, volume of solvents,volume ratio of solvent A and solvent B,and total volume of solvents on the saponification of crude extract of sikworm feces with acetone.The effects of copper sulfate and reaction pH on the substitution of copper for magnesium in chlorophyll molecular was tested.The process technology of acidification and crystallization was also studied. The solubility data of copper chloropyllin acid was measured in the mixture of solvent Ⅰ and solvent Ⅱ.Accrding to those data,anti solvent crystallization method was used to purify copper chlorophyllin acid,and the process condition was studied.The effects of temperature and time on the drying process were investigated.According to the results of the tests,the technological conditions of overallprocess of preparation of sodium copper chlorophyllin was determined.The overall yield of sodium copper chlorophyllin was 59.8%.