羟苯磺酸钙的合成工艺研究  

Study on the synthesis of calcium hydroxybenzenesulfonate

作　　者：赵一玫 谭忠琴 王凯[1] 周霁[2] ZHAO Yimei;TAN Zhongqin;WANG Kai;ZHOU Ji(College of Chemistry and Chemical Engineering, Hubei University, Wuhan 430026, China;School of Chemical Engineering and Phannacy, Wuhan Institute of Technology, Wuhan 430074, China)

机构地区：[1]湖北大学化学化工学院,湖北武汉430062 [2]武汉工程大学化工与制药学院,湖北武汉430074

出　　处：《湖北大学学报（自然科学版）》2019年第4期411-419,共9页Journal of Hubei University：Natural Science

摘　　要：以对苯二酚为原料,与硫酸发生磺酸化反应,再用碳酸钙中和成盐,得到羟苯磺酸钙.我们考察硫酸浓度、硫酸与对苯二酚摩尔比、磺化反应时间、磺化反应温度、中和p H值、一次结晶时间、重结晶时间因素对产率的影响.采用正交设计实验方法和SPSS19软件单变量信度分析,获得最佳的工艺参数,即选用90%的硫酸,按硫酸与对苯二酚摩尔比为1. 4∶1,在80℃下反应3 h后,加碳酸钙调p H=4,一次结晶时间为10 h,重结晶时间为12 h,收率52. 04%.为现行羟苯磺酸钙的工艺改进提供一定的理论基础,对提升产品工艺水平具有现实意义.With hydroquinone as a raw material,calcium hydroxybenzenesulfonate was prepared by two steps of sulfonation reaction with sulfuric acid and neutralization reaction with calcium carbonate. The affecting factors of sulfuric acid concentration,molar ratio of sulfuric acid and hydroquinone,sulfonation reaction time,sulfonation reaction temperature, pH value of neutralization, crystallization time of crude product,recrystallization time were investigated on the yield. Through orthogonal design experimental method and single variable reliability analysis of SPSS19 software,the best processing parameters were obtained,that is,90%sulfuric selected,1. 4 ∶ 1 ratio of sulfuric acid to hydroquinone,at 80 ℃ for 3 hours,pH = 4,10 h crystallization time for crude product,and 12 h recrystallization time with a yield of 52. 04%. These results provide a certain theoretical basis for the current process improvement of calcium hydroxybenzenesulfonate,which has practical significance for improving the technological level of this product.

关 键 词：羟苯磺酸钙 正交设计 工艺参数 合成 微血管病 

分 类 号：O624.42[理学—有机化学]