部分析因实验设计优化α-氯代十二酸合成工艺.docVIP

部分析因实验设计优化α-氯代十二酸合成工艺? 丘宝增1 , 胡静怡2 , 汤吉海1 , 杨 运2 , 陈 献1 , 费兆阳1 , 乔 旭1 , 崔咪芬1 （1. 南京工业大学 化学化工学院，江苏 南京，210009； 2. 江苏省东泰精细化工有限责任公司，江苏 镇江，212132） 摘要：采用5因素2水平的部分析因实验对十二酸氯化合成α-氯代十二酸的工艺进行优化，方差分析得到了反应温度、反应时间、催化剂用量、Cl2流量和O2流量及其交互作用的统计重要度。通过线性模型回归和响应曲面分析了各因素对α-氯代十二酸收率的影响规律，获得浓硫酸催化合成α-氯代十二酸的最佳实验条件为：十二酸20 g，反应温度135 ℃，反应3 h，催化剂用量为10%，Cl2流量为100 mL/min，O2流量为50 mL/min。在最优条件下，α-氯代十二酸的收率为96.0%。 关键词：十二酸；α-氯代十二酸；实验设计；部分析因；优化 中图分类号：TQ028.3 文献标志码：A 文章编号：1671-7627 Optimization of synthesis of α-chlorododecanoic acid using by fractional factorial design QIU Baozeng1, HU Jingyi2, TANG Jinghai1, YANG Yun2, CHEN Xian1, FEI Zhaoyang1, QIAO Xu1, CUI Mifen1, （1. College of Chemistry and Chemical Engineering, Nanjing Tech University, Nanjing, 2. Jiangsu Dongtai Fine Chemical Co. Ltd. Zhengjiang, 212132, China） Abstract: Synthesis process of α-chlorododecanoic acid (α-CDA) through chlorination of dodecanoic acid (DA) was optimized investigated by the fractional factorial design (FFD) of 5 factors and 2 levels. Statistical importance of reaction temperature, reaction time, catalyst amount, O2 and Cl2 flow rates and their interaction was analyzed, respectively. Furthermore, tThe effect laws of every factor to the yield of α-CDA were obtained by linear regression model and analyzed through response surface. The rResults showed that the optimized DA chlorination conditions using concentrated sulfuric acid was as followingfollows with, DA mass of DA was 20 g, reaction temperature was of 135 °C, reaction time was of 3 hours, m(catalyst):m(DA) of =0.1, Cl2 and O2 flow rate was of 100 and 50 mL/min, respectively. Under these conditions , the yield of α-CDA reached 96.0%. Keywords: dodecanoic acid; α-chlorododecanoic acid; experimental design; fractional factorial design; optimization α-氯代脂肪酸是一类直接由脂肪酸合成α-氨基酸和甜菜碱类两性表面活性剂等精细化学品的重要中间体，它们被广泛应用于食品、医药及日化等工业且需求量不断增加 ADDIN NE.Ref.{9EFC9A74-ABA1-4939-90C9-3D8611B73AF4}[1-2]。α-氯代脂肪酸的合成主要采用Cl2对脂肪酸进行自由基取代氯化，光作为一种清洁催化剂，采用不同光源通过引发Cl，Cl取代α氢原子生成α-氯代脂肪酸 AD