全文下载: 20240514.pdf
文章编号: 1672-6987(2024)05-0057-05; DOI: 10.16351/j.1672-6987.2024.05.007
夏孔浩, 丁军委*, 单玉领, 张欣磊(青岛科技大学 化工学院, 山东 青岛 266042)
摘要: 研究了以1,4-萘醌为原料,催化氯化制备2,3-二氯-1,4-萘醌的反应机理及合成工艺优化。研究发现该氯化反应为酸催化反应机理,氯化氢为有效的1,4-萘醌氯化催化剂。通过工艺优化确定了最佳合成条件为:反应温度75 ℃,催化剂用量15 mL,溶剂用量80 mL,原料加入量为75 g,通氯速度为15 mL·min-1,反应时间为15~2 h,产品纯度大于995%。母液经多次套用后产品收率达到91%~93%,产品纯度均达到优等品级别(≥990%)。
关键词: 2,3-二氯-1,4-萘醌; 1,4-萘醌; 酸催化
中图分类号: TQ 612.1文献标志码: A
引用格式: 夏孔浩, 丁军委, 单玉领, 等. 2,3-二氯-1,4-萘醌的合成工艺[J]. 青岛科技大学学报(自然科学版), 2024, 45(5): 57-61.
XIA Konghao, DING Junwei, SHAN Yuling, et al. Study on synthesis technology of 2, 3-dichloro-1, 4-naphthoquinone[J]. Journal of Qingdao University of Science and Technology(Natural Science Edition), 2024, 45(5): 57-61.
Study on Synthesis Technology of 2,3-Dichloro-1,4-Naphthoquinone
XIA Konghao, DING Junwei, SHAN Yuling, ZHANG Xinlei
(College of Chemical Engineering,Qingdao University of Science and Technology, Qingdao 266042, China)
Abstract: The reaction mechanism and synthesis process optimization of 2, 3-dichloro-1, 4-naphthoquinone prepared by catalytic chlorination with 1, 4-naphthoquinone as raw material, hydrogen chloride as catalyst and chlorobenzene as solvent were studied. The optimum synthesis conditions were determined as follows: reaction temperature 75 ℃, catalyst dosage 15 mL, solvent dosage 80 mL, raw material dosage 75 g, chlorination speed 15 mL·min-1, reaction time 15—2 h, product purity more than 995%. After repeated application of mother liquor, the yield of the product reached 91%—93% and the purity of the product was ≥990%.
Key words: 2, 3-dichloro-1, 4-naphthoquinone; 1, 4-naphthoquinone; acid catalyst
收稿日期: 2023-11-02
基金项目: 山东省重点研发计划项目(2019GSF109055).
作者简介: 夏孔浩(1995—),男,硕士研究生.*通信联系人.