应用化学 ›› 2020, Vol. 37 ›› Issue (1): 117-122.DOI: 10.11944/j.issn.1000-0518.2020.01.190160

• 研究论文 • 上一篇    

1,2,3,9-四氢咔唑-4-酮生产废液处理及氯化锌回收利用

刘西德,周迪(),张兆顺   

  1. 曲阜师范大学化学与化工学院 山东 曲阜 273165
  • 收稿日期:2019-05-30 接受日期:2019-05-30 出版日期:2020-01-08 发布日期:2020-01-08
  • 通讯作者: 周迪
  • 基金资助:
    国家自然科学基金(21506114)和曲阜师范大学科研启动基金(BSQD20130116)资助

Wastewater Treatment and Recycle of Zinc Chloride in 1,2,3,9-Tetrahydro-4H-carbazol-4-one Production Process

LIU Xide,ZHOU Di(),ZHANG Zhaoshun   

  1. School of Chemistry and Chemical Engineering,Qufu Normal University,Qufu,Shandong 273165,China
  • Received:2019-05-30 Accepted:2019-05-30 Published:2020-01-08 Online:2020-01-08
  • Contact: ZHOU Di
  • Supported by:
    Supported by the National Natural Science Foundation of China(No. 21506114), and the Scientific Research Foundation of Qufu Normal University(No.BSQD20130116)

摘要:

1,2,3,9-四氢咔唑-4-酮生产废液量大且危害严重,本文探究了NaClO、H2O2氧化处理废液的效果及存在的问题,同时提出了高温碳化处理的新工艺路线。 实验结果表明,采用NaClO、H2O2氧化处理废液未能达到理想要求,且回收的固体色泽差、无催化活性。 而废液经143 ℃蒸馏、残留液500 ℃高温碳化处理40 min后回收的氯化锌,具有良好催化活性,可使单苯腙转化率达到52.6%,实现了其在1,2,3,9-四氢咔唑-4-酮生产过程中的循环利用 。研究结果为1,2,3,9-四氢咔唑-4-酮生产废液处理及资源综合利用提供了一条新途径。

关键词: 1,2,3,9-四氢咔唑-4-酮, 氧化处理, 高温碳化, 氯化锌

Abstract:

A large amount of wastewater in the production process of 1,2,3,9-tetrahydrocarbazol-4-one is generated and leads to severe harm. In this work, the effects and existing problems in oxidation treatment were investigated. Meanwhile, the new process route of high-temperature carbonization treatment was developed. The results show that the oxidation treatments with NaClO and H2O2 fail to achieve the desired effect, and the recycled solid is poor in color and has no catalytic activity. However, zinc chloride recovered through distilling at 143 ℃ and high-temperature carbonization at 500 ℃ for 40 min, exhibits excellent catalytic activity, which makes the conversion of monophenylhydrazone reach 52.6%. Ultimately, the reclamation of zinc chloride in the production of 1,2,3,9-tetrahydrocarbazol-4-one is realized. At the same time, the experimental results provide a new way for the treatment of 1,2,3,9-tetrahydrocarbazol-4-one production wastewater and comprehensive utilization of resources.

Key words: 1,2,3,9-tetrahydro-4H-carbazol, oxidation treatment, high-temperature carbonization, zinc chloride