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应用化学
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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 本期目录 | 过刊浏览 | 高级检索 |
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
曲阜师范大学化学与化工学院 山东 曲阜 273165
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
School of Chemistry and Chemical Engineering,Qufu Normal University,Qufu,Shandong 273165,China
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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。

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刘西德
周迪
张兆顺
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 words1,2,3,9-tetrahydro-4H-carbazol    oxidation treatment    high-temperature carbonization    zinc chloride
收稿日期: 2019-05-30           接受日期: 2019-05-30
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
通讯作者: 周迪     E-mail: zhoudi@qfnu.edu.cn
引用本文:   
刘西德, 周迪, 张兆顺. 1,2,3,9-四氢咔唑-4-酮生产废液处理及氯化锌回收利用[J]. 应用化学, 2020, 37(1): 117-122.
LIU Xide, ZHOU Di, ZHANG Zhaoshun. Wastewater Treatment and Recycle of Zinc Chloride in 1,2,3,9-Tetrahydro-4H-carbazol-4-one Production Process. Chinese Journal of Applied Chemistry, 2020, 37(1): 117-122.
链接本文:  
http://yyhx.ciac.jl.cn/CN/10.11944/j.issn.1000-0518.2020.01.190160      或      http://yyhx.ciac.jl.cn/CN/Y2020/V37/I1/117
图1加入氧化剂体积分数与废液吸光度的关系
Fig.1Relationship between the volume fraction of oxidant and the absorbance of wastewaterAll solutions are diluted 200 times. The wavelength is 310 nm
图2加入氧化剂体积分数与废液COD的关系
Fig.2Relationship between the volume fraction of oxidant and COD of wastewater
图3NaClO、H2O2氧化处理废液回收固体的XRD图谱
Fig.3XRD patterns of the solids after oxidant treatment of the wastewater by NaClO, H2O2 respectively
图4NaClO处理回收的固体(A)、工业用催化剂ZnCl2(B)的TEM照片(含选区电子衍射图及高倍透射电子显微镜照片)
Fig.4TEM images of recycled solid after NaClO treatment(A), industrial catalyst ZnCl2(B)(including electron diffraction patterns of selected positions and high-resolution TEM images)
图5ZnCl2热重分析曲线
Fig.5TGA curves of ZnCl2a.industrial sample; b.sample after high-temperature carbonization
图6高温碳化回收ZnCl2的XRD图谱(A)、TEM照片(含选区电子衍射图案及高倍透射电镜图)(B)
Fig.6XRD patterns(A) and TEM images(including electron diffraction patterns of selected positions and high-resolution TEM images)(B) of recycled ZnCl2 after high-temperature carbonization treatment
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