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›› 2008, Vol. 8 ›› Issue (2): 290-294.

• 过程与工艺 • 上一篇    下一篇

3,5,6-三氯吡啶-2-醇钠在超(近)临界水中的稳定性

刘宁 崔洪友 姚德   

  1. 山东理工大学 山东理工大学化学工程学院 山东理工大学化学工程学院
  • 收稿日期:2007-06-29 修回日期:2007-09-10 出版日期:2008-04-20 发布日期:2008-04-20
  • 通讯作者: 崔洪友

Hydrothermal Stability of Sodium 3,5,6-Trichloropyridin-2-ol in Sub- and Supercritical Water

CUI Hong-you YAO De   

  1. School of Chemical Engineering, Shandong University of Technology School of Chemical Engineering, Shandong University of Technology
  • Received:2007-06-29 Revised:2007-09-10 Online:2008-04-20 Published:2008-04-20
  • Contact: CUI Hong-you

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被引次数

1

摘要： 3,5,6-三氯吡啶-2-醇钠(STCP)热稳定性的研究对于认识2,3,5,6-四氯吡啶(TCP)水解制取STCP过程和STCP废水的处理具有重要的实际意义. 在管式反应器中考察了温度、压力、停留时间和物料配比对STCP稳定性及其降解产物的影响. 结果表明，当温度低于280℃时，STCP具有良好的稳定性；随着反应温度的升高、压力的增大和停留时间的延长，其稳定性降低. 降解产物在525 nm处出现的特征峰是STCP的异构体吡啶酮类化合物引起的. 此外，在加压条件下研究了反应温度、压力、时间和原料配比对TCP水解的影响，其中反应温度是决定水解反应的关键因素，TCP与NaOH摩尔比为1:4时，140℃下反应3 h，收率达95%以上，纯度为99%.

关键词: 6-三氯吡啶-2-醇钠, 超临界, 近临界, 稳定性, 降解

Abstract: The stability of sodium 3,5,6-trichloropyridin-2-ol (STCP) in water at elevated temperatures has implications for the preparation of STCP by hydrolyzing 2,3,5,6-tetrachloropyridine (TCP) and STCP waste treatment processes. Therefore, thermal stability of STCP was investigated in sub- and supercritical water at 240~400℃, 15~30 MPa and residence time from 2 to 12 min in a continuous tubular reactor. The results show that STCP is stable at 280℃ and 25 MPa, but it begins to decompose with the further rising of the temperature, pressure and residence time. Degradation products had an apparent characteristic absorption peak at 520 nm, which was caused by the keto form for STCP. In addition, the reaction temperature, pressure and different ratios of raw materials for preparing STCP by hydrolyzing TCP were studied under elevated pressures in a batch reactor. The results indicate that hydrolysis temperature is a crucial factor to control the reaction rate. The preferred condition for preparing STCP by TCP hydrolysis is that TCP reacts with NaOH for 3 h with a mole ratio of TCP to NaOH 1:4 at 140℃, reaching a STCP yield of higher than 95% with purity of STCP up to 99%.

Key words: sodium 3, 6-trichloropyridin-2-ol, supercritical, subcritical, stability, degradation

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