3,5,6-三氯吡啶-2-醇钠在超(近)临界水中的稳定性  

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

作　　者：刘宁[1] 崔洪友[1] 姚德[1] 

机构地区：[1]山东理工大学化学工程学院,山东淄博255049

出　　处：《过程工程学报》2008年第2期290-294,共5页The Chinese Journal of Process Engineering

基　　金：山东省自然科学基金资助项目(编号:2004ZX24);山东省中青年科学家奖励基金资助项目(编号:2005BS05009)

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525nm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3h,收率达95%以上,纯度为99%。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 STCE 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%.

关 键 词：3 5 6-三氯吡啶-2-醇钠 超临界 近临界 稳定性 降解 

分 类 号：TQ450.9[化学工程—农药化工]