| 2-氯-5-三氟甲基吡啶和3-三氟甲基吡啶的制备 |
| |
| 引用本文： | 董青青,于万金,胡猛,林胜达,刘武灿,张建君,程党国,陈丰秋.2-氯-5-三氟甲基吡啶和3-三氟甲基吡啶的制备[J].化工学报,2015,66(12):4843-4849. |
| |
| 作者姓名： | 董青青 于万金 胡猛 林胜达 刘武灿 张建君 程党国 陈丰秋 |
| |
| 作者单位： | 1.浙江大学化学工程与生物工程学院, 浙江 杭州 310027;2.浙江省化工研究院, 国家ODS替代品工程技术研究中心, 浙江省化工新材料重点实验室, 浙江 杭州 310023 |
| |
| 基金项目： | 浙江省博士后科研择优资助项目(BSH1402061)。 |
| |
| 摘 要： | 研究了以3-甲基吡啶、氟化氢和氯气为原料在流化床反应器中一步法气相氯氟化反应制备2-氯-5-三氟甲基吡啶和3-三氟甲基吡啶的工艺,并对催化剂进行了筛选和考评,发现CrO-Al、Cr Cl-Al的活性较佳。以CrO-Al为催化剂,空速为288 h-1,温度为300℃时,2-氯-5-三氟甲基吡啶和3-三氟甲基吡啶的总收率最高,为66.6%,且失活催化剂在350℃,氮气和空气的体积比为1:1的混合气体下再生后,其催化活性基本可以恢复,2-氯-5-三氟甲基吡啶和3-三氟甲基吡啶的总收率均保持在66%左右。根据实验结果提出了反应机理和结焦机理。对催化剂进行了BET、TG和NH3-TPD表征,发现催化剂失活的主要原因是积炭覆盖了催化剂表面以及孔道,使催化剂强酸中心大量减少所致。
|
| 关 键 词： | 3-甲基吡啶 2-氯5-三氟甲基吡啶 3-三氟甲基吡啶 流化床 催化剂 活性 再生 |
| 收稿时间： | 2015-06-29 |
| 修稿时间： | 2015-09-09 |
Production of 2-chloro-5-trifluoromethylpyridine and 3-trifluoromethylpyridine |
| |
| DONG Qingqing,YU Wanjin,HU Meng,LIN Shengda,LIU Wucan,ZHANG Jianjun,CHENG Dangguo,CHEN Fengqiu.Production of 2-chloro-5-trifluoromethylpyridine and 3-trifluoromethylpyridine[J].Journal of Chemical Industry and Engineering(China),2015,66(12):4843-4849. |
| |
| Authors: | DONG Qingqing YU Wanjin HU Meng LIN Shengda LIU Wucan ZHANG Jianjun CHENG Dangguo CHEN Fengqiu |
| |
| Affiliation: | 1.College of Chemical and Biological Engineering, Zhejiang University, Hangzhou 310027, Zhejiang, China;2.Zhejiang Research Institute of Chemical Industry, ODS Substitutes National Engineering Research Center, Zhejiang Key Laboratory of New Chemical Materials, Hangzhou 310023, Zhejiang, China |
| |
| Abstract: | 2-Chloro-5-trifluoromethylpyridine and 3-trifluoromethylpyridine are produced by β-picoline reacting with chlorine and hydrogen fluoride in a fluidized-bed reactor. The total yield of 2-chloro-5- trifluoromethylpyridine and 3-trifluoromethylpyridine reaches 66.6% over the CrO-Al catalyst at a space velocity of 288 h-1 and temperature of 300℃. The reactivity of the deactivated catalysts is recovered after regeneration at 350℃ with mixed gas of nitrogen and air at volume ratio of 1:1. The total yield is around 66% with regenerated catalysts under the condition of 288 h-1 and 300℃. According to the reaction result, the mechanism of one-step chlorofluorination reaction is proposed, dehydrochlorination-condensation of intermediate products accounted for coking. The results of BET, TG and NH3-TPD characterizations indicate that the deactivation of the catalysts is caused by the carbonaceous by-products which cover the surface and pores of the catalyst. |
| |
| Keywords: | 2-chloro-5-trifluoromethylpyridine 3-trifluoromethylpyridine β-picoline fluidized-bed catalyst reactivity regeneration |
| 本文献已被 CNKI 万方数据 等数据库收录！ |
| 点击此处可从《化工学报》浏览原始摘要信息 |
|
点击此处可从《化工学报》下载全文 |
|
