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2-氯-5-三氟甲基吡啶和3-三氟甲基吡啶的制备

董青青 于万金 胡猛 林胜达 刘武灿 张建君 程党国 陈丰秋

化工学报2015,Vol.66Issue(12):4843-4849,7.
化工学报2015,Vol.66Issue(12):4843-4849,7.DOI:10.11949/j.issn.0438-1157.20151013

2-氯-5-三氟甲基吡啶和3-三氟甲基吡啶的制备

Production of 2-chloro-5-trifluoromethylpyridine and 3-trifluoromethylpyridine

董青青 1于万金 2胡猛 1林胜达 2刘武灿 2张建君 2程党国 1陈丰秋1

作者信息

  • 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
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摘要

Abstract

2-Chloro-5-trifluoromethylpyridine and 3-trifluoromethylpyridine are produced byβ-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.

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

Key words

2-chloro-5-trifluoromethylpyridine/3-trifluoromethylpyridine/β-picoline/fluidized-bed/catalyst/reactivity/regeneration

分类

化学化工

引用本文复制引用

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):4843-4849,7.

基金项目

浙江省博士后科研择优资助项目(BSH1402061). supported by the Postdoctor Foundation of Zhejiang (BSH1402061). (BSH1402061)

化工学报

OA北大核心CSCDCSTPCD

0438-1157

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