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作 者:刘长春[1]
机构地区:[1]江苏食品职业技术学院生物化工系,江苏淮安223001
出 处:《化学试剂》2007年第1期37-38,42,共3页Chemical Reagents
基 金:淮安市科技项目(HAG03040)资助
摘 要:研究了以Pd-Fe/TiO2作催化剂,3-氯-4-氟硝基苯常压加氢制备3-氯-4-氟苯胺的方法,考察了该催化剂对3-氯-4-氟硝基苯的常压加氢反应的性能,探讨了影响加氢反应的主要因素。实验表明,经KBH4处理过的催化剂具有较高的催化活性,Fe的引入同时提高了催化剂的催化活性和选择性。当催化剂中Pd的质量分数为5%,Fe的质量分数为0.2%,催化剂用量为13.2×10-3g Pd/0.1 mol硝基物,溶剂用量为80 mL无水乙醇/0.1 mol硝基物,反应温度50℃时,3-氯-4-氟苯胺的产率为98.0%,纯度达99.0%以上。The process for preparing 3-chloro-4-fluoroanihne from 3-chloro-4-fluoro nitrobenzene via hydrogenation under atmosphere pressure using Pd-Fe/TiO2 as the catalyst was studied. The major factors affecting the reaction process were discussed. The result shows that the catalyst reduced by KBH4 exhibited higher catalytic activity, and both catalytic activity and selectivity increased with the addition of Fe to the catalytic system. When the mass fraction of Pd in the catalyst was 5 %, and the mass fraction of Fe in the catalyst was 0.2%, the quantity of catalyst reached 13.2 ×10^-3g Pd per 0.1 mol of 3-chloro-4-fluoro nitrobenzene in 80 mL of anhydrous ethanol. The yield of 3-chloro-4-fluoroaniline was 98 % at a reaction temperature of 50 ℃ with the product purity exceeding 99%.
关 键 词:3-氯-4-氟苯胺 Pd-Fe/TiO2 常压加氢 催化 合成
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