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出 处:《染料与染色》2004年第5期287-288,251,共3页Dyestuffs and Coloration
摘 要:将间硝基氯苯溶于甲醇,置于压力反应器中,加入Raney—Ni催化剂和脱氯抑制剂CEN,在温度为65℃和1.2MPa的氢气压力下反应80~85分钟,制取了间氟苯胺。反应混合物中的产品含量在75℃达到最高值、反应物中的产品含量随氢气压力的升高而增加,当氢气压力在10MPa~1.2MPa时产物含量最高,Raney—Ni用量为反应物的10%,脱氟抑制剂CEN为0.4%时可使产品的纯度达到99.4%。正交试验确定了优选工艺条件。m-Nitrochlorobenzene was dissolved in methanol in an autoclave, Raney-Ni catalyst and dechlorination-inhibitor were added, hydrogenation was carried out at 1.2MPa and 65 ℃ for 80-85 minutes, giving the product m-chloroaniline. The content of the product in the reaction mixture was the highest when the reaction was at 75℃; The content was improved with the increase of hydrogen pressure, the pressure being 1.0-1.2MPa and the content of the product would be the highest. The amounts of Raney-Ni and dechlorination inhibitor being 10% and 0.4% of the reactant, respectively, a purity of 99.4% of the product achieved.The optimum conditions were determined by orthogonal experiments. '
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