论文部分内容阅读
苯在四氯化碳溶剂中以硝酸和疏酸的混合酸为硝化剂在温和条件下进行硝化,硝基苯的产率高,硫酸可以回收再利用。例如,在带有搅拌器、滴液漏斗、温度计和冷凝器的四颈烧瓶中,加入44.4毫升苯和40毫升四氯化碳,将39.5毫升浓硝酸和41.5毫升浓硫酸混合后从滴液漏斗中滴加,维持温度在15~55℃之间,约40分钟滴完后,在55~62℃继续反应30分钟。有机层分别用水、10%氢氧化钠溶液、水洗涤,干燥、蒸馏,先蒸出溶剂可再用。然后收集204~210.8℃的馏份,得硝基苯60.6克,产率98.53%。废硫酸通过蒸馏浓缩后,可重新用于硝化反应。
Benzene in carbon tetrachloride solvent to nitric acid and acid mixed acid as a nitrating agent nitrification under mild conditions, high yield of nitrobenzene, sulfuric acid can be recycled and reused. For example, in a four-necked flask equipped with a stirrer, a dropping funnel, a thermometer and a condenser, 44.4 ml of benzene and 40 ml of carbon tetrachloride were charged, 39.5 ml of concentrated nitric acid and 41.5 ml of concentrated sulfuric acid After mixing, the mixture was added dropwise from the dropping funnel to maintain the temperature between 15 and 55 ° C. After about 40 minutes, the reaction was continued at 55 to 62 ° C for 30 minutes. The organic layer was washed with water, 10% sodium hydroxide solution and water respectively, dried and distilled. The solvent was distilled off before reuse. Then collected 204 ~ 210.8 ° C distillate, nitrobenzene 60.6 grams, the yield was 98.53%. Waste sulfuric acid after concentration by distillation, can be re-used for nitrification.