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作 者:刘成兵
出 处:《上海化工》2015年第4期10-12,共3页Shanghai Chemical Industry
摘 要:使用酸碱联合水解法,以二氯苄(质量分数≥80%)为原料制备苯甲醛。第一步进行酸性水解,投加0.05%~0.1%的复合锌盐,控制温度在90~120℃之间,搅拌下滴加水,加水时间控制在3 h内,反应至酸性气体排出量微弱;酸性水解完毕后,加水将游离酸和催化剂洗去,得到乳白色油状液体;第二步进行碱性水解,加入与油等体积的水,再加入一定量的纯碱和乌洛托品,开动搅拌并升温至100℃左右,保温1 h;将油层先进行水蒸气蒸馏,再进行减压蒸馏即可获得质量分数≥99.0%的苯甲醛。Uses the benzylidene chloride crude product (mass fraction ≥ 80%) to prepare benzaldehyde by catalyzed acid-alkali hydrolysis. The first step is acidic hydrolysis, and the mass fraction of the compound zinc salts added is within 0.05%-0.1%. Controlling the solution temperature within 90~120 ℃, adds water with stirring until the amount of the generated acidic gas becomes less, and the time should be less than 3 hours. Then removes the free acid and catalyst by water-washing and gets milky white oily liquid. During the second step--alkaline hydrolysis, adds water (the volume is equal to the oily liquid), sodium carbonate, and urotropine to the oily liquid, raises the temperature to about 100 with stirring and holding for 1 hour. To obtain benzaldehyde (mass fraction ≥99.0%), treats the oil layer first by steam distillation and then by reduced pressure distillation.
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