对氟苯甲醛合成方法研究  

Study on Synthesis Method of p-Fluorobenzaldehyde

作　　者：任建军 张伟 REN Jian-jun;ZHANG Wei(Jiyuan Hengshun New Material Co.,Ltd.,Jiyuan Henan 459000,China)

机构地区：[1]济源市恒顺新材料有限公司,河南济源459000

出　　处：《辽宁化工》2023年第12期1800-1803,共4页Liaoning Chemical Industry

摘　　要：以对氟甲苯为原料,N-氯代丁二酰亚胺为氯化剂进行氯化,在催化剂四丁基溴化铵作用下滴水进行水解,用乙酸乙酯进行萃取,精馏制备成品对氟苯甲醛。经过对氯化反应、水解反应、萃取条件进行筛选,得到最佳工艺条件:(1)氯化反应:反应温度95℃,m(N-氯代丁二酰亚胺)∶m(偶氮二异丁腈)∶m(对氟甲苯)=2.7∶0.1∶1;(2)水解反应:反应温度125~135℃,m(四丁基溴化铵)∶m(对氟二氯苄)=1∶1;(3)萃取:碳酸氢钠水溶液浓度为45%,m(乙酸乙酯)∶m(对氟苯甲醛)=0.5∶1。该工艺条件下,反应收率最佳,成品纯度可达到99.8%。Using p-fluorotoluene as raw material,N-chlorosuccinimide was used as chlorinating agent for chlorination,through dripping water,the hydrolysis was carried out under the action of tetrabutylammonium bromide as catalyst,the product was extracted with ethyl acetate,and the finished product p-fluorobenzaldehyde was prepared by rectifying.After screening the chlorination reaction,hydrolysis reaction and extraction conditions,the best technological conditions were obtained as follows:in the chlorination reaction,reaction temperature 95℃,m(N-chlorosuccinimide)∶m(azodiisobutyronitrile)∶m(p-fluorotoluene)=2.7∶0.1∶1;In the hydrolysis reaction,the reaction temperature 125~135℃,m(tetrabutylammonium bromide)∶m(p-fluorobenzyl dichloride)=1∶1;In the extraction,the mass fraction of sodium bicarbonate aqueous solution 45%,m(ethyl acetate)∶m(p-fluorobenzaldehyde)=0.5∶1.Under above conditions,the reaction yield was the best,and the purity of the finished product reached 99.8%.

关 键 词：对氟甲苯 N-氯代丁二酰亚胺 四丁基溴化铵 对氟苯甲醛 

分 类 号：TQ612.1[化学工程—精细化工]