负载型固体碱NaF/NaX的制取及其在DHA制备中的应用

Preparation of NaF/NaX Solid Base Catalyst and Its Applications in Synthesis of Dehydroacetic Acid

运用浸渍法制取了固体碱NaF/NaX,并以NaF/NaX为催化剂、以乙酰乙酸乙酯为原料制备了脱氢乙酸.分析讨论了负载量、煅烧温度、煅烧时间、催化剂用量、反应温度和反应时间对脱氢乙酸产率的影响.结果表明,制取NaF/NaX的最佳条件是:NaF负载量20%、煅烧温度600℃、煅烧时间7 h;制备脱氢乙酸的最佳条件是:催化剂用量0.02 g、温度210℃、反应时间7 h,在此条件下制备脱氢乙酸,产率可达82.5%.

The solid base catalyst NaF/NaX was synthesized by using impregnation method, dehydroacetic acid was prepared from ethylacetoacetate. The effects of loading amount, calcination temperature, calcination time, the amount of catalyst, reaction temperature and time on yield of dehydroacetic acid were analyzed. The results indicated that the best conditions of preparing NaF/NaX were as follows： loading amount 20%, calcination temperature 600 ℃ and calcination time 7 h. The best conditions of preparing dehydroacetic acid were as follows ： the amount of catalyst 0.02 g, temperature 210 ℃ and reaction time 7 h. Under this condition, the yield of dehydroacetic acid reached 82.5%.