固体超强酸SO_4^(2-)/ZrO_2-TiO_2催化合成α-萘乙酸甲酯

Synthetic Method of Methyl 1-Naphthylacetate on Complex Solid Super Acid Catalyst SO_4^(2-)/ZrO_2-TiO_2

采用固体超强酸SO42-/ZrO2-TiO2为催化剂,α-萘乙酸和甲醇为原料,结合甲醇精馏回收工艺,合成了α-萘乙酸甲酯(MENA)。催化剂制备和MENA合成最佳工艺条件为:硫酸浸渍液浓度为0.5～0.55mol/L,焙烧温度550℃～600℃,焙烧时间4.0h,催化剂用量为2.0%～2.5%(占总投料量质量分数),甲醇与萘乙酸投料比为7.0∶1(体积比),回流反应,反应时间2.5h,产品收率达93.6%,催化剂重复使用7次,其产品收率仍在90%以上,催化剂再生容易。

A complex catalyst system SO4^2-/ZrO2-TiO2 was prepared and used in the reaction for the synthesis of methyl 1-naphthylacetate （MENA） with the material of naphthylacetic acid and methanol and the process of methanol distillation recovery. The optimal conditions were as follows： the concentration sulphuric acid impregnation solution 0.5-0.55 mol/L, calcinations temperature 550-600 ℃, calcinations time 4.0 h, catalyst dosage 2.0-2.5% （the mass fraction of the total material）, ratio of methanol and naphthylacetic acid was 7.0 ： 1, reflux reaction time about 1.5 h, the yield of ester is 93.6%, after the catalyst reuse seven times, the yield of ester is above 90%. The catalyst regenerative is easy.