SO_4~(2-)/TiO_2-WO_3催化1,4-丁二醇液相脱水环化合成四氢呋喃

以钛酸四丁酯为原料,十六烷基三甲基溴化铵(CTAB)作模板剂,通过水热法制备出TiO_2,并进一步制得SO_4~(2-)/TiO_2-WO_3固体超强酸,采用IR、XRD、BET对其进行了表征。以催化1,4-丁二醇脱水制备四氢呋喃为探针反应,通过正交实验确定了反应的最佳条件:反应温度180～190℃,反应时间45 min,w(催化剂)= 4.6%(相对1,4丁二醇质量),四氢呋喃的收率可达91.5%。催化剂重复使用3次,收率仍可达87.0%,同时对反应机理进行了探讨。

DEHYDRATION OF 1,4-BUTANEDIOL TO TETRAHYDROFURAN CATALYZED BY SOLID SUPERACID SO_4~(2-)/TiO_2-WO_3

TiO_2 was prepared by a hydrothermal method with tetrabutyl titanate and cetyltrimethylam-monium bromide.The solid superacid SO_4~(2-)/TiO_2-WO_3 was obtained by impregnating the mixture of TiO_2 and H_2WO_4(mass ratio of 10:1) with 1.0 mol/L H_2SO_4.The catalyst was studied in the catalytic synthesis of tetrahydrofuran from 1,4-butanediol and characterized by IR,XRD and BET.The optimal reaction conditions were obtained by orthogonally arranged experiments:mass ratio of 1,4-butanediol to catalyst 100:4.6,reaction temperature 180-190℃and reaction time 45 min.Under these conditions,the yield of tetrahydrofuran reached 91.5%.The catalyst can be reused for 3 times with the yield above 87.0%.The possible mechanism of the reaction was studied.This approach provides a green,safe,operation simple and highly active dehydrogenation process to produce THF.