摘要
选择硅酸四乙酯为硅源,在室温和pH=3.5条件下合成具有较低硅铝比的MCM-41型分子筛。以其为基础载体,采用浸渍和焙烧法制备含钛分子筛型固体超强酸。低温N2吸附、IR、SEM和XRD分析表明,铝已进入分子筛的骨架中;Hammett指示剂测定表明,酸强度H0<-14.52。以戊酸丁酯合成为探针反应,考察了催化剂的催化性能。结果表明,反应温度为138℃、催化剂用量为反应物总质量的1%、丁醇和戊酸的物质的量比为3∶1条件下,产品转化率达98.5%。
Al-MCM-41 mesoporous zeolite with low Si/Al ratio was prepared under acidic atmosphere （pH = 3.5 ） at room temperature, using tetraethyl orthosilicate as the silica source and cethyhrimethyl ammonium bromide as the template. SO4^2-/TiO2-Al-MCM-41 was prepared by impregnation followed by calcination, using the as-synthesized Al-MCM-41 mesoporous zeolite as the carrier, and characterized by powder XRD, low-temperature N2-adsorption-desorption, IR and SEM. The results showed that aluminum ions were successfully incorporated into framework of the mesoporours material. Hammett acidity of the SO4^2-/TiO2-Al-MCM-41 was H0 〈 - 14.52. Catalytic behavior of the SO4^2-/TiO2-Al-MCM-41 solid superacid were investigated using esterification of valeric acid and n-butanol as the probe reaction. Product yield of 98.5% was attained under the following condition： reaction temperature 138 ℃, catalyst dosage = 1% mass of the reactants, n-butyl alcohol to valeric acid mole ratio of 2.5： 1.
出处
《工业催化》
CAS
2010年第1期36-41,共6页
Industrial Catalysis
