以固体超强酸SO_4^(2-)/ZrO_2-Fe_2O_3催化合成醋酸异戊酯

Catalytic Synthesis of Isoamyl Acetate by Solid Superacid SO_4^(2-)/ZrO_2-Fe_2O_3

以合成醋酸异戊酯为探针反应,筛选出制备固体超强酸SO2-4 /ZrO2- Fe2O3 (SZF -1 )的最佳工艺条件为:ZrOCl2·8H2O9. 7g, FeCl3·6H2O16. 2g, 常温陈化24h, 0. 5mol·L-1 H2SO4 (15mL·g-1 )浸泡5h, 550℃焙烧3h。以SZF 1为催化剂合成醋酸异戊酯的反应条件为:异戊醇200mmol, n(异戊醇)∶n(醋酸) =1. 0∶1. 3, SZF -1 1g(反应物总质量的3% ), 环己烷15mL, 回流反应3h, 酯化率93. 47%。催化剂连续使用6次后酯化率仍在70%以上。

The optimum conditions for preparing solid superacid acid SO 2 - _ _ 4/ZrO_ 2-Fe_ 2O_ 3(SZF-1) were found by a proble reaction of synthesis of isoamyl acetate that ZrOCl_ 2·8H_ 2O was 9.7 g, FeCl_ 3· 6H_ 2O was 16.2g, aging at room temperature for 24 h, marinating for 5 h in 0.5 mol·L -1 H_ 2SO_ 4(15 mL·g -1 ), calcinating at 550 ℃ for 3 h. The synthetic conditions of isoamyl acetate using SZF-1 as a catalyst were as follows: isoamylol was 200 mmol, the mole ratio of isoamylol and acetic acid was 1.0 ∶1.3, SZF-1 was 1g(3% of total reactants mass), cyclohexane was 15 mL, refluxing for 3 h. The esterification rate was 93.47% under the reaction conditions and was still over 70% when the catalyst was reused for 6 times.