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本文以四氯化钛为原料,采用凝胶-溶胶法和浸渍法制备纳米固体超强酸TiO2/SO42-。用透射电镜TEM对其进行表征,粒径达到50~100nm。用红外光谱研究SO42-在金属氧化物固体表面上的存在形态与结构形式,表明该催化剂具有催化活性。以纳米固体超强酸TiO2/SO42-为催化剂,研究由对羟基苯甲酸与异丁醇直接酯化合成尼泊金异丁酯。考察了醇酸物质的量比、催化剂用量和反应时间对尼泊金异丁酯收率的影响,并确定适宜工艺条件:醇酸物质的量比为4∶1、催化剂用量占反应物总质量的3.5%、反应时间4h和反应温度120℃,尼泊金异丁酯的收率可达到62.1%。
In this paper, titanium tetrachloride as raw material, using gel-sol method and impregnation method to prepare nano solid superacid TiO2 / SO42-. Characterized by TEM, the particle size reached 50 ~ 100nm. The existence and structure of SO42- on the solid surface of metal oxide were studied by IR spectroscopy, indicating that the catalyst has catalytic activity. Nano-isobutyl ester was synthesized by direct esterification of p-hydroxybenzoic acid and isobutanol with nano-solid superacid TiO2 / SO42- as catalyst. The effects of alkyd ratio, catalyst amount and reaction time on the yield of isobutylparaben were investigated. The optimum technological conditions were determined as follows: the molar ratio of alkyd to acid was 4:1, the amount of catalyst to the total mass of reactants 3.5%, reaction time 4h and reaction temperature 120 ℃, the yield of isobutyl paraben can reach 62.1%.