摘要
以纳米氧化物为前驱体制备的固体超强酸催化剂SO24-/ZrO2,其Hammett酸强度常数小于-12.14。将SO24-/ZrO2用于催化苯甲醛与乙酸酐的缩醛反应,经红外光谱、气相色谱、核磁、熔点测定证明得到的缩醛具有较高的纯度。通过均匀设计实验,考察催化剂制备过程中焙烧温度、硫酸浓度、浸泡时间和活化温度对缩醛产率的影响。优化出缩醛产率最高的催化剂制备条件为:焙烧温度为300℃,浸渍液中硫酸的浓度为4.5 mol/L,浸泡时间为1.0 h,活化温度为305℃,缩醛产率为93.6%。红外光谱和热重分析表明,SO24-/ZrO2超强酸中SO24-吸附量大。重复实验表明使用10次后,SO24-/ZrO2仍保持较高的催化活性,且催化剂易处理,易再生。
By using nanometer oxides as precursor, solid supcracid catalyst SO4^2-/ZrO2 with Hammett constant less than - 12.14 was prepared. The catalyst SO4^2-/ZrO2 was used for the acetalization of benzaldchyde with acetic anhydride. The resuhs of IR,GC, NMP, and inching poinht measurement show that the purity of the target product of acetalization is very high. The influenee of calcining temperature, concentration of sulphuric acid, immersing time and activating temperature on the yield of aldehyde acetal was investigated by uniform design. The optimum conditions for obtaining the highest yicld of aldehyde acctal are as follows： the calcining temperature is 300℃, concentration of sulphuric acid in immersion liquid is 4.5 mol/L, immersing time is 1 hour, activating temperature is 305℃. The yield of aldehyde acctal is 93.6 %. The analysis of IR and TG indicates that the absorptive capacity of SO4^2- on SO4^2-/ZrO2 is large. The reusing experiment of catalyst shows that the catalyst can be reused more than ten times with high catalytic activity. Its treatment and regeneration are easy.
出处
《辽宁石油化工大学学报》
CAS
2006年第1期34-37,共4页
Journal of Liaoning Petrochemical University
关键词
固体超强酸
催化
缩醛反应
Solid superacidity
Catalysis
Acetalization
