摘要
以凹凸棒黏土(ATP)为载体,采用回流吸附法制备了AlCl3负载型固体酸催化剂AlCl3/ATP,并将其用于催化阿司匹林合成反应。利用红外光谱、X射线粉末衍射、比表面(BET)、能谱(EDS)和Hammett指示剂等测试技术对催化剂结构、组成和酸强度进行了表征。以催化合成阿司匹林收率为考察指标,对影响其催化性能的凹土酸处理浓度、热活化温度、催化剂用量和AlCl3负载量进行优化,并比较了载体和负载前后催化剂的催化性能。结果表明,ATP经10 mol/L盐酸室温酸化12 h,300℃热活化2 h后对AlCl3的负载量达1.18 mmol/g,当AlCl3/ATP用量为水杨酸质量的5%时,其催化阿司匹林合成反应收率达92.5%,高于未负载的AlCl3催化剂及载体本身,且该催化剂重复使用多次仍可保持相当的活性。
Immobilized AlCl3 catalyst（AlCl3/ATP） was prepared through solvent refluxing and adsorption method with attapulgite as the support and then used in the synthesis of aspirin.The catalyst was characterized by Fourier transform infrared spectroscopy（FT-IR）,X-ray diffraction（XRD）,specific surface area（BET）,X-ray energy dispersive spectrometry（EDS） and Hammett indicators.Factors influencing the catalytic properties such as concentration of hydrochloric acid,heat-treated temperature,AlCl3 loading and amount of catalyst were optimized according to the yield of aspirin.The catalytic properties of the catalysts and the support were compared before and after loading.The results show that the amount of AlCl3 loading on ATP reached 1.18 mmol/g after ATP acidified with 10 mol/L HCl for 12 h at room temperature and then heat-treated under 300 ℃ for 2 h.The yield of aspirin catalyzed by AlCl3/ATP reaches 92.5% when the dosage of the AlCl3/ATP is 5% mass fraction of salicylic acid,which is higher than that of unloaded AlCl3 and the support itself.The catalyst also exhibits excellent catalytic stability within 5 times reused.
出处
《应用化学》
CAS
CSCD
北大核心
2011年第7期791-797,共7页
Chinese Journal of Applied Chemistry
基金
江苏省科技厅工业支撑计划资助项目(BE2009098)
