以纤维素和硝酸铁为原料,发烟硫酸为磺酸化试剂,采用热解法合成了磁性碳基磺酸化固体酸催化剂(Fe/C-SO3H).利用扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)、X射线光电子能谱(XPS)、傅里叶变换红外(FT-IR)光谱仪和振动样品磁强计(VSM)等手段对催化剂进行了表征,评价了催化剂在纤维素水解反应中的催化活性.结果表明,Fe是以γ-Fe2O3的形式存在于碳本体中,催化剂呈现超顺磁性.对于纤维素的水解反应,在优化条件下,纤维素的转化率可达40.6%.此外,催化剂可稳定分散于反应体系中,并在外加磁场作用下可快速与反应体系分离.但催化剂重复使用时催化活性有所下降,其失活原因经初步认定是由于表面部分磺酸基团在反应过程中脱落.
Magnetic sulfonated carbon-based solid acid catalysts (Fe/C-SO3H) were prepared by the pyrolysis of cellulose and subsequent sulfonation.The catalyst samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FT-IR) spectroscopy, and vibrating sample magnetometry (VSM).Their catalytic properties for the hydrolysis of cellulose were investigated.Results show that Fe exists in the carbon body in the form of γ-Fe2O3 and the Fe/C-SO3H catalyst has superparamagnetic properties.In the hydrolysis reaction, cellulose conversion reached 40.6% over Fe/C-SO3H under optimal conditions.Furthermore, the catalyst could be steadily dispersed in the reaction mixture and be separated using an externally applied magnetic field.However, the catalytic performance dropped after the first run.The reason for deactivation is deduced to be a reduction in the amount of sulfonic acid groups on the surface of the catalyst.