Chen Weiqing, Wu Zhaoji, Peng Ruoxue, Wu Wenjuan, Li Xiaonan, Cao Dan, Zhang Zhigang, Niu Kui
College of Chemical Engineering, Hebei Normal University of Science & Technology Qinhuangdao China 066600
Hebei Key Laboratory of Active Components and Functions in Natural Products Qinhuangdao China 066600
RSC Adv. 2023 Feb 17;13(9):6002-6009. doi: 10.1039/d2ra07947j. eCollection 2023 Feb 14.
Using a simple method of impregnation and then calcination, diatomite supported binary transition metal sulfates (Fe and Zr, designated as Fe(SO)&Zr(SO)@diatomite) were prepared and used as a catalyst in the preparation of renewable biofuels. The synthesised Fe(SO)&Zr(SO)@diatomite catalyst (Fe(SO) : Zr(SO) : diatomite = 1 : 2 : 6, mass ratio) was thoroughly characterised using transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier-transform infrared (FTIR) spectroscopy, microbeam X-ray fluorescence (μ-XRF) spectroscopy and thermogravimetric analysis (TG). The results demonstrated that the sulfate was successfully loaded onto the diatomite with a uniform distribution. The N adsorption/desorption analysis indicated that the catalyst's specific surface area was 1.54 m g. The catalyst exhibited outstanding performance in the preparation of renewable biofuel (biodiesel) from waste fatty acids and the optimal parameters were methanol-to-oil 1.25 : 1, reaction temperature 70 °C, catalyst concentration 10 wt%, reaction time 4 h. The conversion was found to reach 98.90% under optimal parameters, which is better than that of Fe(SO)·HO, Zr(SO)·4HO, Fe(SO)@diatomite and Zr(SO)@diatomite. Moreover, the catalyst can be recycled by simple filtration and reused for three cycles after regeneration without noticeable reduction in catalytic activity.
采用简单的浸渍然后煅烧的方法,制备了硅藻土负载的二元过渡金属硫酸盐(铁和锆,命名为Fe(SO)₄&Zr(SO)₄@硅藻土),并将其用作制备可再生生物燃料的催化剂。使用透射电子显微镜(TEM)、X射线衍射(XRD)、傅里叶变换红外(FTIR)光谱、微束X射线荧光(μ-XRF)光谱和热重分析(TG)对合成的Fe(SO)₄&Zr(SO)₄@硅藻土催化剂(Fe(SO)₄ : Zr(SO)₄ : 硅藻土 = 1 : 2 : 6,质量比)进行了全面表征。结果表明,硫酸盐成功负载在硅藻土上且分布均匀。N吸附/脱附分析表明该催化剂的比表面积为1.54 m²/g。该催化剂在由废脂肪酸制备可再生生物燃料(生物柴油)方面表现出优异性能,最佳参数为甲醇与油的比例为1.25 : 1、反应温度70°C、催化剂浓度10 wt%、反应时间4小时。发现在最佳参数下转化率达到98.90%,优于Fe(SO)₄·H₂O、Zr(SO)₄·4H₂O、Fe(SO)₄@硅藻土和Zr(SO)₄@硅藻土。此外,该催化剂可通过简单过滤回收,并在再生后重复使用三个循环,催化活性无明显降低。