有序介孔炭的合成及其磺化制备固体酸

Synthesis and Sulfonation of Ordered Mesoporous Carbons for Solid Acid Catalyst

对于高酸值油脂原料,在酯交换反应制备生物柴油前需对其进行降酸处理,然而常用的H_2SO_4催化降酸法存在设备腐蚀和环境污染等问题。采用软模板法合成有序介孔炭(OMCs),利用TEM、SAXRD及N_2吸附/脱附等对其进行结构性能表征,探讨了模板剂与前驱体的质量比、热聚合时间、煅烧温度等工艺条件对OMC介孔结构的影响,获得了具有高度有序二维六方孔道结构的介孔炭,孔径3~4 nm,比表面积>600 m^2/g。进而通过自由基加成法对OMC磺化制得磺化介孔炭,其介孔有序性能够得到很好的保持。合成的磺化介孔炭将作为固体酸催化剂用于后续高酸值油脂制备生物柴油的降酸过程。

For oil materials with high acid values,deacidification is necessary before transesterification for biodiesel preparation. However,the conventional method with H_2SO_4 as a catalyst is always accompanied with equipment corrosion and environmental pollution problems. In this paper ordered mesoporous carbons( OMCs) were synthesized by soft template method. Transmission electron microscope( TEM),small angle X-ray diffraction( SAXRD) and nitrogen adsorption-desorption were applied to investigate the influences of the mass ratio of the template agent to the precursor,thermal polymerization time and calcination temperature on the mesostructures of OMCs materials. Highly-Ordered mesoporous carbons with 2D hexagonal structure were obtained,possessing 3—4 nm pore diameter and more than 600 m^2/ g BET specific surface areas. OMCs were then sulfonated through benzenesulfonic acid-containing aryl radical in situ generated from the reaction of 4-aminobenzenesulfonic acid and isoamyl nitrite. The sulfonated OMCs can be used in deacidification of crude oil with high acid value for biodiesel production.