磁性固体酸催化剂Fe_(3)O_(4)/C-SO_(3)H制备及表征  

Preparation and characterization of magnetic solid acid catalyst Fe_(3)O_(4)/C-SO_(3)H

作　　者：喻红梅[1] 华平[1] 李建华[1] 钱锋 Hongmei Yu;Ping Hua;Jianhua Li;Feng Qian(College of Chemistry and Chemical Engineering,Nantong University,Nantong,Jiangsu 226000,China)

机构地区：[1]南通大学化学化工学院,江苏南通226000

出　　处：《日用化学工业》2022年第4期396-403,共8页China Surfactant Detergent & Cosmetics

摘　　要：以四氧化三铁为磁核,生物质碳(葡萄糖、淀粉、蔗糖)为原料,采用先制备Fe_(3)O_(4)/C,再对其进行磺化的方法制备磁性碳基固体酸催化剂Fe_(3)O_(4)/C-SO_(3)H。以辛基葡萄糖苷的合成反应为探针,考察生物质碳种类、碳化温度、碳化时间、酸种类、磺化温度和磺化时间等因素对葡萄糖转化率和催化剂酸含量的影响。利用FT-IR、XRD、TG、SEM和振动样品磁强计(简称VSM)等对催化剂进行表征。结果表明Fe_(3)O_(4)/C-SO_(3)H的最佳制备条件为:以淀粉为生物质碳源,其用量为m(Fe_(3)O_(4))∶m(淀粉)=1∶10,碳化温度为190℃,碳化时间为8 h,以对甲苯磺酸为磺酸源,其质量比为m(Fe_(3)O_(4)/C)∶m(对甲苯磺酸)=1∶0.6,磺化温度为250℃,磺化时间为4 h。在上述条件下,催化剂酸含量为1.17 mmol/g,葡萄糖转化率为97.9%。表征结果也表明,具有良好晶型结构的Fe_(3)O_(4)在后续的碳化和磺化过程中,结构没有发生明显的变化,仍保留着良好的磁学性能。催化剂Fe_(3)O_(4)/C-SO_(3)H具备一定的孔道结构,热稳定性能良好。Fe_(3)O_(4)/C-SO_(3)H was a magnetic carbonbased solid acid catalyst.It was prepared with Fe_(3)O_(4),biomass carbon and sulfonic acid source,in which Fe_(3)O_(4)was the magnetic core and biomass carbon(glucose,starch,sucrose)was the raw material.Firstly,Fe_(3)O_(4)/C was prepared by the carbonization reaction taken place between Fe_(3)O_(4)and biomass.Then,sulfonation of Fe_(3)O_(4)/C with p-toluenesulfonic acid was carried out,and thus Fe_(3)O_(4)/C-SO_(3)H was prepared.The synthesis of octyl glucoside was used as a probe reaction.The activity of the catalyst was measured by the conversion of glucose and thecatalyst acid content.The influencing factors such as biomass carbon type,carbonization temperature,carbonization time,acid type,sulfonation temperature and sulfonation time were investigated.The catalyst was characterized by FT-IR,XRD,TG,SEM and Vibrating Sample Magnetometer(VSM).The results show that,the optimum preparation conditions of Fe_(3)O_(4)/C-SO_(3)H are as follows:Starch is the best biomass carbon source among glucose,starch and sucrose;the mass ratio of Fe_(3)O_(4)to starch is 1∶10;carbonization temperature is 190℃;carbonization time is 8 h;among the three sulfonic acid sources(p-toluenesulfonic acid,dodecylbenzene sulfonic acid and concentrated sulfuric acid),p-toluenesulfonic acid is the best;the mass ratio of Fe_(3)O_(4)/C to p-toluenesulfonic acid is 1∶0.6;the sulfonation temperature is 250℃;the sulfonation time is 4 h.Under the optimized conditions,the acid content of the catalyst is 1.17 mmol/g,and the glucose conversion is 97.9%.XRD results show that the crystal structure of magnetic Fe_(3)O_(4)particles does not significantly change after carbonization and sulfonation,and the catalyst still retains good magnetic properties.FT-IR analysis shows that sulfonic groups are successfully loaded on the carrier Fe_(3)O_(4)/C.Thermogravimetric analysis shows that Fe_(3)O_(4)/C-SO_(3)H has good thermal stability below 300℃.SEM shows that magnetic Fe_(3)O_(4)particles are irregular spheric

关 键 词：磁性催化剂 固体酸催化剂 辛基葡萄糖苷 

分 类 号：TQ423[化学工程]