改性分子筛催化果糖脱水制5-羟甲基糠醛  

Modified molecular sieves for catalytic dehydration of fructose to 5-hydroxymethylfurfural

作　　者：刘中海 高赛男 秦冬玲 杨刚 LIU Zhonghai;GAO Sainan;QIN Dongling;YANG Gang(State Key Laboratory of Materials-Oriented Chemical Engineering,College of Chemical Engineering,Nanjing Tech University,Nanjing 211800,China)

机构地区：[1]南京工业大学化工学院材料化学工程国家重点实验室

出　　处：《南京工业大学学报（自然科学版）》2020年第1期56-61,共6页Journal of Nanjing Tech University(Natural Science Edition)

基　　金：国家科技支撑计划(2013BAE11B03)

摘　　要：采用离子交换法制备Sn、Cu、Fe改性的SAPO 34分子筛,通过扫描电子显微镜(SEM)、X线衍射仪(XRD)、N 2物理吸附、NH 3程序升温脱附(NH 3 TPD)和X线荧光光谱仪(XRF)对改性后的催化剂进行形貌和结构表征。将改性前后的催化剂用于果糖脱水制5羟甲基糠醛(5 HMF)反应中,考察反应时间、反应介质、催化剂使用量对产物产率的影响。结果表明:改性后的样品表面聚集了无定形颗粒,结晶度、孔容和酸性有所下降;以Sn SAPO 34作为催化剂,在30 mL二甲基亚砜溶剂中添加0.25 g催化剂、1 g果糖,反应1 h后,转化率可达99.5%,5 HMF的产率为47.7%。在最优条件下将催化剂重复使用5次,产率有所下降,经过分离焙烧后再使用,产率可恢复至原来的水平。Three kinds of metal Sn,Cu and Fe modified SAPO-34 were prepared with ion exchange.The samples were characterized by scanning electron microscope(SEM),X-ray diffraction(XRD),N 2 physical adsorption,NH 3 temperature programmed desorption(NH 3-TPD)and X ray fluorescence(XRF).The modified molecular sieves were applied to the production of 5-hydroxymethylfurfural(5-HMF)from fructose.The influence of different experimental variables,such as time,solvent and catalyst dosage were investigated.Results showed that amorphous particles aggregated on the surface of the modified samples,and the crystalline and acidity of the modified samples were reduced.In 30 mL dimethyl sulfoxide(DMSO)with 0.25 g Sn-SAPO-34 and 1 g fructose,the yield of 5-HMF was 47.7%and conversion rate of fructose was 99.5%after 1 h.The catalysts could be recycled and reused for five runs with little loss of catalytic activity,and could be resued with separation and calcination.

关 键 词：SAPO34分子筛 分子筛改性 果糖脱水 5羟甲基糠醛 

分 类 号：TQ426.6[化学工程]