不同形貌固体酸的纤维素乙酰化催化性能研究  

Investigation on Catalytic Performance of Cellulose Acetylation of Solid Acids with Different Morphologies

作　　者：贾冉冉 刘虎 佘洁 黄小川 李力成[1] JIA Ran-ran;LIU Hu;SHE Jie;HUANG Xiao-chuan;LI Li-cheng(College of Chemical Engineering,Nanjing Forestry University,Nanjing 210037,China)

机构地区：[1]南京林业大学化学工程学院,江苏南京210037

出　　处：《纤维素科学与技术》2022年第1期71-80,共10页Journal of Cellulose Science and Technology

基　　金：国家自然科学基金资助项目(031030182);国家自然科学基金面上项目(21978134);江苏省自然科学基金面上项目(K20191392)。

摘　　要：为了考察不同形貌的固体酸对纤维素乙酰化反应性能的影响,制备了微球状(NSP)、片状(NS)、棒状(NR)及颗粒状(NP)四种不同形貌的钛基硫酸促进型固体超强酸,将其用于纤维素乙酰化反应合成醋酸纤维素中。利用扫描电子显微镜(SEM)、X-射线衍射分析(XRD)、氮气吸脱附测试(BET)、傅里叶变换红外光谱(FT-IR)等技术对催化剂的形貌、晶体结构类型、比表面积及孔容、结构组分进行分析,利用XRD、FT-IR对产物醋酸纤维素(CA)的结构性质进行表征。酸碱滴定结果表明,上述不同形貌的钛基硫酸促进型固体超强酸材料催化合成的醋酸纤维素(CA)的取代度大小顺序为微球>片>棒>颗粒状固体酸,表明微球形貌的固体酸的催化性能最优。进一步考察反应温度及时间对催化合成CA的影响。结果表明,制备CA的最佳工艺为:2 g纤维素,8 mL醋酸酐,1 g固体超强酸催化剂,酯化反应温度65℃,反应时间为2 h。In order to investigate the influence of solid acids with different morphologies on the performance of acetylation of cellulose,four different morphologies of titanium-based sulfuric acid promoted solid acids with microspheres(NSP),slices(NS),rods(NR)and particles(NP)were prepared in this paper.Titanium-based sulfuric acid promoted solid super acid,which is used in cellulose acetylation reaction to synthesize cellulose acetate.Use scanning electron microscope(SEM),X-ray diffraction analysis(XRD),nitrogen adsorption and desorption test(BET),Fourier transform infrared spectroscopy(FT-IR)and other techniques to analyzed the morphology,crystal structure type and specific surface area,the pore volume and structural components of the catalyst,and the structural properties of the cellulose acetate(CA)were characterized by XRD and FT-IR.The acid-base titration results show that the order of substitution degree of cellulose acetate(CA)synthesized by the titanium-based sulfuric acid-promoted solid super acid materials with different morphologies is microspheres>slices>rods>particles solid acid.It shows that the catalytic performance of the solid acid with microspheres morphology is the best.Further study the effect of reaction temperature and time on the catalytic synthesis of CA.The results show that the best process for preparing CA is:2 g cellulose,8 mL acetic anhydride,1 g solid super acid catalyst,esterification temperature 65℃,reaction time 2 h.

关 键 词：乙酰化 氧化钛 形貌 固体酸 醋酸纤维素 

分 类 号：TQ352[化学工程]