摘要
以乙酰乙酸纤维素酯为主链,葡萄糖、纤维二糖和纤维素纳米晶为支链,利用Biginelli反应成功合成了3种糖支链纤维素。通过核磁共振波谱、红外光谱、元素分析和X射线衍射对糖支链纤维素的分子结构进行了表征,结果表明:接枝点处新生成的官能团C=O(C=O)-NH、C—N、—NH的出现证明了葡萄糖支化纤维素、纤维二糖支化纤维素和纤维素支化纤维素的成功制备。单因素试验结果表明:合成3种糖支链纤维素的最佳反应条件为溶剂pH值5~6、反应时间10 h、反应温度70℃。其中,糖支链为葡萄糖(支链聚合度为1)且用量为0.6,主链取代度为0.87时,合成的糖支链纤维素葡萄糖支化纤维素的支化度最高,可达(11.82±0.57)%,产率可达(90.70±1.82)%;糖支链为纤维二糖(支链聚合度为2)且用量为0.4,主链取代度为0.87时,合成的糖支链纤维素纤维二糖支化纤维素的支化度最高,可达(7.30±0.11)%,产率可达(90.25±2.15)%;糖支链为纤维素纳米晶(支链聚合度为100)且用量为0.01,主链取代度为0.87时,合成的糖支链纤维素纤维素支化纤维素的支化度最高,可达(0.68±0.09)%,产率可达(92.45±1.25)%。
Using cellulose acetoacetate as main chain and glucose,cellobiose and cellulose nanocrystals as branch chain,saccharide branched cellulose was synthesized by Biginelli reaction.The molecular structure of saccharide branched cellulose was characterized by NMR spectrum,Infrared spectroscopy,Elemental analysis and X-ray diffraction.The results showed that the emergence of new functional groups of C=O(C=O)-NH,C—N and—NH at the grafting point proved the successful preparation of glucose branched cellulose,cellobiose branched cellulose and cellulose branched cellulose.The results of single factor experiment showed that the optimum reaction conditions for the synthesis of the three kinds of saccharide branched cellulose were solvent pH of 5-6,reaction time of 10 h and reaction temperature of 70℃.Among them,when the saccharide branch chain was glucose(branch chain degree of polymerization was 1)and the consumption was 0.6,the main chain degree of substitution was 0.87,the degree of branching of glucose branched cellulose was the highest,up to(11.82±0.57)%and the yield reached(90.70±1.82)%.When the saccharide branch chain was cellobiose(branch chain degree of polymerization was 2)and the consumption was 0.4,the main chain degree of substitution was 0.87,the degree of branching of cellobiose branched cellulose was the highest,up to(7.30±0.11)%and the yield reached(90.25±2.15)%.When the saccharide branch chain was cellulose nanocrystal(branch chain degree of polymerization was 100)and the consumption was 0.01,the main chain degree of substitution was 0.87,the degree of branching of cellobiose branched cellulose was the highest,up to(0.68±0.09)%and the yield reached(92.45±1.25)%.
作者
刘煜
祁海松
LIU Yu;QI Haisong(State Key Laboratory of Pulp and Paper Engineering,South China University of Technology,Guangzhou 510641,China)
出处
《生物质化学工程》
CAS
2024年第5期21-27,共7页
Biomass Chemical Engineering
基金
国家自然科学基金资助项目(22278158)。
