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作 者:谭云方[1] 黄祖强[1] 张燕娟[2] 胡华宇[1] 刘小萍[1] 陈燕萌[1] 黄红铭[1]
机构地区:[1]广西大学化学化工学院,南宁530004 [2]广西化工研究院,南宁530001
出 处:《湖北农业科学》2013年第4期906-909,共4页Hubei Agricultural Sciences
基 金:国家自然科学基金项目(51163002);广西研究生教育创新计划资助项目(105931003022)
摘 要:以甘蔗浆粕纤维素为原料、月桂酸为酯化剂,以自制的高能效搅拌磨为反应器,通过边机械活化边反应的方法固相合成了月桂酸纤维素酯。以月桂酸纤维素酯的取代度为评价指标,考察反应温度、催化剂用量、反应物配比、助剂用量、反应时间对固相酯化反应的影响,并利用傅立叶红外(FT-IR)光谱对产品和原料的结构进行分析,证实了酯化产物的生成。结果表明,适宜的机械活化固相酯化合成工艺条件为甘蔗浆粕纤维素10.00 g,催化剂用量1.00∶0.30,反应物配比1∶4,助剂用量1.00∶3.20,反应温度45℃,反应时间60 min。在该条件下,获得了取代度为1.94的月桂酸纤维素酯。Cellulose laurate were synthesized by mechanical activation of solid phase reaction using sugarcane pulp cellulose as starting material,laurate as esterifying agent,and self-designed stirring-type ball mill as reactor.The effects of activation temperature,activation time,proportion of reactant,dosage of auxiliary and catalyst,etc.were investigated respectively by using the degree of substitution(DS) of cellulose laurate as evaluating parameter.Then the structure of the products and starting materials was characterized by fourier transform infrared spectroscopy(FTIR);and the results proved that esterification products were successfully synthesized.The results indicated that the suitable conditions for producing cellulose laurate under mechanical activation of solid phase reaction were,the mass of sugarcane pulp cellulose was 10.00 g;the molar number of catalyst sodium hypophosphite was 30% of cellulose dehydration glucoside unit;the molar ratio of reactants was 1∶4;the molar ratio of cellulose dehydration glucoside unit and zinc chloride was 1.00∶3.20;the esterification reaction temperature was 45 ℃;and the esterification reaction time was 60 min.Under the optimized reaction conditions,the DS of cellulose laurate was 1.94.
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