超声波辅助下K_2O/C催化制备纤维低聚糖脂肪酸酯表面活性剂  

Ultrasonic- assisted Synthesis of Cellulosic Oligosaccharide Esters Surfactant Catalyzed by K_2O/C

作　　者：王奎[1,2,3,4,5] 蒋剑春[1,2,3,4,5] 卢辛成[1,2,3,4] 徐俊明[1,2,3,4,5] 梁馨予[1,2,3,4] 

机构地区：[1]中国林业科学研究院林产化学工业研究所 [2]生物质化学利用国家工程实验室 [3]国家林业局林产化学工程重点开放性实验室 [4]江苏省生物质能源与材料重点实验室,江苏南京210042 [5]中国林业科学研究院林业新技术研究所,北京100091

出　　处：《林产化学与工业》2015年第4期72-78,共7页Chemistry and Industry of Forest Products

基　　金：中国林科院林业新技术所基本科研业务费专项资金(CAFINT2013C05)

摘　　要：采用真空浸渍法制备炭基固体碱催化剂K2O/C,并在超声波辅助条件下,利用制备的K2O/C催化纤维低聚糖与油酸甲酯制备纤维低聚糖脂肪酸酯表面活性剂。选取L9(34)正交试验确定制备K2O/C催化剂的最佳条件为:炭基载体平均孔径为2.87 nm,K2CO3与炭基载体的质量比值为0.5,真空浸渍后,450℃下煅烧2 h。考察了超声波辅助下超声波时间、超声波频率、反应温度、反应时间和催化剂用量对产品得率的影响。研究发现:在20 k Hz,150 W超声功率下,将物质的量之比为2∶1的油酸甲酯和纤维低聚糖(水溶液)超声波作用15 min,形成均一稳定的乳化体系,真空条件下,移除体系中的水分后,加入占总物料量5%的K2O/C催化剂,125℃下反应2 h,纤维低聚糖脂肪酸酯的最高得率为85.6%,其酯化度为18.8%,亲水亲油平衡值(HLB)为9.89,表面张力为32.1 m N/m,乳化力为28.1%,硬水稳定性4级。The solid base catalyst K2O/C was prepared by the vacuum impregnation method. The orthogonal experiment was employed to optimize the preparation condition. The results indicated that the optimal reaction parameters were carbon carrier with average pore size 2.87 nm, K2CO3/C mass ratio 0.5, catalyst calcination temperature 450 ℃, and calcination time 2 h. The prepared catalyst K2O/C was adopted to catalyze the transesterification reaction of cellulosic oligosaccharide esters from cellulosic oligosaccharide and methyl oleate under ultrasonic assistance. The optimum conditions were obtained as follows： the ultrasonic frequency 20 kHz, the ultrasonic power 150 W, treatment time 15 min, the mole ratio of methyl oleate to cellulosic oligosaccharide esters 2 ： 1, the mass fraction of K2O/C 5% , the reaction temperature 125℃, and the reaction time 2 h. Under these conditions, the yield of cellulosic oligosaeeharide esters reached 85.6%. The synthesized product has esterification degree 18.8% , HLB 9.89, surface tension 32.1 mN/m, and the emulsifying ability 28.1%. The product showed good performance on surface tension, emulsion and stability in hard water.

关 键 词：K2O/C 纤维低聚糖 表面活性剂 超声波辅助 

分 类 号：TQ35[化学工程]