超声波辅助下K2O/C催化制备纤维低聚糖脂肪酸酯表面活性剂

doi:10.3969/j.issn.0253-2417.2015.04.012

林产化学与工业 ›› 2015, Vol. 35 ›› Issue (4): 72-78.doi: 10.3969/j.issn.0253-2417.2015.04.012

超声波辅助下K₂O/C催化制备纤维低聚糖脂肪酸酯表面活性剂

王奎^1,2, 蒋剑春^1,2, 卢辛成¹, 徐俊明^1,2, 梁馨予¹

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

收稿日期:2014-12-19 出版日期:2015-08-25 发布日期:2015-08-29
通讯作者: 蒋剑春(1955—),男,研究员,博士,博士生导师,主要从事生物质能源和炭材料的研究开发工作;E-mail:bio-energy@163.com。 E-mail:bio-energy@163.com
作者简介:王奎(1985—),男,助理研究员,博士,研究方向为天然多糖化学利用;E-mail:way910@163.com
基金资助:
中国林科院林业新技术所基本科研业务费专项资金(CAFINT2013C05)

Ultrasonic-assisted Synthesis of Cellulosic Oligosaccharide Esters Surfactant Catalyzed by K₂O/C

WANG Kui^1,2, JIANG Jian-chun^1,2, LU Xin-cheng¹, XU Jun-ming^1,2, LIANG Xin-yu¹

1. Institute of Chemical Industy of Forest Products, CAF;National Engineering Lab.for Biomass Chemical Utilization; Key and Open Lab.of Forest Chemical Engineering, SFA;Key Lab.of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China;
2. Research Institute of Forestry New Technology, CAF, Beijing 100091, China

Received:2014-12-19 Online:2015-08-25 Published:2015-08-29

摘要/Abstract

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 kHz,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 mN/m,乳化力为28.1%,硬水稳定性4级。

关键词: K₂O/C, 纤维低聚糖, 表面活性剂, 超声波辅助

Abstract: 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 oligosaccharide 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.

Key words: K₂O/C, cellulosic oligosaccharide, surfactant, ultrasonic-assisted

中图分类号:

TQ35

王奎, 蒋剑春, 卢辛成, 徐俊明, 梁馨予. 超声波辅助下K₂O/C催化制备纤维低聚糖脂肪酸酯表面活性剂[J]. 林产化学与工业, 2015, 35(4): 72-78.

WANG Kui, JIANG Jian-chun, LU Xin-cheng, XU Jun-ming, LIANG Xin-yu. Ultrasonic-assisted Synthesis of Cellulosic Oligosaccharide Esters Surfactant Catalyzed by K₂O/C[J]. Chemistry and Industry of Forest Products, 2015, 35(4): 72-78.

参考文献

[1] 金谷.表面活性剂化学[M].合肥:中国科学技术大学出版社,2008. JIN Gu.Chemistry of Surfactant[M].Hefei:University of Science and Technology of China Press,2008.
[2] FOLEY P,AZADEH K P,BEACH E S,et al.Drivation and synthesis of renewable surfactants[J].Chemical Society Reviews,2012,41(4):1499-1518.
[3] NETA N S,TEIXEIRA J A,RODRIGUES L R.Sugar ester surfactants:Enzymatic synthesis and applications in food industry[J].Critical Reviews in Food Science and Nutritio,2015,55(5):595-610.
[4] HOLMBERG K.Natural surfactants[J].Current Opinion in Colloid & Interface Science,2001,6(2):148-159.
[5] 李延科.糖基表面活性剂蔗糖酯的研究[D].大连:大连理工大学博士学位论文,2004. LI Yan-ke.Study on sugar-based surfactant:Sucrose esters[D].Dalian:Doctoral Dissertation of Dalian University of Science and Technology,2004.
[6] LIU Song-bai,SANG Ruo-cheng,HONG Shan,et al.A novel type of highly effective nonionic gemini alkyl o-gluscoside surfacatant:A versatile strategy of design[J].Langmuir,2013,29(27):8511-8516.
[7] OFTRING A,KAPPES E,BAUR R,et al.Alkyl mono- and polyglucoside ether carboxylates and their preparation and use thereof:US,5179201[P].1993-01-12.
[8] SHI Yu-gang,LI Jian-rong,CHU Yen-ho.Enzyme-catalyzed regioselective synthesis of sucrose-based esters[J].Journal of Chemical Technology and Biotechnology,2011,86(12):1457-1468.
[9] PENG Lin-cai,LIN Lu,LI Hui,et al.Conversion of carbohydrates biomass into levulinate esters using heterogeneous catalysts[J].Applied Energy,2011,88(12):4590- 4596.
[10] WANG Kui,XIE Xin-feng,SI Zhan,et al.Microwave assisted hydrolysis of holocellulose catalyzed with sulfonated car derived from lignin-rich residue[J/OL].Advances in Materials Science and Engineering[2012-12-03].http://www.hindawi.com/journds/amse/aa/106137.
[11] 刘雪梅,蒋剑春,孙康,等.热解活化法制备微孔发达椰壳活性炭及其吸附性能研究[J].林产化学与工业,2012,32(2):126-130. LIU Xue-mei,JIANG Jian-chun,SUN Kang,et al.Preparation and adsorption properties of activated carbon with developed micropore from coconut shell by pyrolysis activation[J].Chemistry and Industry of Forest Products,2012,32(2):126-130.
[12] 卢辛成,蒋剑春,孙康,等.磷酸活化稻秆制备中孔活性炭的研究[J].林产化学与工业,2013,33(4):43-47. LU Xin-cheng,JIANG Jian-chun,SUN Kang,et al.Preparation of mesoporous activated carbon from rice straw using phosphoric acid[J].Chemistry and Industry of Forest Products,2013,33(4):43-47.
[13] 邹长军,张丽颖,姚伟宁.超强碱催化剂碱强度(H_>37)的指示剂测定法[J].分析实验室,2005,24(2):73-75. ZOU Chang-jun,ZHANG Li-ying,YAO Wei-ning.Determination of the base strength of super base by indicator method[J].Chinese Journal of Analysis Laboratory,2005,24(2):73-75.
[14] 庄永斌,刘兆滨,黄伟卿.GB/T 5549—2010 表面活性剂用拉起液膜法测定表面张力[S].北京:中国标准出版社,2011-12-01. ZHUANG Yong-bin,LIU Zhao-bin,HUANG Wei-qing.GB/T 5549—2010 Surface active agents- Determination of surface tension by drawing up liquid films[S].Beijing:Standards Press of China,2011-12-01.
[15] 庄永斌,王伟松,孟照平.GB/T 6369—2008 表面活性剂乳化力的测定比色法[S].北京:中国标准出版社,2008-10-01. ZHUANG Yong-bin,WANG Wei-song,MENG Zhao-ping.GB/T 6369—2008 Surface active agents-Determination of emulsifying power:Colorimetric method[S].Beijing:Standards Press of China,2008-10-01.
[16] 庄永斌,唐福伟,黄伟卿.GB/T 7381—2010 表面活性剂在硬水中稳定性的测定方法[S].北京:中国标准出版社,2011-12-01. ZHUANG Yong-bin,TANG Fu-wei,HUANG Wei-qing.GB/T 7381—2010 Surface active agents-Determination of stability in hard water[S].Beijing:Standards Press of China,2011-12-01.
[17] 蔡孟深,李中军.糖化学-基础、反应、合成、分离及结构[M].北京:化学工业出版社,2006:68-69. CAI Meng-shen,LI Zhong-jun.Carbohydrate Chemistry:Fundamentals,Reactions,Synthesis,Isolation and Structures[M].Beijing:Chemical Industry Press,2006:68-69.

超声波辅助下K₂O/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 K₂O/C

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 15

编辑推荐

Metrics

本文评价

关于本刊

投稿指南

在线期刊

相关单位

联系我们

[1]	王凤, 龙柱, 陈杰, 王斌, 张凤山. 腰果酚聚氧乙烯醚复配脱墨剂的制备及应用[J]. 林产化学与工业, 2017, 37(6): 95-100.
[2]	刘磊磊, 赵帅, 王欢, 彭胜, 郭婕. 响应面法优化超声波辅助乙醇/盐双水相萃取栀子中京尼平苷[J]. 林产化学与工业, 2017, 37(2): 93-100.
[3]	闫鑫焱, 饶小平, 宋湛谦, 商士斌. 聚萜烯马来酸酐聚乙二醇酯高分子表面活性剂的制备及性能研究[J]. 林产化学与工业, 2017, 37(2): 129-134.
[4]	许小向, 尹小莉, 洪艳平, 邹凯, 上官新晨, 梁强. 火炬松松针多糖提取工艺及其抗氧化性研究[J]. 林产化学与工业, 2016, 36(3): 114-120.
[5]	宋冰蕾, 余小娜, 陈燕, 裴晓梅, 周萍萍, 翟兆兰. 含酰胺基团松香基双子表面活性剂的合成与性能[J]. 林产化学与工业, 2015, 35(6): 39-46.
[6]	郑建强, 刘莉, 饶小平, 宋湛谦, 商士斌. 松香基胆碱季铵盐表面活性剂的合成及抑菌活性研究[J]. 林产化学与工业, 2015, 35(5): 98-104.
[7]	夏田娟, 毕良武, 赵振东, 程贤, 邢雅丽. 迷迭香叶中鼠尾草酸的分离纯化[J]. 林产化学与工业, 2015, 35(5): 105-110.
[8]	贝俊杰, 曹云峰. 疏水改性羧甲基纤维素及其在废纸脱墨中的应用[J]. 林产化学与工业, 2015, 35(3): 80-84.
[9]	毛翠平, 武书彬. 有机改性硅藻土对聚乙酸乙烯酯乳液吸附性能及其动力学的研究[J]. 林产化学与工业, 2014, 34(6): 8-12.
[10]	王娟, 王丹, 商士斌, 沈明贵, 齐帆. 松香基季铵盐型杂双子表面活性剂的合成及性能研究[J]. 林产化学与工业, 2014, 34(6): 111-116.
[11]	王娟, 王丹, 商士斌, 沈明贵, 齐帆. 松香基聚氧乙烯胺型双子表面活性剂的合成及性能研究[J]. 林产化学与工业, 2014, 34(5): 109-114.
[12]	田金玲, 任世学, 方桂珍, 艾青. 二甲基-正丁基-磺化木质素基氯化铵的合成及性能研究[J]. 林产化学与工业, 2014, 34(4): 42-50.
[13]	林广沅, 吴国民, 孔振武. 表面活性剂对有机硅包覆松香基环氧树脂微胶囊的影响[J]. 林产化学与工业, 2014, 34(1): 25-30.
[14]	游凤, 黄立新, 张彩虹, 谢普军, 张耀雷. 超声波辅助减压提取枣皮多酚的研究[J]. 林产化学与工业, 2014, 34(1): 107-112.
[15]	彭密军;吕强;彭胜;张昌伟;张琳杰;瞿湘. 杜仲总木脂素的超声波辅助提取工艺研究[J]. 林产化学与工业, 2013, 33(4): 89-92.