交叉Claisen酯缩合反应制备淀粉/纤维素基微孔滤膜
作者:张瑞峰 ,2  黄少斌12  吴文清12  祝光富3
单位: 1.华南理工大学环境科学与工程学院,广州 510006;2.工业聚集区污染控制与生态修复教育部重点实验室,广州 510006;3.广东上九生物降解塑料有限公司,东莞 523128
关键词: 醋酸酯淀粉;柠檬酸三丁酯;乙醇钠;交叉Claisen酯缩合;微孔滤膜
出版年,卷(期):页码: 2013,33(2):29-36

摘要:
将自制醋酸酯淀粉(SA)混合醋酸纤维素(CA)后溶于丙酮溶剂中,在交联剂柠檬酸三丁酯(TBC)和催化剂乙醇钠(SE)的作用下进行交叉Claisen酯缩合反应,然后使用相分离法制备出了淀粉/纤维素基微孔滤膜。制备的微孔滤膜使用傅里叶变换红外光谱(FT-IR)、X-衍射(XRD)、热重(TGA)、扫描电镜(SEM)、杯式超滤器等进行测试和表征。结果表明,在该体系下自制SA可以更好地溶解并发生交联反应,SA和CA与TBC之间有效发生了交叉Claisen酯缩合反应,该反应还可以极大地降低SA的结晶度,制备的微孔滤膜在200℃以下具有良好的热稳定性能和力学性能,滤膜具有丰富的海绵状微孔结构,平均孔隙率在70%~80%之间,对实验室配制的恶臭假单胞菌液的截留率最高达到95%。
 Use starch acetate which prepared in the laboratory and cellulose acetate as raw materials, then make them blended and dissolved in acetone, under the effect of tributyl citrate and sodium ethoxide to conduct the crossed-Claisen condensation reaction, and finally prepared some microfiltration membranes by phase separation method. Those prepared microfiltration membranes were characterized and tested by FT-IR, XRD, TGA, SEM and cup-type ultrafilter. The results shows that starch acetate have better performance of dissolve and reaction in this cross-linking system, tributyl citrate conduct efficacious ester condensation reaction with starch acetate and Cellulose Acetate in this cross-linking system, and this type of reaction can also greatly reduce the degree of crystallinity of Starch Acetate. Those prepared microfiltration membranes have good performance of mechanical and steady thermal performance below the temperature of 200℃, and have abundant sponge-like porous structure, their average porosity between 70% to 80%, the retention rate of microfiltration membranes about pseudomonas putida which prepared in the laboratory can reach 95%.
张瑞峰(1985-),男,江苏仪征人,硕士研究生,主要从事纤维素醚改性和高分子微孔滤膜制备与改性研究,< 371217623@qq.com>。*通讯联系人,< chshuang@scut.edu.cn >

参考文献:
[1] 李文俊, 卢玉华, 孙志军, 等. 基于相分离制备高分子微孔材料的新探索[J]. 膜科学与技术, 2011, 31(3): 53-58.
[2] Takaaki T, Masatou U, Youhei W, Tomoaki K, et al. Poly(L-lactic acid) Microfiltration Membrane Formation via Thermally Induced Phase Separation with Drying[J]. J Chem Eng Jpn, 2011, 44(7): 467-475.
[3] Sikder J, Pereira C, Palchoudhury S, et al. Synthesis and characterization of cellulose acetate-polysulfone blend microfiltrationmembrane for separation of microbial cells from lactic acid fermentation broth[J]. Desalination, 2009, 249(2): 802-808.
[4] Douglas R L, Sung S K, Kevin E K. Microporous membrane formation via thermally-induced phase separation. II. Liquid—liquid phase separation[J]. J Membr Sci, 1991, 64(1-2): 1-11.
[5] Abdul R R, Wan A W A R, Lee T S, et al. Approaches to improve compatibility of starch filled polymer system: A review[J]. Mater Sci Eng C, 2009, 29(8): 2370-2377.
[6] Ruhul H M, Basel F A S, Mamdouh A H. Effect Of Starch Addition On The Properties Of Low Density Polyethylene For Developing Environmentally Degradable Plastic Bags[J]. J Chem Eng, 2011, 26(1): 38-40.
[7] 谢  钦, 吴  磊, 高群玉. 食用醋酸酯甘薯淀粉性质的研究[J]. 粮食与饲料工业, 2010, 6: 24-35.
[8] 戴小敏. 醋酸醋型改性淀粉的表征及其膜性能研究[D]:[硕士学位论文], 大连: 中国科学院大连化学物理研究所, 2003: 7-9.
[9] Xu Y X, Hanna M A. Preparation and properties of biodegradable foams from starch acetate and poly(tetramethylene adipate-co-terephthalate) [J]. Carbohydr Polym, 2005, 59(4): 521-529.
[10] Johnson D J, Malek S A A, Al-Rashdi B A M, et al. Atomic force microscopy of nano?ltration membranes: Effect of imaging mode and environment[J]. J Membr Sci, 2012,389: 486-498.
[11] Mei J, Ou Y F, Chen J N. Studies on Polymerization and the Properties of Cellulose Acetate at High Temperature[J]. J Cellul Sci Technol, 2000, 8(1): 9-16.
[12] Kenta T, Yuuya N, Tomohito O, et al. Practical and Robust Method for Stereoselective Preparations of Ketene Silyl (Thio)acetal Derivatives and NaOH-Catalyzed Cross-Claisen Condensation Between Ketene Silyl Acetals and Methyl Esters[J]. Tetrahedron. 2009, 65(28): 5596-5607.
[13] Yoshihiro N, Aya O, Makoto Y, et al. Indium Tribromide Catalyzed Cross-Claisen Condensation between Carboxylic Acids and Ketene Silyl Acetals Using Alkoxyhydrosilanes[J]. Angew Chem, 2011, 123(37): 8782-8784.
 

服务与反馈:
文章下载】【加入收藏

《膜科学与技术》编辑部 地址:北京市朝阳区北三环东路19号蓝星大厦 邮政编码:100029 电话:010-64426130/64433466 传真:010-80485372邮箱:mkxyjs@163.com

京公网安备11011302000819号