羧甲基壳聚糖和季铵盐壳聚糖的制备工艺

doi:10.3969/j.issn.1000-2006.201606008

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南京林业大学学报（自然科学版） ›› 2017, Vol. 41 ›› Issue (03): 151-156.doi: 10.3969/j.issn.1000-2006.201606008

羧甲基壳聚糖和季铵盐壳聚糖的制备工艺

刘雪娇, 景宜^*

南京林业大学轻工科学与工程学院,江苏南京 210037

出版日期:2017-06-18 发布日期:2017-06-18
基金资助:
收稿日期:2016-06-05 修回日期:2016-09-29
基金项目:国家自然科学基金项目(31370583)
第一作者:刘雪娇(1553439321@qq.com)。*通信作者:景宜(jingyi@njfu.com.cn),教授,博士。
引文格式:刘雪娇, 景宜. 羧甲基壳聚糖和季铵盐壳聚糖的制备工艺[J]. 南京林业大学学报(自然科学版),2017,41(3):151-156.

Preparation technology of carboxymethyl chitosan and quaternary chitosan

LIU Xuejiao, JING Yi^*

College of Light Industrial Science and Engineering, Nanjing Forestry University, Nanjing 210037, China

Online:2017-06-18 Published:2017-06-18

摘要/Abstract

摘要： 【目的】对羧甲基壳聚糖和季铵盐壳聚糖的制备工艺进行优化,改善壳聚糖在水中的溶解性。【方法】分别以氯乙酸(ClCH₂COOH)和3-氯-2-羟丙基三甲基氯化铵(CTA)为改性剂,对壳聚糖进行羧甲基化和季铵化改性,并以改性壳聚糖对蒙脱土的插层效果为基准进行有关CM-CTS合成条件研究。【结果】通过X-射线衍射(XRD)、透射电镜(TEM)、红外吸收光谱(FT-IR)和核磁共振氢谱(¹H-NMR)的分析,得出了壳聚糖的优化改性条件。制备羧甲基壳聚糖的优化条件为:反应时间6.0 h,反应温度60 ℃,m(氯乙酸)/m(壳聚糖)为3,m(NaOH)/m(壳聚糖)为4.5; 制备季铵盐壳聚糖的优化条件为:反应时间10 h,反应温度75 ℃,m(CTA)/m(壳聚糖)为4.5,m(NaOH)/m(壳聚糖)为0.8。【结论】对壳聚糖进行羧甲基化和季铵化改性,向壳聚糖中引入新的官能团,不仅可以改善壳聚糖的水溶性,同时壳聚糖/蒙脱土纳米复合材料的制备也极大地扩展了壳聚糖的应用范围。

Abstract: 【Objective】Carboxymethylation or quaternization of chitosan(CTS)improved its solubility in water. 【Method】We investigated the effect of modifying chitosan by carboxymethylation or quaternization using chloroacetic acid(ClCH₂COOH)or 3-chloro-2-hydroxypropyltrimethylammonium chloride(CTA)as grafting agents. CTS intercalation by montmorillonite was used to evaluate the effect of the above modification. 【Result】Optimal modification conditions determined by X-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy and ¹H-nuclear magnetic resonance analyses were as follows: reaction time = 6.0 h, reaction temperature = 60 ℃, m(ClCH₂COOH):m(CTS)= 3.0:1.0, m(NaOH):m(CTS)= 4.5:1.0. The following optimum conditions for CTA-CTS synthesis were determined: reaction time = 10 h, reaction temperature = 75 ℃, m(CTA):m(CTS)= 4.5:1.0, m(NaOH):m(CTS)= 0.8:1.0. 【Conclusion】Introduction of new functional groups by carboxymethylation or quaternization of chitosan can not only improve its solubility in water, but also afford chitosan/montmorillonite nanocomposites, greatly expanding the application scope of chitosan.

中图分类号:

TB332

刘雪娇,景宜. 羧甲基壳聚糖和季铵盐壳聚糖的制备工艺[J]. 南京林业大学学报（自然科学版）, 2017, 41(03): 151-156.

LIU Xuejiao, JING Yi. Preparation technology of carboxymethyl chitosan and quaternary chitosan[J].Journal of Nanjing Forestry University (Natural Science Edition), 2017, 41(03): 151-156.DOI: 10.3969/j.issn.1000-2006.201606008.

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羧甲基壳聚糖和季铵盐壳聚糖的制备工艺

Preparation technology of carboxymethyl chitosan and quaternary chitosan

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