CN105618005A - 一种磁性壳聚糖的制备方法和应用 - Google Patents
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Abstract
本发明提供了一种磁性壳聚糖的制备方法，步骤为：1)在25mL乙二醇中加入0.45-1.8g的FeCl3·6H2O固体，将烧杯放入超声仪中并用玻璃棒缓慢搅拌，随后加入0.54-2.15g的壳聚糖粉末并不断搅拌，至形成淡黄色粘稠液体；2)向上述粘稠液体中加入2mL(1.8646mol/L)己二胺溶液并不断搅拌；3)将步骤2)处理的液体转移至反应釜中，160℃-220℃反应6h-10h；4)反应完成后，得到黑色混合液，分别用二次水、无水乙醇清洗2-3次，进行磁滞分离，干燥，得到黑色产物MFe3O4/CS？NPs。该方法操作简单、一步合成；所制备的磁性壳聚糖用于吸附处理染料废水，具有易分离、可重复利用、无二次污染、成本低等优点。
Description
技术领域
本发明涉及污水处理材料，具体属于一种磁性壳聚糖吸附剂的制备方法，以及磁性壳聚糖在染料废水处理中的应用。
背景技术
现代工业的迅速发展产生了大量含染料的废水,因其污染物不可降解且易通过食物链在生物体内富集,对环境和人类生活构成了很大的威胁。在当前染料废水的处理方法中,生物吸附法因操作简单、处理效率高而广泛应用。其中壳聚糖由于具有资源丰富、环境友好、吸附能力高、扩散性能好、选择性吸附、易恢复活性等优点,受到广泛关注。
壳聚糖(Chitosan)是自然界中储量第二大的生物质资源甲克素的脱乙酰产物。它作为一种线型天然高分子,具有良好的生物相容性和可降解性，其大分子链上含有大量的羟基、氨基,对染料有一定的吸附作用,可作为一种吸附剂处理废水中的染料。对壳聚糖进行化学改性,可以生成相应的衍生物,用于染料废水的处理方面具有良好的应用前景。
最近，磁性分离技术受到科研工作者的广泛关注，其中磁性材料Fe3O4最为常见。人们对于Fe3O4的研究经历了从微米到纳米的变化过程。发现当Fe3O4微球处于纳米等级时，其结构上不同于固态物质并且与单个原子也存在很大的差别，正是这种独特的结构使Fe3O4微球具有新颖、高效、独特的物理和化学性质如超顺磁性等。正是因为这种独特的性质使得Fe3O4微球在染料、磁记录、生物医学、磁传感器、催化剂等众多的领域中都有潜在的应用价值，使得其成为科学研究者研究的重点和热点。
目前，磁性壳聚糖吸附法处理染料废水已得到应用。但是，现有磁性壳聚糖的合成方法复杂、成本高、吸附效率低、重复利用率低，因此，研究一种易合成、成本低、吸附效率高、可重复利用的磁性壳聚糖显得尤为重要。
发明内容
本发明所要解决的技术问题是提供一种磁性壳聚糖的制备方法，该方法操作简单、一步合成；所制备的磁性壳聚糖处理污水时易分离、可重复利用、无二次污染、成本低。
本发明提供的一种磁性壳聚糖的制备方法，步骤为：
1)在25mL乙二醇中加入0.45-1.8g的FeCl3·6H2O固体，将烧杯放入超声仪中并用玻璃棒缓慢搅拌，随后加入0.54-2.15g的壳聚糖粉末并不断搅拌，至形成淡黄色粘稠液体；
2)向上述粘稠液体中加入2mL(1.8646mol/L)己二胺溶液并不断搅拌；
3)将步骤2)处理的液体转移至反应釜中，160℃-220℃反应6h-10h；
4)反应完成后，得到黑色混合液，分别用二次水、无水乙醇清洗2-3次，进行磁滞分离，得到黑色产物；
5)将黑色产物放入真空干燥箱中干燥24h，得到的黑色粉末为最终产物MFe3O4/CSNPs。
优选步骤1)中FeCl3·6H2O固体的加入量为1.5g。壳聚糖粉末加入量为1.79g。
优选步骤3)中反应温度为220℃，反应时间8h。
上述所制备的磁性壳聚糖可在染料废水处理中应用。特别是在处理氨基黑10B染料废水中应用。
与现有技术相比，本发明的优点：磁性壳聚糖合成方法为一步水热法，制备方法简单，反应条件温和；合成所需药品数比其他文献报道中有所减少，节约药品，降低成本。所得产物具有良好的分散性与稳定性，而且在外置磁场的存在下即可分离收集，易回收，脱附后可重复利用，节约经济成本，易实现规模化应用。
附图说明
图1为实施例3制备的MFe3O4/CSNPs的透射电镜图。
图2为实施例3制备的MFe3O4/CSNPs的扫描电镜图。
图3为实施例3制备的MFe3O4/CSNPs的傅里叶红外光谱图。
图4为实施例3制备的MFe3O4/CSNPs的磁化率曲线。
图5为实施例3制备的MFe3O4/CSNPs吸附氨基黑10B的等温吸附曲线。
图6为实施例3制备的MFe3O4/CSNPs吸附氨基黑10B的吸附动力学曲线。
图7为实施例3制备的MFe3O4/CSNPs吸附氨基黑10B时pH对吸附量的影响图。
具体实施方式
以下是结合附图和实施例对本发明做进一步详细说明。
实施例1
1.磁性壳聚糖的制备
1)在25mL乙二醇中加入1.5g的FeCl3·6H2O固体，将烧杯放入超声仪中并用玻璃棒缓慢搅拌，随后加入1.79g的壳聚糖粉末并不断搅拌；
2)用移液枪向上述溶液中移入2mL(1.8646mol/L)己二胺溶液并不断搅拌；
3)将上述溶液转移至50ml反应釜内衬中，组装好反应釜后，将其放入160℃的鼓风干燥箱中反应6h；
4)反应完成后，取出反应釜，得到黑色混合液，分别用二次水、无水乙醇清洗2-3次，进行磁滞分离，得到黑色产物；
5)将此产物放入真空干燥箱中干燥24h，得到的黑色粉末为最终产物MFe3O4/CSNPs。
2.氨基黑10B的吸附实验
1)取0.001g的MFe3O4/CSNPs加入一定体积2mg/mL氨基黑10B溶液中；
2)将混合上述混合液体放置摇床摇1h；
3)在氨基黑10B最大吸收波长618nm处分别测MFe3O4/CSNPs吸附氨基黑10B前后溶液的吸光度，从而计算MFe3O4/CSNPs对氨基黑10B的最大吸附量，为13.81mg/g。
实施例2
1.磁性壳聚糖的制备
1)在25mL乙二醇中加入1.5g的FeCl3·6H2O固体，将烧杯放入超声仪中并用玻璃棒缓慢搅拌，随后加入1.79g的壳聚糖粉末并不断搅拌；
2)用移液枪向上述溶液中移入2mL(1.8646mol/L)己二胺溶液并不断搅拌；
3)将上述溶液转移至50ml反应釜内衬中，组装好反应釜后，将其放入180℃的鼓风干燥箱中反应8h；
4)反应完成后，取出反应釜，得到黑色混合液，分别用二次水、无水乙醇清洗2-3次，进行磁滞分离，得到黑色产物；
5)将此产物放入真空干燥箱中干燥24h，得到的黑色粉末为最终产物MFe3O4/CSNPs。
2.氨基黑10B的吸附实验
1)取0.001g的MFe3O4/CSNPs加入一定体积2mg/mL氨基黑10B溶液中；
2)将混合上述混合液体放置摇床摇1h；
3)在氨基黑10B最大吸收波长618nm处分别测MFe3O4/CSNPs吸附氨基黑10B前后溶液的吸光度，从而计算MFe3O4/CSNPs对氨基黑10B的最大吸附量，为30.13mg/g。
实施例3
1.磁性壳聚糖的制备
1)在25mL乙二醇中加入1.5g的FeCl3·6H2O固体，将烧杯放入超声仪中并用玻璃棒缓慢搅拌，随后加入1.79g的壳聚糖粉末并不断搅拌；
2)用移液枪向上述溶液中移入2mL(1.8646mol/L)己二胺溶液并不断搅拌；
3)将上述溶液转移至50ml反应釜内衬中，组装好反应釜后，将其放入220℃的鼓风干燥箱中反应8h；
4)反应完成后，取出反应釜，得到黑色混合液，分别用二次水、无水乙醇清洗2-3次，进行磁滞分离，得到黑色产物；
5)将此产物放入真空干燥箱中干燥24h，得到的黑色粉末为最终产物MFe3O4/CSNPs。
2.氨基黑10B的吸附实验
1)取0.001g的MFe3O4/CSNPs加入一定体积2mg/mL氨基黑10B溶液中；
2)将混合上述混合液体放置摇床摇1h；
3)在氨基黑10B最大吸收波长618nm处分别测MFe3O4/CSNPs吸附氨基黑10B前后溶液的吸光度，从而计算MFe3O4/CSNPs对氨基黑10B的最大吸附量，为99.94mg/g。
实施例4
1.磁性壳聚糖的制备方法同实施例3
2.亚甲基蓝的吸附实验
1)取0.001g的MFe3O4/CSNPs加入一定体积2mg/mL亚甲基蓝溶液中；
2)将混合上述混合液体放置摇床摇1h；
3)在亚甲基蓝最大吸收波长665nm处分别测MFe3O4/CSNPs吸附亚甲基蓝前后溶液的吸光度，从而计算MFe3O4/CSNPs对亚甲基蓝的最大吸附量,为54.42mg/g。
实施例5
1.磁性壳聚糖的制备方法同实施例3
2.酸性大红G的吸附实验
1)取0.001g的MFe3O4/CSNPs加入一定体积2mg/mL酸性大红G溶液中；
2)将混合上述混合液体放置摇床摇1h；
3)在酸性大红G最大吸收波长504nm处分别测MFe3O4/CSNPs吸附酸性大红G前后溶液的吸光度，从而计算MFe3O4/CSNPs对酸性大红G的最大吸附量，为46.21mg/g。
Claims (7)
1.一种磁性壳聚糖的制备方法，其特征在于，步骤为：
1)在25mL乙二醇中加入0.45-1.8g的FeCl3·6H2O固体，将烧杯放入超声仪中并用玻璃棒缓慢搅拌，随后加入0.54-2.15g的壳聚糖粉末并不断搅拌，至形成淡黄色粘稠液体；
2)向上述粘稠液体中加入2mL浓度为1.8646mol/L的己二胺溶液并不断搅拌；
3)将步骤2)处理的液体转移至反应釜中，160℃-220℃反应6h-10h；
4)反应完成后，得到黑色混合液，分别用二次水、无水乙醇清洗2-3次，进行磁滞分离，得到黑色产物；
5)将黑色产物放入真空干燥箱中干燥24h，得到的黑色粉末为最终产物MFe3O4/CSNPs。
2.如权利要求1所述的磁性壳聚糖的制备方法，其特征在于，所述步骤1)中FeCl3·6H2O固体的加入量为1.5g。
3.如权利要求1所述的磁性壳聚糖的制备方法，其特征在于，所述步骤1)中壳聚糖粉末加入量为1.79g。
4.如权利要求1所述的磁性壳聚糖的制备方法，其特征在于，所述步骤3)中反应温度为220℃。
5.如权利要求1所述的磁性壳聚糖的制备方法，其特征在于，所述步骤3)中反应时间为8h。
6.如权利要求1所述方法制备的磁性壳聚糖在染料废水处理中的应用。
7.如权利要求1所述方法制备的磁性壳聚糖在处理氨基黑10B废水中的应用。
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