CN105817208A - 一种罗丹明b接枝壳聚糖吸附剂及其制备和应用 - Google Patents
一种罗丹明b接枝壳聚糖吸附剂及其制备和应用 Download PDFInfo
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Abstract
本发明公开了一种罗丹明B接枝壳聚糖吸附剂及其制备和应用，属于吸附材料制备工艺领域。先将罗丹明B和水合肼反应制得罗丹明B酰肼；然后以乙二醛为交联剂，将罗丹明B酰肼接枝到壳聚糖上得到吸附剂；本发明提供的罗丹明B接枝壳聚糖吸附剂，其利用壳聚糖与罗丹明B的吸附性，键合牢固、性质稳定，选择性好，富集倍数较大。该吸附剂可用于环境水样中汞离子的吸附与检测。
Description
技术领域
本发明属于吸附材料制备工艺领域，具体涉及一种罗丹明B接枝壳聚糖吸附剂及其制备和应用。
背景技术
由于重金属离子种类、含量以及存在形态各异，且具有不易降解、毒害性大等特点，对水体污染严重，严重危及人类的生命安全。汞属于过渡金属元素，同时也是毒性非常强的重金属元素。由于汞不能被环境中的微生物分解，并且汞能自发的在生物体内富集，在一定条件下与生物体内部的有机物结合，转化为毒性更强的有机汞，因此，汞在环境中产生的污染非常严重。自从1956年日本爆发水俣病以来，人们对水体汞污染和汞中毒有了更加深刻的认识，美国更是将汞作为最优先重点处理的污染物之一。现阶段水体中汞污染的治理方法主要包括吸附法、离子交换法、膜分离法、混凝法、硫化汞沉淀法和还原法。在上述这些方法中，吸附法由于具有容易控制、能做进一步处理等优点，已经发展成为汞污染水体常见高效的处理办法。该方法的原理就是有针对性地制备一种吸附材料，使其选择性地吸收污染水体中的汞离子，使水体中的汞浓度降至排放标准以下或达到饮用水标准。而研制高性能、高吸附和高富集倍数的吸附材料是固相萃取技术的关键，受到研究者的高度重视。
壳聚糖(CS)作为一种汞离子天然吸附剂，是除了纤维素以外最丰富的自然资源，可由甲壳素脱乙酰基所得，具有较强的吸附分离能力。因其分子结构中含有氨基和羟基两种活泼基团，故壳聚糖可以通过交联、接枝、酰化、醚化等化学方法实现改性制备出具有不同理化特性和用途的壳聚糖衍生物。AkhmadSabarudin（MicrochemicalJournal，2011，99:34-39）等采用二-2-丙醇胺改性壳聚糖用于水中Ge的吸附。
罗丹明是一类重要的荧光材料，将其负载在壳聚糖上后，所合成吸附剂也具有了荧光性，增加了吸附剂的功能性。
发明内容
本发明的目的在于提供一种罗丹明B接枝壳聚糖吸附剂及其制备方法和应用。本发明将罗丹明B负载在大分子壳聚糖上，利用壳聚糖与罗丹明B的吸附性，键合牢固、性质稳定，所制得的吸附剂选择性好，富集倍数较大，能选择性吸附或检测环境水样中的汞离子。
为实现上述目的，本发明采用如下技术方案：
一种罗丹明B接枝壳聚糖吸附剂的制备方法，包括以下步骤：
（1）罗丹明B酰肼的合成：先将2.5mmol罗丹明B溶解在30mL乙醇中，然后在室温下逐滴加入3mL85%v/v水合肼，同时强力搅拌；加料完成后，加热回流2h，直到暗紫色变成橙色透明，然后冷却，减压除去溶剂；再加入50mL1MHCl溶解固体，再缓慢加入70mL1MNaOH，并搅拌，直到pH到达9~10为止；由此产生的沉淀用水洗涤3次，干燥，最后得到粉红固体即为罗丹明B酰肼；
（2）罗丹明酰肼接枝壳聚糖：取步骤（1）合成的罗丹明B酰肼1g溶解在50mL甲醇中，再依次加入过量乙二醛和2g壳聚糖，搅拌，并在N2环境中回流反应8h，冷却至室温后，将所得固体依次用甲醇、水清洗三次，过滤，干燥，制得吸附剂。
所述的罗丹明B接枝壳聚糖吸附剂的应用，用于环境水样中汞离子的吸附与检测。
本发明的显著优点在于：
（1）本发明的吸附剂是利用壳聚糖与罗丹明B之间的吸附性，将罗丹明B负载在大分子壳聚糖上，合成的一种固相萃取材料，具有很好的稳定性；结合了罗丹明B的识别性能和壳聚糖吸附功能，可以提高其吸附能力与选择性；
（2）本发明合成的罗丹明B接枝壳聚糖吸附剂，具有富集倍数大，重现性好的优点。
附图说明
图1a为CS的扫描电子显微镜图谱(10000倍)；
图1b为CS-RB的扫描电子显微镜图谱(10000倍)；
图2为CS-RB材料在10~150mg/L不同浓度的含Hg2+溶液中搅拌30min充分吸附后，Hg2+的浓度曲线变化图；
图3为CS-RB材料受不同水质影响的吸附效果图；
图4为CS-RB作为汞离子探针时的荧光光谱图；
图5为在513nm处的荧光强度和汞离子的浓度关系图；
图6为CS-RB吸附剂吸附浓度为10~70mg/L的汞离子后的颜色变化情况。
具体实施方式
为进一步公开而不是限制本发明，以下结合实例对本发明作进一步的详细说明。
实施例1
罗丹明B接枝壳聚糖吸附剂的制备
（1）合成罗丹明B酰肼：先用2.5mmol罗丹明B溶解在30mL乙醇中，3mL(过量)水合肼(85%，v/v)在室温下逐滴加入，同时强力搅拌；加热回流2h，直到暗紫色变成橙色透明，然后冷却，减压除去溶剂；再加入50mL1MHCl溶解固体，再缓慢加入70mL1MNaOH，并搅拌，直到pH到达9~10为止；由此产生的沉淀用水洗涤3次，干燥，最后得到粉红固体；
（2）罗丹明酰肼接枝壳聚糖：取步骤（1）合成的罗丹明B酰肼1g溶解在50mL甲醇中，再依次加入2mL乙二醛和2g壳聚糖，搅拌，并在N2环境中回流反应8h，冷却至室温后，将所得固体用甲醇，水清洗三次，过滤，干燥，制得吸附剂。
1、罗丹明B接枝壳聚糖吸附剂粒径及形貌的表征
从图1a中可以看出，CS的表面光滑且有些为片状结构；而在交联上罗丹明B后，表面变得粗糙，说明接枝的罗丹明B改变了壳聚糖表面形貌；通过氮吸附实验测得吸附剂CS和CS-RB的比表面积分别为16.34m2/g；23.28m2/g，说明在接枝罗丹明后，其比表面积增大。
2、吸附容量测定
采用吸附试验法，通过FAAS测定吸附剂在10~150mg/L不同浓度的溶液中搅拌30min充分吸附后Hg2+的浓度。结果如图2所示。结果表明，当Hg2+溶液在较低浓度时，其吸附容量随着Hg2+浓度的增加而增加，当Hg2+溶液初始浓度较高时，则出现平台，说明吸附剂对Hg2+的吸附达到了饱和状态。实验结果显示该吸附剂对Hg2+的饱和吸附容量为71mg/g。
3、水质对CS-RB吸附性能的影响
吸附剂的吸附性能还可能跟水质有关，为了考察吸附剂在不同水质中的适应性，我们对其进行了实验探究。以纯水、自来水、湖水三种水质各配制50ppm汞溶液，取三种水质配制的汞溶液各10mL，平行取两份；平行两份中分别加入15mg的CS和15mg的CS-RB，混匀后，对滤液中残余的Hg2+量进行检测。实验发现不同水样对CS-RB的吸附能力几乎没有明显影响，其吸附效果均能达到90%以上，因此CS-RB材料可用于不同水质中重金属离子进行吸附、净化。同时研究发现，CS-RB的吸附率可达90%，而单纯的CS只能吸附45%。实验结果说明，壳聚糖对Hg2+虽然也具有较强的吸附能力，但当其修饰上Hg2+荧光探针材料后，该吸附材料对Hg2+的吸附效率将大大提高了。结果如图3所示。
4、CS-RB作为汞离子探针的应用
罗丹明是一类重要的荧光材料，将其负载在壳聚糖上后，所合成吸附剂也具有了荧光性。如图4所示，为CS-RB作为汞离子探针时荧光光谱图。当加入汞离子后，CS-RB吸附材料的荧光强度增强，随着汞离子浓度的增加，其荧光强度也随之增强。在513nm处的荧光强度和加入的汞离子的浓度有很好的线性关系，如图5所示，其线性关系为A=28.4075c+0.56312，R=0.9991。图6为CS-RB吸附剂吸附浓度为10~70mg/L的汞离子后的颜色变化情况，从图6中可以看出，随着浓度的增加，吸附剂的颜色逐渐加深（淡黄色变成深红色），说明汞离子不仅可以从荧光光谱中进行检测，还可以用视觉简单地进行分辨。
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (4)
1.一种罗丹明B接枝壳聚糖吸附剂，其特征在于：先将罗丹明B和水合肼反应制得罗丹明B酰肼；然后以乙二醛为交联剂，将罗丹明B酰肼接枝到壳聚糖上得到吸附剂。
2.根据权利要求1所述的罗丹明B接枝壳聚糖吸附剂，其特征在于：罗丹明B酰肼是按以下方法合成的：先将2.5mmol罗丹明B溶解在30mL乙醇中，然后在室温下逐滴加入3mL85%v/v水合肼，同时强力搅拌；加料完成后，加热回流2h，冷却，减压除去溶剂；再加入50mL1MHCl溶解固体，再缓慢加入70mL1MNaOH，并搅拌，直到pH到达9~10，由此产生的沉淀用水洗涤3次，干燥，最后得到罗丹明B酰肼。
3.一种制备如权利要求1所述的罗丹明B接枝壳聚糖吸附剂的方法，其特征在于：将1g罗丹明B酰肼溶解在50mL甲醇中，再依次加入过量乙二醛和2g壳聚糖，搅拌，并在N2环境中回流反应8h；冷却至室温后，将所得固体依次用甲醇、水清洗三次，过滤，干燥，制得吸附剂。
4.一种如权利要求1所述的罗丹明B接枝壳聚糖吸附剂的应用，其特征在于：用于环境水样中汞离子的吸附与检测。
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| CN113070050A (zh) * | 2021-04-28 | 2021-07-06 | 山东大学 | 一种能可视化识别并除去汞离子的壳聚糖基水凝胶吸附剂及其制备方法与应用 |
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| CN113070050B (zh) * | 2021-04-28 | 2022-06-21 | 山东大学 | 一种能可视化识别并除去汞离子的壳聚糖基水凝胶吸附剂及其制备方法与应用 |
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