CN107519845B - 一种离子液体改性交联多孔壳聚糖吸附剂及其制备和应用 - Google Patents
一种离子液体改性交联多孔壳聚糖吸附剂及其制备和应用 Download PDFInfo
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Abstract
本发明公开了一种离子液体改性交联多孔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。其制备方法包括:(1)交联多孔壳聚糖的合成;(2)离子液体改性交联多孔壳聚糖的合成。本发明提供的离子液体改性交联改性多孔壳聚糖吸附剂,以戊二醛为交联剂,以壳聚糖为载体,制备出交联多孔壳聚糖,再将1‑烯丙基‑3‑甲基咪唑氯盐接枝到交联多孔壳聚糖球上,制得离子液体改性交联多孔壳聚糖吸附材料。本发明通过在交联多孔壳聚糖上引入大量离子液体,增加其对有机污染物的亲和性,提高吸附剂的吸附性能,键合牢固、性质稳定,可以在较宽的pH范围内使用。该吸附剂可用于环境水样中染料的吸附。
Description
技术领域
本发明属于吸附材料制备工艺领域,具体涉及一种离子液体改性交联多孔壳聚糖吸附剂及其制备和应用。
背景技术
合成染料在纺织,制革,造纸,油漆,化妆品和食品等许多行业都有广泛的应用。其中偶氮染料使用量占所有商业染料的70%以上。这些染料若未经净化处理排入环境中,不仅污染水体颜色,且会对生物体带来毒性,致突变性,甚至致癌性。因此,当前亟需发展一种高效去除水环境中的染料污染物的方法。吸附法作为一种污水处理方法,由于其具有成本低,效率高,操作简单,耗时短,并且还能够和其他的污水治理技术相互补充应用等优点,已经得到了大规模的运用。虽然一些吸附材料如活性炭、粘土和沸石等已被用于处理染料废水。但是制备高吸附性能且成本低廉的吸附材料,对研究吸附法处理染料仍具有重要意义。
壳聚糖在自然界中含量丰富,原料易得,与生物之间具有良好的相容性,并且能够降解,是一类极具发展前景的天然高分子材料。壳聚糖分子中包含有大量的-NH2和-OH,被广泛运用于水污染的治理中,如染料废水的脱色、污水中重金属离子的回收等,但壳聚糖吸附材料多是无孔粉末状,其比表面积和孔隙度低。
离子液体(ILs)是由阴阳离子组成的新型有机化合物,其具有不挥发、不可燃、热稳定性好、电导性好以及电化学窗口宽等优点,被广泛应用于萃取分离和电化学领域。离子液体与合适的聚合物基质的相互作用为吸附染料提供了可能性。在这方面,已经报道了离子液体对交联聚合物的改性作为吸附阴离子染料的新型吸附剂。为了提高吸附能力,我们认为探索其他更简单的材料如交联多孔壳聚糖基质以吸附和回收阴离子染料将是有趣的。目前,尚无将离子液体接枝于交联多孔壳聚糖上应用于水样中日落黄(SY)染料的相关报道。
发明内容
本发明的目的在于提供一种离子液体改性的交联多孔壳聚糖吸附剂及其制备和应用。本发明所提供的离子液体改性的交联多孔壳聚糖吸附剂材料,通过在交联多孔壳聚糖上引入大量离子液体,增加其对有机污染物的亲和性,提高吸附剂的吸附性能,键合牢固、性质稳定,可以在较宽的pH范围内使用,其对于环境中染料吸附富集能力良好。
为实现上述目的,本发明采用如下技术方案:
一种离子液体改性的交联多孔壳聚糖吸附剂的制备方法,包括以下步骤:
(1)合成交联多孔壳聚糖:用143 mL 体积分数1%的乙酸溶液搅拌溶解5 g壳聚糖(CS),待壳聚糖完全溶解且静止至气泡完全逸出,得到均匀的壳聚糖溶液;用0.5 mL的胶头滴管将配制好的壳聚糖溶液缓慢逐滴滴加到质量分数10%的氢氧化钠溶液中,滴加完后低转速磁力搅拌3 h,用去离子水洗至中性,置于去离子水中保存,即得到多孔壳聚糖球(CB);交联多孔壳聚糖(CCB)的制备则是将100 mL的壳聚糖球(CB)加入100 mL去离子水和2 mL体积分数50%的戊二醛溶液(GLA),25 ℃磁力搅拌45 min;之后分别用乙醇和去离子水依次洗涤数次,将交联多孔壳聚糖(CCB)置于去离子水中保存;
(2)合成离子液体改性交联多孔壳聚糖:取50 mL交联多孔壳聚糖(CCB)加到35 mL含有0.25 g过硫酸铵(APS) 的去离子水中,通入氮气,缓慢搅拌30 min;随后将体系温度升至60 ℃;将1.5 g离子液体[AMIM]Cl溶于15 mL去离子水中,并于15 min内逐滴加入反应液中,氮气保护反应12 h;待反应结束后,用去离子水将产物洗涤至中性,冷冻干燥,将产物(P[AMIM]Cl-g-CCB)捣碎备用。而P[AMIM]Cl-g-CCS则是采用原料壳聚糖(CS)代替CB在同等条件下制备得到。
本发明的显著优点在于:
(1)本发明合成的离子液体改性交联多孔壳聚糖吸附剂,是以交联多孔壳聚糖为基体,并接入1-烯丙基-3-甲基咪唑氯盐,具有很好的稳定性;结合了离子液体和交联多孔壳聚糖吸附功能,可以提高其吸附能力;
(2)本发明合成的离子液体改性交联多孔壳聚糖吸附剂,具有可以在较宽的pH范围内使用,吸附容量大的优点。
附图说明
图1为P[AMIM]Cl-g-CCB吸附剂的制备流程图;
图2为P[AMIM]Cl-g-CCB和CCB吸附剂吸附日落黄的吸附容量随溶液初始pH值的变化图;
图3为吸附时间对吸附效果的影响效果图;
图4为日落黄溶液的初始浓度对吸附效果的影响效果图;
图5 为日落黄溶液的初始浓度对吸附效果的影响效果图。
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
离子液体改性交联多孔壳聚糖吸附剂的制备
(1)合成交联多孔壳聚糖:用143 mL 体积分数1%的乙酸溶液搅拌溶解5 g壳聚糖(CS),待壳聚糖完全溶解且静止至气泡完全逸出,得到均匀的壳聚糖溶液;用0.5 mL的胶头滴管将配制好的壳聚糖溶液缓慢逐滴滴加到质量分数10%的氢氧化钠溶液中,滴加完后低转速磁力搅拌3 h,用去离子水洗至中性,置于去离子水中保存,即得到多孔壳聚糖球(CB);交联多孔壳聚糖(CCB)的制备则是将100 mL的壳聚糖球(CB)加入100 mL去离子水和2 mL体积分数50%的戊二醛溶液(GLA),25 ℃磁力搅拌45 min;之后分别用乙醇和去离子水依次洗涤数次,将交联多孔壳聚糖(CCB)置于去离子水中保存;
(2)合成离子液体改性交联多孔壳聚糖:取50 mL交联多孔壳聚糖(CCB)加到35 mL含有0.25 g过硫酸铵(APS) 的去离子水中,通入氮气,缓慢搅拌30 min;随后将体系温度升至60 ℃;将1.5 g离子液体[AMIM]Cl溶于15 mL去离子水中,并于15 min内逐滴加入反应液中,氮气保护反应12 h;待反应结束后,用去离子水将产物洗涤至中性,冷冻干燥,将产物(P[AMIM]Cl-g-CCB)捣碎备用;而P[AMIM]Cl-g-CCS则是采用原料壳聚糖(CS)代替CB在同等条件下制备得到。图1为P[AMIM]Cl-g-CCB的制备流程图。
实施例2
pH对离子液体改性交联多孔壳聚糖吸附剂吸附性能的影响
通过对不同pH值溶液的静态试验,采用紫外分光光度法测得其吸附容量。图2为离子液体改性交联多孔壳聚糖吸附日落黄的吸附容量随溶液初始pH值的变化情况。其初始日落黄的浓度:50 ppm;吸附剂用量:5 mg;吸附时间:3 h;温度:25℃;试样体积:10 mL。
实施例3
吸附时间的优化
搅拌时间对提高吸附效率具有重要意义。本实验分别考察了吸附剂在10-120 min的情况下对日落黄吸附性能的影响,结果如图3所示,吸附容量均随着吸附时间的增加而升高。初始阶段吸附剂对日落黄的吸附很快,随着吸附时间的增加,日落黄的吸附容量快速增长,然后吸附速度逐渐变缓,最后出现一个平台,此时吸附达到平衡状态。为使其吸附效果较好,并且节省吸附时间,故而本实验对于日落黄的后续实验吸附时间采用60 min。
实施例4
饱和吸附容量
日落黄溶液初始浓度对吸附效果的影响,结果见图4所示。由图可知,当日落黄溶液在较低浓度时,其吸附容量随之增加而增加,当初始浓度较高时,则出现平台,说明吸附剂对它们的吸附达到了饱和状态。 实验结果显示吸附剂P[AMIM]Cl-g-CCB、P[AMIM]Cl-g-CCS和CCB对日落黄(SY)的饱和吸附容量分别为300.28 mg/g、226.78 mg/g和36.08 mg/g。
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 (2)
1.一种离子液体改性交联多孔壳聚糖吸附剂的制备方法,其特征在于:以戊二醛为交联剂,以壳聚糖为载体,制备出交联多孔壳聚糖,再将1-烯丙基-3-甲基咪唑氯盐接枝到交联多孔壳聚糖球上,制得离子液体改性交联多孔壳聚糖吸附剂;所述的交联多孔壳聚糖的制备方法为:用143 mL 体积分数1%的乙酸溶液搅拌溶解5 g壳聚糖CS,待壳聚糖完全溶解且静止至气泡完全逸出,得到均匀的壳聚糖溶液;用0.5 mL的胶头滴管将配制好的壳聚糖溶液缓慢逐滴滴加到质量分数10%的氢氧化钠溶液中,滴加完后低转速磁力搅拌3 h,用去离子水洗至中性,置于去离子水中保存,即得到多孔壳聚糖球CB;交联多孔壳聚糖CCB的制备则是将100 mL的壳聚糖球CB加入100 mL去离子水和2 mL 体积分数50%的戊二醛溶液GLA,25 ℃磁力搅拌45 min;之后分别用乙醇和去离子水依次洗涤数次,将交联多孔壳聚糖CCB置于去离子水中保存。
2.根据权利要求1所述的离子液体改性交联多孔壳聚糖吸附剂的制备方法,其特征在于:所述离子液体改性交联多孔壳聚糖吸附剂的制备方法具体为:取50 mL交联多孔壳聚糖CCB加到35 mL含有0.25 g过硫酸铵APS的去离子水中,通入氮气,缓慢搅拌30 min;随后将体系温度升至60 ℃;将1.5 g离子液体[AMIM]Cl溶于15 mL去离子水中,并于15 min内逐滴加入反应液中,氮气保护反应12 h;待反应结束后,用去离子水将产物洗涤至中性,冷冻干燥,将产物P[AMIM]Cl-g-CCB捣碎备用。
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