CN104289199A - 一种用于重金属去除的磁性hpcs/go吸附剂的制备方法及应用 - Google Patents

一种用于重金属去除的磁性hpcs/go吸附剂的制备方法及应用 Download PDF

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CN104289199A
CN104289199A CN201410574931.2A CN201410574931A CN104289199A CN 104289199 A CN104289199 A CN 104289199A CN 201410574931 A CN201410574931 A CN 201410574931A CN 104289199 A CN104289199 A CN 104289199A
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hpcs
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王耀光
魏琴
杜斌
闫涛
胡丽华
闫良国
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University of Jinan
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Abstract

本发明公开了一种用于重金属去除的磁性HPCS/GO吸附剂的制备方法及应用，特征是：将0.3～0.5g羟丙基壳聚糖加入含有20mL水和4～6mL冰醋酸的溶液中，室温下超声2～5h，加入0.05～0.15g磁性SrFe12O19搅拌1～2h，缓慢搅拌下加入3mL液体石蜡，继续搅拌0.5h，加入3mL、25%戊二醛以交联羟丙基壳聚糖，并加入0.1～0.3g氧化石墨烯，在50oC下反应1～2h，用2mol/LNaOH调整pH在9～10，80℃下保持1h，得到的产物依次用石油醚、乙醇、去离子水洗涤至pH为7.0，制得一种用于重金属去除的磁性HPCS/GO吸附剂。该吸附剂制备方法简单易行，吸附重金属的吸附容量高，易分离，可重复利用，吸附过程无二次污染，用于废水中重金属处理效果优良。

Description

一种用于重金属去除的磁性HPCS/GO吸附剂的制备方法及应用
技术领域
本发明属于水处理技术领域，特别涉及一种用于重金属去除的磁性HPCS/GO吸附剂的制备方法及在水处理中对重金属离子吸附的应用技术。
背景技术
近年来，随着工农业的快速发展和人类大规模的生产活动，人们在使用水的同时，也往往使某些有害的物质进入水体，引起天然水体发生物理和化学上的变化。多年来，我国水资源质量不断下降，水环境持续恶化，由于污染所导致的缺水和事故不断发生，不仅使工厂停产、农业减产甚至绝收，而且造成了不良的社会影响和较大的经济损失，严重地威胁了社会的可持续发展，威胁了人类的生存。
其中，重金属污染是水环境污染的重要一部分，它是一种蓄积性的慢性污染，是目前水体污染中最危险的潜在危害，由于具有持久性、生物富集和放大作用，严重危害人类的生存和生命安全，并且一直受到国内外环境学家的关注。重金属种类不同，在溶液中存在的形态各异，因而处理方法也不同。目前已知的处理重金属废水的方法有：化学沉淀法、膜分离法、离子交换法、絮凝法、反渗透法和吸附法。其中，吸附法由于其操作简单和宽的应用范围成为最常用的方法之一。然而，传统的吸附剂有诸如吸附效率差、吸附量低等缺点，因此，开发低成本、高效的吸附剂显得尤为重要。
大量的吸附剂如沸石、粘土、金属氧化物、活性炭等被人们所研究，同时，氧化石墨烯由于其独特的二维结构和大的比表面积也成为研究吸附重金属离子的热点，壳聚糖对重金属离子的吸附也显示出优异的性能。J.R. Rangel-Mendez等研究了壳聚糖对铅离子和镉离子的吸附量分别为7.46和1.79mg/g；Arh-Hwang Chen等研究了表氯醇交联的壳聚糖对铅离子的吸附量为34.1 mg/g；Z.H. Guo等研究了磁性氧化石墨烯对Cr6+的吸附量可达1.03mg/g。然而，将壳聚糖的衍生物与氧化石墨烯结合制得吸附剂用来吸附重金属离子还未见报道。同时，赋予吸附剂磁性可以实现吸附剂与溶液的快速分离。基于此我们制备了一种新型的磁性羟丙基壳聚糖/氧化石墨烯吸附剂，该吸附剂制备方法简单易行，对重金属的吸附容量高，对铬离子、铅离子、镉离子和汞离子的吸附量分别为71.2、81.0、86.2和88.7 mg/g，易分离，可重复利用，吸附过程无二次污染。
发明内容
本发明的目的之一在于提供一种用于重金属去除的磁性HPCS/GO吸附剂的制备方法，获取的一种用于重金属去除的磁性HPCS/GO吸附剂对水中的重金属离子进行吸附分离。
本发明的目的通过以下技术方案实现。
一种用于重金属去除的磁性HPCS/GO吸附剂的制备方法，特征在于该方法具有以下工艺步骤：
将0.3~0.5g羟丙基壳聚糖加入20mL水和4~6mL冰醋酸溶液中，在室温下超声2~5h使其充分溶解，加入0.05~0.15g磁性SrFe12O19搅拌1~2h，在缓慢搅拌下加入3mL液体石蜡，继续搅拌0.5h，加入3 mL、25%戊二醛以交联羟丙基壳聚糖，同时，加入0.1~0.3g氧化石墨烯，在50oC下反应1~2h，用2mol/LNaOH调整pH在9~10，在80oC下保持1h，得到的产物依次用石油醚、乙醇、去离子水洗涤至pH为7.0，制得用于重金属去除的磁性HPCS/GO吸附剂。
本发明的另一目的是提供磁性HPCS/GO吸附剂对水中重金属离子吸附的应用，特点在于如下步骤：
取25mL、30~60mg/L的重金属离子溶液于100mL锥形瓶中，调节pH为3~6，加入10~16mg磁性羟丙基壳聚糖/氧化石墨烯吸附剂，25oC下放在恒温水浴振荡器中振荡1.0~3.0h，取出锥形瓶，用强力磁铁分离吸附剂与溶液，取清液检测重金属离子的浓度，依据溶液中重金属离子的初始浓度C 0和吸附后溶液中重金属离子的浓度C e计算重金属离子的去除率。
本发明的优点及有益效果是：
（1）本发明获得的磁性HPCS/GO吸附剂是一种新型的纳米复合物吸附剂材料，具有良好的物理化学性能和优异的机械强度，吸附容量大，对Cr6+、Pb2+、Cd2+、Hg2+的吸附量分别为71.2、81.0、86.2和88.7 mg/g，可反复使用。
（2）本发明磁性HPCS/GO吸附剂的制备过程简单，条件易于控制，易操作，生产成本低。
（3）本发明获得的磁性HPCS/GO吸附剂对水中的重金属离子吸附效率高，吸附和分离速度快，解吸性能好，能够在较宽的酸碱范围内使用。
具体实施方式
实施例1磁性HPCS/GO吸附剂的制备
将0.3g羟丙基壳聚糖加入20mL水和4mL冰醋酸溶液中，在室温下超声2h使其充分溶解，加入0.05g磁性SrFe12O19搅拌1h，在缓慢搅拌下加入3mL液体石蜡，继续搅拌0.5h，加入3mL、25%戊二醛以交联羟丙基壳聚糖，同时，加入0.1g氧化石墨烯，在50oC下反应1h，用2mol/LNaOH调整pH在9~10，在80oC下保持1h，得到的产物依次用石油醚、乙醇、去离子水洗涤至pH为7.0，制得磁性HPCS/GO吸附剂。
实施例2 磁性HPCS/GO吸附剂的制备
将0.35g羟丙基壳聚糖加入20mL水和4.5mL冰醋酸溶液中，在室温下超声3h使其充分溶解，加入0.10g磁性SrFe12O19搅拌1.2h，在缓慢搅拌下加入3mL液体石蜡，继续搅拌0.5h，加入3mL、25%戊二醛以交联羟丙基壳聚糖，同时，加入0.15g氧化石墨烯，在50oC下反应1.2h，用2mol/LNaOH调整pH在9~10，在80oC下保持1h，得到的产物依次用石油醚、乙醇、去离子水洗涤至pH为7.0，制得磁性HPCS/GO吸附剂。
实施例3 磁性HPCS/GO吸附剂的制备
将0.4g羟丙基壳聚糖加入20mL水和5mL冰醋酸溶液中，在室温下超声4h使其充分溶解，加入0.10g磁性SrFe12O19搅拌1.5h，在缓慢搅拌下加入3mL液体石蜡，继续搅拌0.5h，加入3mL、25%戊二醛以交联羟丙基壳聚糖，同时，加入0.2g氧化石墨烯，在50oC下反应1.8h，用2mol/LNaOH调整pH在9~10，在80oC下保持1h，得到的产物依次用石油醚、乙醇、去离子水洗涤至pH为7.0，制得磁性HPCS/GO吸附剂。
实施例4 磁性HPCS/GO吸附剂的制备
将0.5g羟丙基壳聚糖加入20mL水和6mL冰醋酸溶液中，在室温下超声5h使其充分溶解，加入0.15g磁性SrFe12O19搅拌2h，在缓慢搅拌下加入3mL液体石蜡，继续搅拌0.5h，加入3mL、25%戊二醛以交联羟丙基壳聚糖，同时，加入0.3g氧化石墨烯，在50oC下反应2h，用2mol/LNaOH调整pH在9~10，在80oC下保持1h，得到的产物依次用石油醚、乙醇、去离子水洗涤至pH为7.0，制得磁性HPCS/GO吸附剂。
实施例5 磁性HPCS/GO吸附剂对Cr（VI）的吸附
取25mL、30mg/L的Cr6+离子溶液于100mL锥形瓶中，调节pH为3，加入10mg磁性羟丙基壳聚糖/氧化石墨烯吸附剂，25oC下放在恒温水浴振荡器中振荡1.0h，取出锥形瓶，用强力磁铁分离吸附剂与溶液，取清液检测Cr6+离子的浓度，依据溶液中Cr6+离子的初始浓度C 0和吸附后溶液中Cr6+离子的浓度C e计算得Cr6+离子的去除率为95.0%，吸附量为71.2mg/g。
实施例6 磁性HPCS/GO吸附剂对Pb2+离子的吸附
取25mL、40mg/L的Pb2+离子溶液于100mL锥形瓶中，调节pH为5.5，加入12mg磁性羟丙基壳聚糖/氧化石墨烯吸附剂，25oC下放在恒温水浴振荡器中振荡2.0h，取出锥形瓶，用强力磁铁分离吸附剂与溶液，取清液检测Pb2+离子的浓度，依据溶液中Pb2+离子的初始浓度C 0和吸附后溶液中Pb2+离子的浓度C e计算得Pb2+离子的去除率为97.2%，吸附量为81.0mg/g。
实施例7 磁性HPCS/GO吸附剂对Cd2+离子的吸附
取25mL、50mg/L的Cd2+离子溶液于100mL锥形瓶中，调节pH为6，加入14mg磁性羟丙基壳聚糖/氧化石墨烯吸附剂，25oC下放在恒温水浴振荡器中振荡2.5h，取出锥形瓶，用强力磁铁分离吸附剂与溶液，取清液检测Cd2+离子的浓度，依据溶液中Cd2+离子的初始浓度C 0和吸附后溶液中Cd2+离子的浓度C e计算得Cd2+离子的去除率为96.5%，吸附量为86.2mg/g。
实施例8 磁性HPCS/GO吸附剂对Hg2+离子的吸附
取25mL、60mg/L的Hg2+离子溶液于100mL锥形瓶中，调节pH为6，加入16mg磁性羟丙基壳聚糖/氧化石墨烯吸附剂，25oC下放在恒温水浴振荡器中振荡3.0h，取出锥形瓶，用强力磁铁分离吸附剂与溶液，取清液检测Hg2+离子的浓度，依据溶液中Hg2+离子的初始浓度C 0和吸附后溶液中Hg2+离子的浓度C e计算得Hg2+离子的去除率为94.6%，吸附量为88.7mg/g。

Claims (3)

1.一种用于重金属去除的磁性HPCS/GO吸附剂的制备方法，其特征在于，包括以下步骤：
将0.3~0.5g羟丙基壳聚糖HPCS加入20mL水和4~6mL冰醋酸溶液中，在室温下超声2~5h使其充分溶解，加入0.05~0.15g磁性SrFe12O19搅拌1~2h，在缓慢搅拌下加入3mL液体石蜡，继续搅拌0.5h，加入3mL、25%戊二醛以交联羟丙基壳聚糖，同时，加入0.1~0.3g氧化石墨烯GO，在50oC下反应1~2h，用2mol/LNaOH调整pH在9~10，在80oC下保持1h，得到的产物依次用石油醚、乙醇、去离子水洗涤至pH为7.0，制得一种用于重金属去除的磁性HPCS/GO吸附剂。
2.如权利要求1所述的一种用于重金属去除的磁性HPCS/GO吸附剂的制备方法，其特征在于，用于水中重金属离子的去除，步骤如下：
取25mL、30~60mg/L的重金属离子溶液于100mL锥形瓶中，调节pH为3~6，加入10~16mg的磁性HPCS/GO吸附剂，25oC下放在恒温水浴振荡器中振荡1.0~3.0h，取出锥形瓶，用强力磁铁分离吸附剂与溶液，取清液检测重金属离子的浓度，依据溶液中重金属离子的初始浓度C 0和吸附后溶液中重金属离子的浓度C e计算重金属离子的去除率。
3.如权利要求1所述的一种用于重金属去除的磁性HPCS/GO吸附剂的制备方法，其特征在于，重金属离子选自下列之一：Cr6+、Pb2+、Cd2+、Hg2+。
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CN110694591A (zh) * 2019-09-05 2020-01-17 武汉东湖科创中试基地科技有限公司 Fe-GO/Cs复合微球的制备方法及其用途
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CN113083238B (zh) * 2021-03-12 2022-07-26 华南理工大学 一种氨基硫脲功能化氧化石墨烯/壳聚糖复合吸附剂及其制备方法与应用

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