CN110052255B - 一种超分子聚合物磁性重金属吸附剂、制备方法及其应用 - Google Patents
一种超分子聚合物磁性重金属吸附剂、制备方法及其应用 Download PDFInfo
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Abstract
本发明公开了一种超分子聚合物磁性重金属吸附剂及其制备方法,包括以下步骤:S1、将三聚硫氰酸和纳米Fe3O4固体粉末加入蒸馏水中,超声处理,得到悬浮溶液;S2、将三聚氰胺加入到S1中得到的悬浮溶液中,搅拌均匀,然后于80~110℃水热反应2~4h,反应结束后,自然冷却至室温,然后离心、洗涤、干燥,即得到超分子聚合物磁性重金属吸附剂。本发明还公开了上述重金属吸附剂在废水中吸附重金属离子领域上的应用。本发明制备的超分子聚合物磁性重金属吸附剂因含有大量氨基、巯基对重金属离子吸附容量大,且因具有超磁性而易于分离。
Description
技术领域
本发明属于重金属吸附剂制备技术领域,具体涉及一种超分子聚合物磁性重金属吸附剂、制备方法及其应用。
背景技术
随着工业化的快速发展,重金属污染成为危害人体健康和生态系统的重要因素。因此,全球水处理行业对于废水中重金属的有效去除问题都非常重视。在各类处理技术中,吸附技术因操作简易、具有可回收性、不产生大量二次污染物而被广泛采用。吸附剂在吸附处理技术中占据核心地位,已有的吸附剂,如活性炭、硅藻土、功能化氧化硅、碳纳米管、金属氧化物等,或存在分离难、吸附量小,或存在选择性差、再生困难等不足,制约了吸附技术的实际应用。因此,对于重金属治理而言,制造新型多功能吸附剂的任务尤显重要。
含有氮、硫、氧元素的氨基、巯基、羟基和羧基等,因为原子核外电子轨道中有孤对电子,被称为路易斯碱;而重金属离子(称之为路易斯酸)因含有空轨道,易与氨基、巯基、羟基和羧基等中的氮、硫、氧等元素的共用孤对电子,形成络合物被去除。因此,富含氮、硫、氧元素的物质,作为构建新型重金属吸附剂的关键模块,受到广泛关注,例如典型的含氨基、巯基的有机物2,4,6-三巯基-1,3,5-均三嗪,1,3,5-三嗪-2,4,6-三胺等。但因上述纯物质吸附重金属后很难与水分离,导致在实际应用中受到较大限制。
发明内容
本发明的目的在于克服现有技术的不足,提供一种超分子聚合物磁性重金属吸附剂、制备方法及其应用。
本发明的第一个目的是提供一种超分子聚合物磁性重金属吸附剂的制备方法,包括以下步骤:
S1、将三聚硫氰酸(2,4,6-三巯基-1,3,5-均三嗪)和纳米Fe3O4固体粉末加入蒸馏水中,超声处理,得到悬浮溶液;
S2、将三聚氰胺(1,3,5-三嗪-2,4,6-三胺)加入到S1中得到的悬浮溶液中,搅拌均匀,然后于80~110℃水热反应2~4h,反应结束后,自然冷却至室温,然后离心、洗涤、干燥,即得到超分子聚合物磁性重金属吸附剂,其中,1,3,5-三嗪-2,4,6-三胺与S1中使用的2,4,6-三巯基-1,3,5-均三嗪的摩尔比为0.8~2.2:1。
优选的,步骤S1中,所述2,4,6-三巯基-1,3,5-均三嗪与纳米Fe3O4固体粉末的质量比为1:0.2~0.8。
优选的,步骤S2中,所述1,3,5-三嗪-2,4,6-三胺与S1中使用的2,4,6-三巯基-1,3,5-均三嗪的摩尔比为1:1。
优选的,步骤S2中,所述水热反应的温度和时间分别为100℃和2h。
本发明的第二个目的是提供一种上述制备方法制备得到的超分子聚合物磁性重金属吸附剂。
本发明的第三个目的是提供一种上述超分子聚合物磁性重金属吸附剂在吸附废水中重金属离子领域上的应用。
优选的,所述重金属离子为Pb2+、Zn2+、Mg2+或Cd2+。
本发明与现有技术相比,其有益效果在于:
(1)本发明提供的超分子聚合物磁性重金属吸附剂因含有大量氨基、巯基对重金属离子吸附容量大;
(2)本发明提供的超分子聚合物磁性重金属吸附剂因具有超磁性而易于在外加磁场下与废水实现磁分离;
(3)本发明通过超声处理和一次水热反应,即可得到超分子聚合物磁性重金属吸附剂,合成方法简单、操作方便;
(4)本发明提供的超分子聚合物磁性重金属吸附剂对重金属离子Pb2+、Zn2+、Mg2+或Cd2+具有很好的吸附性,并且Pb2+离子在复杂系统中也具有极好的抗干扰能力,本发明提供的超分子聚合物磁性重金属吸附剂对复杂系统中的Pb2+离子仍然具有良好的灵敏度和选择性,在废水净化领域具有良好的市场应用前景。
附图说明
图1为本发明实施例1制备的超分子聚合物磁性重金属吸附剂的扫描电镜图;
图2为本发明实施例1制备的超分子聚合物磁性重金属吸附剂的XRD图;
图3为本发明实施例1制备的超分子聚合物磁性重金属吸附剂吸附Pb2+离子浓度-时间曲线图。
具体实施方式
下面结合附图对发明的具体实施方式进行详细描述,但应当理解本发明的保护范围并不受具体实施方式的限制。下列实施例中未注明具体条件的试验方法,通常按照常规条件,或者按照各制造商所建议的条件。
以下实施例中纳米Fe3O4固体粉末的制备参考文献:Angewandte Chemie.2005,117,2842-2845。
实施例1
一种超分子聚合物磁性重金属吸附剂的制备方法,包括以下步骤:
S1、将0.886g的2,4,6-三巯基-1,3,5-均三嗪和0.400g的纳米Fe3O4固体粉末加入60mL蒸馏水中,超声处理1h,得到悬浮溶液;
S2、将S1得到的悬浮溶液加入反应釜中,接着加入0.630g的1,3,5-三嗪-2,4,6-三胺,搅拌均匀,然后于100℃水热反应2h,反应结束后,自然冷却至室温,离心收集灰色固体,用水和乙醇洗涤多次,然后于真空烘箱中60℃干燥24h后得到灰色粉末,即为超分子聚合物磁性重金属吸附剂。
实施例2
一种超分子聚合物磁性重金属吸附剂的制备方法,包括以下步骤:
S1、将0.443g的2,4,6-三巯基-1,3,5-均三嗪和0.089g的纳米Fe3O4固体粉末加入40mL蒸馏水中,超声处理1h,得到悬浮溶液;
S2、将S1得到的悬浮溶液加入反应釜中,接着加入0.694g的1,3,5-三嗪-2,4,6-三胺,搅拌均匀,然后于95℃水热反应3h,反应结束后,自然冷却至室温,离心收集灰色固体,用水和乙醇洗涤多次,然后于真空烘箱中60℃干燥24h后得到灰色粉末,即为超分子聚合物磁性重金属吸附剂。
实施例3
一种超分子聚合物磁性重金属吸附剂的制备方法,包括以下步骤:
S1、将0.443g的2,4,6-三巯基-1,3,5-均三嗪和0.220g的纳米Fe3O4固体粉末加入40mL蒸馏水中,超声处理1h,得到悬浮溶液;
S2、将S1得到的悬浮溶液加入反应釜中,接着加入0.473g的1,3,5-三嗪-2,4,6-三胺,搅拌均匀,然后于80℃水热反应4h,反应结束后,自然冷却至室温,离心收集灰色固体,用水和乙醇洗涤多次,然后于真空烘箱中60℃干燥24h后得到灰色粉末,即为超分子聚合物磁性重金属吸附剂。
实施例4
一种超分子聚合物磁性重金属吸附剂的制备方法,包括以下步骤:
S1、将0.886g的2,4,6-三巯基-1,3,5-均三嗪和0.709g的纳米Fe3O4固体粉末加入60mL蒸馏水中,超声处理1h,得到悬浮溶液;
S2、将S1得到的悬浮溶液加入反应釜中,接着加入0.505g的1,3,5-三嗪-2,4,6-三胺,搅拌均匀,然后于110℃水热反应2h,反应结束后,自然冷却至室温,离心收集灰色固体,用水和乙醇洗涤多次,然后于真空烘箱中60℃干燥24h后得到灰色粉末,即为超分子聚合物磁性重金属吸附剂。
下面以实施例1为例,对本发明合成的超分子聚合物磁性重金属吸附剂的结构和吸附性能进行研究
(1)结构研究
图1为本发明实施例1提供的超分子聚合物磁性重金属吸附剂的扫描电镜图。通过图1可看出,重金属吸附剂由长短不等的棒状聚合物和直径约为400nm的Fe3O4磁性纳米颗粒复合组成,分布非常均匀。
图2为本发明实施例1提供的超分子聚合物磁性重金属吸附剂的XRD图。通过图2可以看出,合成的重金属吸附剂里含有超分子聚合物和Fe3O4的特征峰,其结果与图1的形貌结果一致。
(2)吸附性能研究
在5个50mLd的碘量瓶中分别加入25mg本发明实施例1制备的超分子聚合物磁性重金属吸附剂,然后向5个碘量瓶中依次分别加入25mL的Pb2+、Mg2+、Zn2+和Cd2+的金属盐溶液(各金属盐溶液中金属离子的浓度均为200mg/L)以及上述四种离子的混合金属盐溶液(其中,Pb2+、Mg2+、Zn2+和Cd2+的浓度均为200mg/L),分别调pH至4,在25℃于恒温水浴振荡器中以120rpm摇动6h,接着用外加磁铁从样品溶液中分离出磁性重金属吸附剂,然后用电感耦合等离子体质谱仪(ICP-MS)分析溶液中所有金属离子的浓度。
通过测定得到:超分子聚合物磁性重金属吸附剂对单一金属离子Pb2+、Mg2+、Zn2+和Cd2+的平衡吸附量分别为164.8mg/g、81.0mg/g、72.6mg/g和54.4mg/g,说明超分子聚合物磁性重金属吸附剂对Pb2+、Mg2+、Zn2+和Cd2+均有较好的吸附性;同时,经检测得到,在上述各金属离子共存情况下,超分子聚合物磁性重金属吸附剂分别对Pb2+、Mg2+、Zn2+和Cd2+的平衡吸附量为112.3mg/g、48.1mg/g、35.7mg/g和23.8mg/g,通过上述结果可知,在Pb2+与其它二价金属离子共存的情况下,超分子聚合物磁性重金属吸附剂对Pb2+能够选择识别并吸附,并且具有更高的捕获能力,吸附能力顺序为:Pb2+>Zn2+>Mg2+>Cd2+。因此,该磁性吸附剂对Pb2+、Mg2 +、Zn2+和Cd2+重金属离子具有较好的吸附性,尤其对Pb2+具有更好的吸附性,可以作为吸附剂在废水净化处理中进行实际应用。
(3)超分子聚合物磁性重金属吸附剂对Pb2+的吸附时间研究
分别取25mL的浓度为200mg/L的Pb2+溶液加入11个碘量瓶中,接着加入30mg超分子聚合物磁性重金属吸附剂,将上述碘量瓶置于恒温水浴振荡器中于25℃下以120rpm分别摇动10min、20min、30min、60min、80min、100min、120min、180min、240min、480min及720min,用外加磁铁从上述各样品溶液中分离出磁性重金属吸附剂,然后用电感耦合等离子体质谱仪(ICP-MS)分析各碘量瓶中的Pb2+的浓度。图3为超分子聚合物磁性重金属吸附剂吸附Pb2+的浓度-时间曲线图。通过图3可以看出,在早期阶段,平衡吸附量在100分钟内迅速降低,然后随着时间增加继续降低,240分钟后增加量很少。因此,超分子聚合物磁性重金属吸附剂对Pb2+的吸附最佳时间为240min。
综上所述,本发明实施例提供的超分子聚合物磁性重金属吸附剂对重金属离子Pb2+、Zn2+,Mg2+或Cd2+均具有很好的吸附性,且对Pb2+具有更高的捕获能力和吸附能力,同时对Pb2+的吸附最佳时间为240min。
需要说明的是,本发明权利要求书中涉及数值范围时,应理解为每个数值范围的两个端点以及两个端点之间任何一个数值均可选用,由于采用的步骤方法与实施例相同,为了防止赘述,本发明描述了优选实施例及其效果,但本领域内的技术人员一旦得知了基本创造性概念,则可对这些实施例作出另外的变更和修改。所以,所附权利要求意欲解释为包括优选实施例以及落入本发明范围的所有变更和修改。
显然,本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。
Claims (6)
1.一种超分子聚合物磁性重金属吸附剂的制备方法,其特征在于,包括以下步骤:
S1、将三聚硫氰酸和纳米Fe3O4固体粉末加入蒸馏水中,超声处理,得到悬浮溶液;
S2、将三聚氰胺加入到S1中得到的悬浮溶液中,搅拌均匀,然后于80~110℃水热反应2~4h,反应结束后,自然冷却至室温,然后离心、洗涤、干燥,即得到超分子聚合物磁性重金属吸附剂,其中,三聚氰胺与S1中使用的三聚硫氰酸的摩尔比为0.8~2.2:1;
步骤S1中,所述三聚硫氰酸与纳米Fe3O4固体粉末的质量比为1:0.2~0.8。
2.根据权利要求1所述的超分子聚合物磁性重金属吸附剂的制备方法,其特征在于,步骤S2中,所述三聚氰胺与S1中使用的三聚硫氰酸的摩尔比为1:1。
3.根据权利要求1所述的超分子聚合物磁性重金属吸附剂的制备方法,其特征在于,步骤S2中,所述水热反应的温度和时间分别为100℃和2h。
4.一种根据权利要求1~3任一项所述的制备方法制备得到的超分子聚合物磁性重金属吸附剂。
5.一种根据权利要求4所述的超分子聚合物磁性重金属吸附剂在吸附废水中重金属离子领域上的应用。
6.根据权利要求5所述超分子聚合物磁性重金属吸附剂在吸附重金属离子领域上的应用,其特征在于,所述重金属离子为Pb 2+、Zn2+或Cd2+。
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