CN115569637B - 快速去除污染物的可回收纳米材料改性磁性浒苔水凝胶 - Google Patents
快速去除污染物的可回收纳米材料改性磁性浒苔水凝胶 Download PDFInfo
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Abstract
本发明属于水处理技术领域,涉及可回收纳米材料改性磁性浒苔水凝胶。该方法包括:(1)将浒苔粉末分散于水中,加入高锰酸钾,不断搅拌,反应10min;反应结束后,冷冻干燥;(2)加入聚乙二醇使改性浒苔悬浮,加入纳米材料,搅拌分散均匀;(3)取交联剂加入步骤(2)得到的悬浮体系中,不断搅拌,室温下反应30min,静置凝固后,多次清洗,冷冻干燥,得到纳米材料改性浒苔凝胶;(4)将纳米材料改性浒苔凝胶浸泡在含有Fe3+和Fe2+的铁盐水溶液中溶胀;(5)待其达到溶胀平衡后,转移至NaOH溶液中浸泡1 d,得到纳米材料改性磁性浒苔水凝胶。本发明利用浒苔自身官能团之间互相交联,制备出的水凝胶具有较强的稳定性。
Description
技术领域
本发明属于水处理技术领域,涉及可回收纳米材料改性磁性浒苔水凝胶及其制备方法和用途。
背景技术
工业化的快速发展在给人类社会生活带来便利的同时,也带来了巨大的问题。其中,水污染问题最为严重。工业废水中的重金属离子和染料将在食物链中富集并最终进入人体,这将导致人体致畸、致癌和诱变效应。染料和重金属离子废水在污染水体环境的同时,对水生态系统、动物和人类的生命安全也造成很大的威胁。近年来,随着环保意识的逐渐增强,处理染料和重金属离子废水的新方法不断提出,处理方法日趋新异。目前,对染料和重金属离子废水的处理方法虽然很多,但大多存在投入高、重 复利用率低、工艺繁琐、处理的金属离子单一、会给环境造成二次污染、对重金属离子选择性差、不能同时分离多种重金属离子等缺点。而吸附法具有适用范围广、反应速度快、可适应不同反应条件、环境友 好等特点和优势,受到了国内外研究机构及科研工作者的高度关注,成为当下研究的热点。特别是采用水凝胶吸附材料处理重金属和染料废水具有独特的优势,成为废水处理的研究重点。
浒苔作为一种绿藻纲植物,生长在中潮带滩涂。浒苔虽然无毒,但是和赤潮一样,每到夏天都会大量繁殖泛滥在海边,不仅会影响海边人民的活动,还会带来恶臭的味道,浒苔也能遮蔽阳光,影响海底藻类的生长;死亡的浒苔也会消耗海水中的氧气。由于全球气候变化、水体富营养化等原因,造成海洋大型海藻浒苔绿潮暴发。合理利用浒苔制备吸附剂可以降低吸附剂的开发成本,具有绿色环保价值。
发明内容
本发明的目的是提供一种利用浒苔为原料制备回收的磁性浒苔水凝胶的制备方法。浒苔自身含有氨基、羧基、羟基等基团,羟基占比最大,可自身交联(避免过多化学试剂的加入和环境毒性)。首先浒苔的羟基部分被高锰酸钾氧化成羧基,再通过添加N-羟基琥珀酰亚胺交联剂进行自身交联得到浒苔水凝胶。纳米级别的氧化镧对有机污染物和重金属具有吸附和催化降解的协同高效能,但是其极易团聚和使用后难以回收,暴漏于环境中会产生环境毒性。将其固定于浒苔水凝胶内部,可解决团聚问题,使其发挥最大效能,也可以将其固定于凝胶内部,使用后回收,避免其暴漏于环境中,同时也可以使污染物去除。
为了实现上述目的,本发明采用的技术方案是:快速去除污染物的可回收纳米材料改性磁性浒苔水凝胶的制备方法,包括:
(1)将制备的浒苔粉末分散于水中,加入高锰酸钾,不断搅拌,反应10-20min;反应结束后,冷冻干燥,得到改性浒苔粉末;其中,浒苔粉末与高锰酸钾的质量配比为20:1;浒苔粉末与水的质量体积比为:(0.5-1):1,g/ml;
(2)取步骤(1)的改性浒苔粉末分散于水中,以(0.5-1):1的体积比加入聚乙二醇使改性浒苔悬浮,加入纳米材料,搅拌分散均匀;纳米材料与浒苔粉末的质量比为1:10;
(3)取交联剂0.2-0.5g加入步骤(2)得到的悬浮体系中,不断搅拌,室温下反应20-30min,静置凝固后,多次清洗,冷冻干燥,得到纳米材料改性浒苔凝胶;交联剂与浒苔粉末的质两配比为(0.2-0.5):(1-2);
(4)将纳米材料改性浒苔凝胶浸泡在含有Fe3+和Fe2+的铁盐水溶液中溶胀;
(5)待其达到溶胀平衡后,转移至浓度为0.5%-1%的NaOH 溶液中再浸泡1-2 d,得到纳米材料改性磁性浒苔水凝胶。
优选地,铁盐水溶液中Fe3+与Fe2+的物质的量比为2∶1,溶液的浓度为 1 mol/L。
优选地,所述的纳米材料选自纳米氧化镧或纳米氧化铈。
优选地,所述的交联剂为N-羟基琥珀酰亚胺。
优选地,本发明提供一种快速去除污染物的可回收纳米材料改性磁性浒苔水凝胶,以浒苔粉末为原料,采用所述的方法制备而成。
优选地,本发明还进一步提供一种快速去除污染物的可回收纳米材料改性磁性浒苔水凝胶的用途,用于去除水中有机污染物或重金属。
优选地,本发明还进一步提供一种去除水中有机污染物或重金属的方法,在含有邮寄污染物或重金属的水中加入所述的快速去除污染物的可回收纳米材料改性磁性浒苔水凝胶,浒苔水凝胶的投加量为0.5-1g/L。
本发明与现有技术相比,有益效果在于:
(1)本发明提供的浒苔水凝胶具备磁性,可回收,回收率达97%;
(2)本发明提供的磁性浒苔水凝胶对污染物表现出良好的吸附性能;
(3)本发明合理的利用了泛滥的浒苔作为吸附复合材料,对生态环境具有积极的作用;
(4)本发明提供的制备方法利用浒苔自身官能团之间互相交联,操作简单,避免了引入过多化学试剂,制备出的水凝胶具有较强的稳定性。
附图说明
图1为磁性改性前、后纳米材料改性浒苔水凝胶对甲基橙的吸附情况对比;
图2为甲基橙溶液不同初始浓度本发明的水凝胶吸附效果的影响;
图3为磁性改性前、后纳米材料改性浒苔水凝胶对铬的吸附情况对比;
图4为铬溶液不同初始浓度本发明的水凝胶吸附效果的影响;
图5为本发明提供的水凝胶的磁性示意图。
具体实施方式
为了便于理解本发明,下面结合附图和具体实施例,对本发明进行更详细的说明。附图中给出了本发明的较佳的实施例。但是,本发明可以以许多不同的形式来实现,并不限于本说明书所描述的实施例。相反地,提供这些实施例的目的是使对本发明公开内容的理解更加透彻全面。
实施例1 本实施例提供的快速去除污染物的可回收纳米材料改性磁性浒苔水凝胶的制备方法,具体包括以下步骤:
(1)浒苔清洗,冷冻干燥,粉碎,过100目筛网。取2g浒苔粉末分散于20ml水中,加入0.1g 高锰酸钾,不断搅拌,反应10min。清水冲洗多次,冷冻干燥。高锰酸钾作为氧化剂,使浒苔中部分羟基氧化为羧基,利于自交联。
(2)取步骤(1)的改性浒苔粉末2g分散于20ml水中,加入1ml聚乙二醇600使改性浒苔悬浮,加入0.1g纳米氧化镧,搅拌分散均匀,使纳米氧化镧进入到浒苔管状结构中。
纳米氧化镧极易团聚,在管状结构中的纳米氧化镧可高分分散,避免其团聚,以实现有机污染物和重金属和吸附/催化降解一体化反应。
(3)取0.2 g N-羟基琥珀酰亚胺交联剂加入步骤(2)得到的悬浮体系中,不断搅拌,室温下反应30min,静置凝固后,多次清洗,冷冻干燥,得到氧化镧改性浒苔凝胶。
(4)将氧化镧改性凝胶浸泡含有Fe3+和Fe2+的铁盐水溶液中溶胀 1d,Fe3+与Fe2+的物质的量比为2∶1,溶液的浓度为 1 mol/L。本步骤采用原位改性,牢固,简单,均一。
(5)待其达到溶胀平衡后,转移至浓度为0.5% 的NaOH 溶液中再浸泡1 d,在水凝胶网络中原位生成了Fe3O4,得到纳米材料改性磁性浒苔水凝胶。
本实施例制备的快速去除污染物的可回收纳米材料改性磁性浒苔水凝胶具有磁性,能够被磁铁吸附,如图5所示。
实施例2 本实施例提供的快速去除污染物的可回收纳米材料改性磁性浒苔水凝胶的制备方法,具体包括以下步骤:
(1)浒苔清洗,冷冻干燥,粉碎,过100目筛网。取1g浒苔粉末分散于20ml水中,加入0.05g 高锰酸钾,不断搅拌,反应10min。清水冲洗多次,冷冻干燥。高锰酸钾作为氧化剂,使浒苔中部分羟基氧化为羧基,利于自交联。
(2)取步骤(1)的改性浒苔粉末2g分散于20ml水中,加入2ml聚乙二醇600使改性浒苔悬浮,加入0.2g纳米氧化铈,搅拌分散均匀,使纳米氧化铈进入到浒苔管状结构中。
纳米氧化镧极易团聚,在管状结构中的纳米氧化镧可高分分散,避免其团聚,以实现有机污染物和重金属和吸附/催化降解一体化反应。
(3)取0.18g N-羟基琥珀酰亚胺交联剂加入步骤(2)得到的悬浮体系中,不断搅拌,室温下反应30min,静置凝固后,多次清洗,冷冻干燥,得到氧化镧改性浒苔凝胶。
(4)将氧化镧改性凝胶浸泡含有Fe3+和Fe2+的铁盐水溶液中溶胀 1d,Fe3+与Fe2+的物质的量比为2∶1,溶液的浓度为 1 mol/L。本步骤采用原位改性,牢固,简单,均一。
(5)待其达到溶胀平衡后,转移至浓度为0.8% 的NaOH 溶液中再浸泡1 d,在水凝胶网络中原位生成了Fe3O4,得到纳米材料改性磁性浒苔水凝胶。
实施例3 实施例1制备的可回收纳米材料改性磁性浒苔水凝胶对不同浓度甲基橙的吸附实验
对比例:纳米材料改性浒苔水凝胶的制备(未经磁性改性)
(1)浒苔清洗,冷冻干燥,粉碎,过100目筛网。取2g浒苔粉末分散于20ml水中,加入0.1g 高锰酸钾,不断搅拌,反应10min。清水冲洗多次,冷冻干燥。
(2)取步骤(1)的改性浒苔粉末2g分散于20ml水中,加入1ml聚乙二醇600使改性浒苔悬浮,加入1g纳米氧化镧,搅拌分散均匀,使纳米氧化镧进入到浒苔管状结构中。
(3)取0.2 g N-羟基琥珀酰亚胺交联剂加入步骤二得到的悬浮体系中,不断搅拌,室温下反应30min,静置凝固后,多次清洗,冷冻干燥,得到纳米材料改性浒苔凝胶。
吸附实验:
取一定量吸附剂于50mL离心管中,加入不同浓度的甲基橙溶液,放进水浴恒温震荡器中震荡,调节转速为210rpm,在不同时间用5mL注射器取出样品,过0.45 μm滤膜得到滤液。用紫外分光光度计,在最大吸收波长λm = 272 nm处测定滤液的吸光度。
表1 本发明的水凝胶对甲基橙的去除实验
如图1所示,通过磁性改性前、后对同一浓度的甲基橙进行吸附对比,磁性改性后的水凝胶(实施例1制备的)具有更好的吸附性能,且磁改后的饱和点要远快于未经磁性改性的(对比例)。
图2不同甲基橙的浓度对水凝胶吸附的影响各不相同,当浓度处于350 mg/L的时候吸附量是处于最佳状态,从350 mg/L之前的水凝胶的吸附量一直处于增长的状态,这可能是因为随着浓度差的越来越大对于水凝胶的吸附处于促进的作用,致使吸附量的不断增加。当甲基橙浓度高于350 mg/L后,此时的浓度差已经不能再起到促进的作用,因为水凝胶此时已经处于饱和状态,吸附量并不会再随着浓度差的增加而增加。
实施例4实施例1制备的可回收纳米材料改性磁性浒苔水凝胶对铬的吸附实验
取一定量吸附剂于50mL离心管中,加入不同浓度的重铬酸钾溶液,放进气浴恒温震荡器中震荡,调节转速为210rpm,在不同时间用5mL注射器取出样品,过0.45 μm滤膜得到滤液。再通过添加显色剂,显色10分钟后反应以去离子水作为空白对照,用紫外分光光度计,在最大吸收波长λm = 540 nm处测定滤液的吸光度。
表2 本发明的水凝胶对铬的去除实验
如图3所示,通过改性前后对同一浓度的铬进行吸附对比,磁性改性后的水凝胶具有更好的吸附性能,且磁改后的饱和点要远快于未经磁性改性的(对比例)。
如图4所示,不同铬的浓度对水凝胶吸附的影响各不相同,当浓度处于80 mg/L的时候吸附量是处于最佳状态,从80 mg/L之前的水凝胶的吸附量一直处于增长的状态,这可能是因为随着浓度差的越来越大对于水凝胶的吸附处于促进的作用,致使吸附量的不断增加。当铬浓度高于80 mg/L后,此时的浓度差已经不能再起到促进的作用,因为水凝胶此时已经处于饱和状态,吸附量并不会再随着浓度差的增加而增加。
Claims (7)
1.一种快速去除污染物的可回收纳米材料改性的磁性浒苔水凝胶的制备方法,其特征在于,包括:
(1)将制备的浒苔粉末分散于水中,加入高锰酸钾,不断搅拌,反应10-20min;反应结束后,冷冻干燥;其中,浒苔粉末与高锰酸钾的质量配比为20:1;浒苔粉末与水的质量体积比为(0.5-1):1,g/ml;
(2)取步骤(1)的改性浒苔粉末分散于20ml水中,加入1ml或2ml聚乙二醇600使改性浒苔悬浮;加入纳米材料,搅拌分散均匀;纳米材料与浒苔粉末的质量比为1:10;所述的纳米材料选自纳米氧化镧或纳米氧化铈;
(3)取交联剂0.2-0.5g加入步骤(2)得到的悬浮体系中,不断搅拌,室温下反应20-30min,静置凝固后,多次清洗,冷冻干燥,得到纳米材料改性浒苔凝胶;交联剂与浒苔粉末的质量配比为(0.2-0.5):(1-2);
(4)将纳米材料改性浒苔凝胶浸泡在含有Fe3+和Fe2+的铁盐水溶液中溶胀;
(5)待其达到溶胀平衡后,转移至浓度为0.5%-1%的NaOH 溶液中再浸泡1-2 d,得到纳米材料改性磁性浒苔水凝胶。
2. 根据权利要求1所述的快速去除污染物的可回收纳米材料改性的磁性浒苔水凝胶的制备方法,其特征在于,铁盐水溶液中Fe3+与Fe2+的物质的量比为2∶1,溶液的浓度为 1mol/L。
3.根据权利要求1所述的快速去除污染物的可回收纳米材料改性的磁性浒苔水凝胶的制备方法,其特征在于,所述的交联剂为N-羟基琥珀酰亚胺。
4.一种快速去除污染物的可回收纳米材料改性的磁性浒苔水凝胶,其特征在于:以浒苔粉末为原料,采用如权利要求1-3任一项所述的方法制备而成。
5.如权利要求4所述的快速去除污染物的可回收纳米材料改性的磁性浒苔水凝胶的回收方法,其特征在于:采用磁铁吸附回收使用后的浒苔水凝胶。
6.一种如权利要求4所述的快速去除污染物的可回收纳米材料改性的磁性浒苔水凝胶的用途,其特征在于:用于去除水中有机污染物或重金属。
7.一种去除水中有机污染物或重金属的方法,其特征在于:在含有有机污染物或重金属的水中加入如权利要求4所述的快速去除污染物的可回收纳米材料改性的磁性浒苔水凝胶,投加量为0.5-1g/L。
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