CN112547017A - 一种MIL-100(Fe)磁性纳米复合材料及其制备方法 - Google Patents
一种MIL-100(Fe)磁性纳米复合材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及吸附材料领域,具体涉及一种MIL‑100(Fe)磁性纳米复合材料及其制备方法。MIL‑100(Fe)磁性纳米复合材料,其为氧化石墨烯、磁性物质和MIL‑100(Fe)的复合物。制备方法中,将氧化石墨烯、Fe3O4‑COOH、硝酸铁、均苯三甲酸和硝酸溶解于水中得到的混合液,超声处理30~60min后,于110~130℃下加热12~24小时得到粉末。本发明得到的MIL‑100(Fe)磁性纳米复合材料可以利用MIL‑100(Fe)、氧化石墨烯、磁性物质复合的相互作用,从而显著的提高吸附去除废水中含染料的有机污染物的效果,稳定性好,可重复使用。
Description
技术领域
本发明涉及吸附材料领域,具体涉及一种MIL-100(Fe)磁性纳米复合材料及其制备方法。
背景技术
有机染料的整个生产过程中,都会产生大量的染料废水,特别是在磺化、硝化、还原氧化、重氮化和盐析过程中。有机染料含有对人类和环境有害的化学成分,其中大多数会对人类和哺乳动物有机体产生致癌作用。
作为新兴起的多孔材料MOF,一种有机-无机杂化金属有机骨架材料,可调控性大,通过改变金属和配体种类来改变孔径大小结构,进而改变比表面积,使其具有“特定”的吸附功能,即不同种类的MOFs对不同物质具有不同的吸附效果,采用羧酸类的配位化合物可使其结构稳定,在进行吸附、脱附后不易坍塌。氧化石墨烯(GO)可通过静电作用、π-π堆积和氢键相互作用进行废水处理,也被认为是潜在的环境清洁吸附剂,但是MOF或GO从水溶液中的低分离效率仍然限制了其工业应用。迄今为止,如何同时利用MOF/GO的吸附特性和开发有效方法来克服分离问题仍然是一个挑战。
发明内容
(一)要解决的技术问题
鉴于现有技术的上述缺点、不足,本发明提供一种MIL-100(Fe)磁性纳米复合材料,其为氧化石墨烯、磁性物质和MIL-100(Fe)的复合物,其可以充分利用磁性纳米颗粒和金属有机骨架、氧化石墨烯的优势,使其具有更高的吸附效率和在水中更高的分离效率。
相应地,本发明还提供上述MIL-100(Fe)磁性纳米复合材料的制备方法。
(二)技术方案
为了达到上述目的,本发明采用的主要技术方案包括:
第一方面,本发明实施例提供一种MIL-100(Fe)磁性纳米复合材料,其为氧化石墨烯、磁性物质和MIL-100(Fe)的复合物。
可选地,其为GO@Fe3O4-COOH@MIL-100(Fe)。
第二方面,本发明实施例还提供上述MIL-100(Fe)磁性纳米复合材料的制备方法,其包括以下步骤:将氧化石墨烯、Fe3O4-COOH、硝酸铁、均苯三甲酸和硝酸溶解于水中得到的混合液,超声处理30~60min后,于110~130℃下加热12~24小时得到粉末。
可选地,其还包括以下步骤:将粉末用水和无水乙醇分别洗涤两次,每次洗涤时间为30~60min;洗涤后放置于80~100℃中真空干燥8~10小时,研磨得到MIL-100(Fe)磁性纳米复合材料。
可选地,混合液中氧化石墨烯的质量分数为2~6wt%。
可选地,混合液中各组分按摩尔份分别为Fe3O4-COOH为0.001~0.002份、硝酸铁为0.003~0.005份、均苯三甲酸0.002~0.004份、硝酸浓度为0.006~0.015份。
(三)有益效果
本发明的有益效果是:本发明的MIL-100(Fe)磁性纳米复合材料,由于采用氧化石墨烯、磁性物质和MIL-100(Fe)的组合,相对于现有技术而言,其可以利用MIL-100(Fe)、氧化石墨烯、磁性物质复合的相互作用,从而显著的提高吸附去除废水中含染料的有机污染物的效果,稳定性好,可重复使用,在废水处理中具有良好的应用前景,且具有良好的磁性,从而实现固液分离的简易分离。
附图说明
图1为本发明实施例2所得磁性纳米复合材料的扫描电镜图;
图2为本发明实施例2所得磁性纳米复合材料的XRD图;
图3为不同吸附剂对罗丹明B吸附脱色去除率的柱状图。
具体实施方式
为了更好的解释本发明,以便于理解,下面结合附图,通过具体实施方式,对本发明作详细描述。
【实施方式一】
本发明为了提高金属有机骨架MIL-100(Fe)、氧化石墨烯以及磁性材料的去除污染物的能力,并提高其稳定性,实现多次的重复利用,提供了一种MIL-100(Fe)磁性纳米复合材料,其为氧化石墨烯、磁性物质和MIL-100(Fe)的复合物。
本发明通过氧化石墨烯、磁性物质和MIL-100(Fe)制成的MIL-100(Fe)磁性纳米复合材料,使氧化石墨烯、磁性物质和MIL-100(Fe)之间发生协同效应,显著提高吸附特性。
优选地,其具体为GO@Fe3O4-COOH@MIL-100(Fe),其具有很强的吸附特性和稳定性。在MIL-100(Fe)的金属有机骨架中,优选与氧化石墨烯GO和磁性物质Fe3O4-COOH制得的复合物,其具有最好的吸附性。采用石墨烯替换氧化石墨烯,或者采用其它的磁性物质替换Fe3O4-COOH制得的复合物,吸附性和稳定性都显著小于GO@Fe3O4-COOH@MIL-100(Fe)。
【实施方式二】
本发明为成功制得上述MIL-100(Fe)磁性纳米复合材料,提供了以下的制备方法,其包括以下步骤:将氧化石墨烯、Fe3O4-COOH、硝酸铁、均苯三甲酸和硝酸溶解于水中得到的混合液,超声处理30~60min后,于110~130℃下加热12~24小时得到粉末。
本发明的制备方法简单,上述的方法可以克服氧化石墨烯、Fe3O4-COOH和MIL-100(Fe)之间团聚的困难,且制得的MIL-100(Fe)磁性纳米复合材料引入较少的杂质。
为了提高MIL-100(Fe)磁性纳米复合材料,其还包括以下步骤:将粉末用水和无水乙醇分别洗涤两次,每次洗涤时间为30~60min;洗涤后放置于80~100℃中真空干燥8~10小时,研磨得到MIL-100(Fe)磁性纳米复合材料。
其中,混合液中氧化石墨烯的质量分数为2~6wt%。
其中,混合液中各组分按摩尔份分别为Fe3O4-COOH为0.001~0.002份、硝酸铁为0.003~0.005份、均苯三甲酸0.002~0.004份、硝酸浓度为0.006~0.015份。
为了更好的理解上述技术方案,下面将参照附图更详细地描述本发明的示例性实施例。虽然附图中显示了本发明的示例性实施例,然而应当理解,可以以各种形式实现本发明而不应被这里阐述的实施例所限制。相反,提供这些实施例是为了能够更清楚、透彻地理解本发明,并且能够将本发明的范围完整的传达给本领域的技术人员。
实施例1
MIL-100(Fe)磁性纳米复合材料,其步骤为:
S1依次将氧化石墨烯、Fe3O4-COOH、硝酸铁、均苯三甲酸和硝酸溶解于25mL的水中得到的混合物,使氧化石墨烯含量为2wt%,使Fe3O4-COOH、硝酸铁、均苯三甲酸和硝酸浓度分别为0.001mol/L、0.003mol/L、0.002mol/L和0.006mol/L,再超声30min使之形成清晰的混合溶液;
S2将得到的混合溶液转移到不锈钢反应釜中,在110℃下加热12小时;
S3冷却至室温后,离心得到的棕色粉末,用水和无水乙醇分别洗涤两次,每次洗涤时间为30min;洗涤后放置于80℃中真空干燥8小时,研磨得到MIL-100(Fe)磁性纳米复合材料。
实施例2
MIL-100(Fe)磁性纳米复合材料,其步骤为:
S1依次将氧化石墨烯、Fe3O4-COOH、硝酸铁、均苯三甲酸和硝酸溶解于25mL的水中得到的混合物,使氧化石墨烯含量为4wt%,使Fe3O4-COOH、硝酸铁、均苯三甲酸和硝酸浓度分别为0.0015mol/L、0.004mol/L、0.003mol/L和0.01mol/L,再超声45min使之形成清晰的溶液;
S2将得到的溶液转移到不锈钢反应釜中,在120℃下加热18小时;
S3冷却至室温后,离心得到的棕色粉末,用水和无水乙醇分别洗涤两次,每次洗涤时间为45min;洗涤后放置于90℃中真空干燥9小时,研磨得到MIL-100(Fe)磁性纳米复合材料。
实施例3
MIL-100(Fe)磁性纳米复合材料,其步骤为:
S1依次将氧化石墨烯、Fe3O4-COOH、硝酸铁、均苯三甲酸和硝酸溶解于25mL的水中得到的混合物,使氧化石墨烯含量为6wt%,使Fe3O4-COOH、硝酸铁、均苯三甲酸和硝酸浓度分别为0.002mol/L、0.005mol/L、0.004mol/L和0.015mol/L,再超声60min使之形成清晰的混合溶液;
S2将得到的混合溶液溶液转移到不锈钢反应釜中,在130℃下加热24小时;
S3冷却至室温后,离心得到的棕色粉末,用水和无水乙醇分别洗涤两次,每次洗涤时间为60min;洗涤后放置于100℃中真空干燥10小时,研磨得到MIL-100(Fe)磁性纳米复合材料。
为验证本发明所得到的MIL-100(Fe)磁性纳米复合材料的吸附等特性,通过以下的试验进行验证。
试验一、吸附污染物试验
取相同重量的本实施例1-3所制备的所制备的GO@Fe3O4-COOH@MIL-100(Fe)磁性纳米复合材料与Fe3O4-COOH(对比例1)、氧化石墨烯(对比例2)、Fe3O4-COOH@MIL-100(Fe)(对比例3)、GO@MIL-100(Fe)(对比例4)、氧化石墨烯和Fe3O4-COOH的复合物(对比例5)分别进行罗丹明B去除率效果的对比实验,其中罗丹明B初始浓度为50mg/L,吸附液体积50mL,吸附剂用量0.05g,实验结果见表1。如图3所示列举了实施例2和对比例1-3的测定数据柱状图。
表1罗丹明B去除效果实验
从表1可知,本发明所制备的GO@Fe3O4-COOH@MIL-100(Fe)纳米复合材料对罗丹明B去除率可达97%以上,较Fe3O4-COOH、氧化石墨烯、Fe3O4-COOH@MIL-100(Fe)、GO@MIL-100(Fe)、氧化石墨烯和Fe3O4-COOH的复合物平均分别提高了318.1%、35.9%、10.5%、9%和13.2%以上,说明本发明复合材料具有良好的染料罗丹明B吸附能力,且氧化石墨烯可以提高Fe3O4-COOH@MIL-100(Fe)吸附罗丹明B的能力。
试验二
将本发明实施例2所得到的磁性颗粒复合物进行电镜扫描,得到如图1所示的扫描电镜图。
试验三
将本发明实施例2所得到的磁性颗粒复合物经过XRD测试得到如图2所示的图。
试验四
经过试验表明,本发明实施例1-3得到的磁性颗粒复合物具有很好的稳定性,在经过10次以上的重复使用,其去除罗丹明B的能力保持在85%以上。
最后应说明的是:以上各实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述各实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (6)
1.一种MIL-100(Fe)磁性纳米复合材料,其特征在于,其为氧化石墨烯、磁性物质和MIL-100(Fe)的复合物。
2.如权利要求1所述的MIL-100(Fe)磁性纳米复合材料,其特征在于:其为GO@Fe3O4-COOH@MIL-100(Fe)。
3.一种如权利要求1所述的MIL-100(Fe)磁性纳米复合材料的制备方法,其特征在于,其包括以下步骤:将氧化石墨烯、Fe3O4-COOH、硝酸铁、均苯三甲酸和硝酸溶解于水中得到的混合液,超声处理30~60min后,于110~130℃下加热12~24小时得到粉末。
4.如权利要求3所述的MIL-100(Fe)磁性纳米复合材料的制备方法,其特征在于,其还包括以下步骤:将粉末用水和无水乙醇分别洗涤两次,每次洗涤时间为30~60min;洗涤后放置于80~100℃中真空干燥8~10小时,研磨得到所述MIL-100(Fe)磁性纳米复合材料。
5.如权利要求3所述的MIL-100(Fe)磁性纳米复合材料的制备方法,其特征在于:所述混合液中氧化石墨烯的质量分数为2~6wt%。
6.如权利要求3所述的MIL-100(Fe)磁性纳米复合材料的制备方法,其特征在于:所述混合液中各组分按摩尔份分别为Fe3O4-COOH为0.001~0.002份、硝酸铁为0.003~0.005份、均苯三甲酸0.002~0.004份、所述硝酸浓度为0.006~0.015份。
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