CN114538524A - 一种四氧化三铁八面体纳米晶的制备方法及应用 - Google Patents
一种四氧化三铁八面体纳米晶的制备方法及应用 Download PDFInfo
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Abstract
一种四氧化三铁八面体纳米晶的制备方法及应用，涉及溶剂热反应和界面反应技术领域，向乙二醇中加入一定量的铁盐，搅拌混合后再加入一定量的碳酸盐，继续搅拌后得到胶状前驱体；转入反应釜中通过溶剂热反应，最后经过滤分离、洗涤干燥从而获得四氧化三铁八面体纳米晶。本发明仅以铁盐、乙二醇和碳酸盐为主要原料，采用溶剂热法成功制备出了高稳定性高化学活性的Fe3O4八面体纳米晶。同时，本发明提供了对Mn(VII)的痕量检测及大容量去除，并得到MnFe2O4产物，且去除Mn(VII)具有不可逆性。可望用于饮用水中Mn(VII)痕量检测和工业废水中Mn(VII)大容量去除等领域。
Description
技术领域
本发明涉及溶剂热反应和界面反应技术领域，具体是涉及一种四氧化三铁八面体纳米晶的制备方法及应用。
背景技术
四氧化三铁(Fe3O4)纳米晶(1～100nm)是一种常见的环境友好磁性材料，在磁流体、微波吸收、催化剂载体、高级催化氧化、生物医药和重金属离子分离等领域应用广泛。众所周知，Fe3O4纳米晶尺寸越小，其比表面积越大，吸附性能就越好。然而，当Fe3O4尺寸减小到30nm左右时，其物理和化学性都将发生突变：可由亚铁磁性转变为超顺磁性，磁性减弱，不利于磁分离操作；同时，自身易发生氧化，导致其去除污染物具有不可逆性，易发生“二次”污染。
因此，如何解决纳米尺度Fe3O4自身非稳定性和吸附性之间的矛盾是一个值得研究的课题。Fe3O4为面心立方结构，容易制备出具有磁各向异性的Fe3O4八面体晶体。然而，已报道的Fe3O4八面体晶体的尺寸多为100nm以上，其稳定性和磁性能虽然都很高，但其表面活性较低，实际应用前景不好。
发明内容
本发明针对已有Fe3O4制备技术中所存在的不足之处，以乙二醇为还原剂，碳酸盐提供的OH-为结构和形态控制剂，在乙二醇体系中制备出八面体Fe3O4磁性四氧化三铁纳米粉体。此方法具有操作简单、成本低廉、获得产物的结构和形态可控等优点，为制备磁性八面体氧化铁纳米材料提供了一种简易、反应时间短、环保和可控的方法。在经过机械搅拌刻蚀法，进行其对Mn(VII)的痕量检测或去除，并得到MnFe2O4产物。此方法具有操作简单、成本低廉、方式新颖等优点。
为了实现上述目的，本发明所采用的技术方案为：
一种四氧化三铁八面体纳米晶的制备方法，其特征在于，包括如下步骤：
①、向乙二醇中加入一定量的铁盐，搅拌混合后再加入一定量的碳酸盐，继续搅拌后得到胶状前驱体；
②、将上述胶状前驱体转入反应釜中，通过溶剂热反应，最后经过滤分离、洗涤干燥从而获得四氧化三铁八面体纳米晶。
作为本发明制备方法的优选技术方案：
步骤①中向50mL乙二醇中加入1.2～2.7g的铁盐，搅拌混合后再加入1～3g的碳酸盐。
所述铁盐选自氯化铁、硝酸铁或者硫酸铁。
所述碳酸盐选自碳酸钠或者碳酸钾。
所述胶状前驱体的pH值为7～10。
步骤②中溶剂热反应温度为140～160℃，反应时间为12～24h。
本发明仅以铁盐、乙二醇和碳酸盐为主要原料，采用溶剂热法成功制备出了高稳定性高化学活性的Fe3O4八面体纳米晶。初步研究表明，该Fe3O4八面体纳米晶能高效去除水体中Mn(VII)特性。此方法具有使用原料少，成本低，环境友好以及获得的产物结构和形态可控等特点，可用于水体中Mn(VII)的大容量去除和痕量检测。
与现有技术相比，本发明的有益效果表现在：
1.本发明实现了八面体Fe3O4纳米晶一步法合成，为八面体磁性纳米材料的制备提供了一种新的方法，同时提供了对Mn(VII)的痕量检测及大容量去除，并得到MnFe2O4产物，且去除Mn(VII)具有不可逆性。可望用于饮用水中Mn(VII)痕量检测和工业废水中Mn(VII)大容量去除等领域。
2.本发明方法具有操作简单、成本低廉，且获得的产物结构和形态可控等优点。
附图说明
图1a和b分别对应实施例1制备产物的SEM图和XRD图。
图2a和b分别对应实施例2反应生成产物的EDS图和反应过程示意图。
具体实施方式
下面结合附图和具体实施例对本发明进行详细说明。
本发明方法所得产物的结构和形态分别采用X射线粉末衍射(XRD,D3500)和场发射扫描电子显微镜(FE-SEM,SU8010)等仪器来表征和分析。
实施例1：四氧化三铁八面体纳米晶制备
称取1.42g FeCl3.6H2O溶解于50mL乙二醇中，再加入2g碳酸钠粉末，经搅拌混合后，然后将其转入反应釜中，于150℃下反应18h，反应后取出产物进行洗涤干燥。
利用XRD和SEM手段分别对制备产物的结构和形态进行表征，其结果如图1所示。SEM观察表明(图1a)，所得产物形态为八面体，其平均粒径约为50～80nm。产物物相结果分析表明(图1b)，此条件下获得的产物为Fe3O4(XRD标准谱图：PDF#19-0629)。
Fe3O4八面体纳米晶的形成可看成以下四个过程：首先，FeCl3.6H2O、Na2CO3和乙二醇发生反应得到Fe(OH)3，然后Fe(OH)3和乙二醇反应得到Fe2O3·xH2O，之后Fe2O3·xH2O和OH-反应得到α-FeOOH，最后α-FeOOH和乙二醇反应得到八面体Fe3O4纳米晶。上述四个过程可以用式子(1)和(2)和(3)和(4)分别表示：
实施例2：去除水体中Mn(VII)的方法与机理
称取0.2g KMnO4稀释到500mL去离子水中，向上述溶液中再加入1g实施例1制备的Fe3O4八面体纳米晶，室温下经超声混合反应18h，反应结束后，反应溶液由紫红色变为透明(图2b)，说明溶液中的Mn(VII)与Fe3O4八面体纳米晶发生了界面还原反应。
将反应产物磁分离洗净后，利用EDS对其进行成分分析，结果表明，八面体表明的化学成分主要由Fe、Mn和O组成(图2a)，可以初步确定Mn(VII)与Fe3O4发生了界面反应生成了MnFe2O4产物，其过程可用式子(5)来表示。
因此，研究表明本发明获得的Fe3O4八面体纳米晶可以有效去除水体中Mn(VII)。此外，利用该实验现象和结果还可以对水体中痕量Mn(VII)进行检测分析，此方法操作简单、方便快捷、新颖有效。
以上内容仅仅是对本发明的构思所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明的构思或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。
Claims (8)
1.一种四氧化三铁八面体纳米晶的制备方法，其特征在于，包括如下步骤：
①、向乙二醇中加入一定量的铁盐，搅拌混合后再加入一定量的碳酸盐，继续搅拌后得到胶状前驱体；
②、将上述胶状前驱体转入反应釜中，通过溶剂热反应，最后经过滤分离、洗涤干燥从而获得四氧化三铁八面体纳米晶。
2.如权利要求1所述的制备方法，其特征在于，步骤①中向50mL乙二醇中加入1.2～2.7g的铁盐，搅拌混合后再加入1～3g的碳酸盐。
3.如权利要求1或2所述的制备方法，其特征在于，所述铁盐选自氯化铁、硝酸铁或者硫酸铁。
4.如权利要求1或2所述的制备方法，其特征在于，所述碳酸盐选自碳酸钠或者碳酸钾。
5.如权利要求1所述的制备方法，其特征在于，步骤②中溶剂热反应温度为140～160℃，反应时间为12～24h。
6.如权利要求1～5任一项所述方法制备的四氧化三铁八面体纳米晶，其特征在于，四氧化三铁纳米晶呈八面体形貌，平均粒径为50～80nm。
7.如权利要求6所述四氧化三铁八面体纳米晶在去除工业废水中Mn(VII)的应用。
8.如权利要求6所述四氧化三铁八面体纳米晶在痕量检测饮用水中Mn(VII)的应用。
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