CN109126833A - 一种制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法 - Google Patents
一种制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法 Download PDFInfo
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Abstract
本发明公开了一种制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法,包括以下步骤:(1)将FeSO4.7H2O加入到去离子水中配成硫酸亚铁水溶液;(2)称取AgNO3加入到步骤(1)中所述的硫酸亚铁水溶液中,在常温常压下,通过快速还原反应得到Ag‑Fe2(SO4)3‑H2O反应体系;(3)再向步骤(2)中制得的Ag‑Fe2(SO4)3‑H2O反应体系中加入FeSO4.7H2O,在空气中快速搅拌反应多个小时后即得AgFe3(SO4)2(OH)6粉体。与现有技术相比,本发明的有益效果为:(1)实现了银铁矾可见光催化剂的简单合成,为铁矾的制备和应用开辟了新的领域。(2)本发明的方法具有实验操作简单、成本低廉,同时,获得的产物量大、产物可见光性能优异。
Description
技术领域
本发明涉及微纳米结构材料的制备技术领域,特别是一种制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法。
背景技术
光催化剂是指在光子的激发下能够起到催化作用的各类半导体材料。主要包括二氧化钛(TiO2)、氧化锌(ZnO)、氧化锡(SnO2)、二氧化锆(ZrO2)和硫化镉(CdS)等多种化合物半导体。光催化除污技术具有设备简单、操作条件易控制、非选择性的氧化有机污染物、运行费用低、无二次污染并且催化剂可回收利用等突出优点,在有机废水治理方面有着广阔的应用前景。光催化逐步向更高效利用日光,实用化方向发展,寻找能直接利用太阳光的催化剂是光催化领域的一个重要发展方向。
铁矾是指两种或两种以上金属的硫酸盐所组成的碱式硫酸盐的复盐,主要有:黄钾铁矾、草黄铁矾、黄铵铁矾、银铁矾、黄钠铁矾和铅铁矾六种,它们都是在酸性环境中形成的。铁矾一旦形成,就很稳定,不溶于酸,因此,铁矾的沉淀反应可用于从硫酸盐溶液中除铁。铁矾分子式可写成MFe3(SO4)2(OH)6,M+为一价阳离子(主要包括Na+、K+、NH4 +、Ag+、Rb+和0.5Pb2+等)。例如,钠铁矾[Na2Fe6(SO4)4(OH)12]、铅铁矾[Pb0.5Fe3(SO4)2(OH)6]和银铁矾[Ag2Fe6(OH)12(SO4)4]都是已知的铁矾。通常,铁矾可采用化学法和生物化学法来制备。铁矾本身一般具有解毒杀虫、敛疮等的功效,在医学领域应用广泛。同时,煅烧质量纯的铁矾可得到用于研磨的各类材料。
发明内容
本发明的目的是提供一种制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法,以解决现有技术中的不足,它能够在常温常压下成功得到了具有优异可见光催化性能的AgFe3(SO4)2(OH)6磁性催化剂,操作简单、成本低廉和环境友好。
本发明提供了一种制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法,包括以下步骤:
(1)将FeSO4.7H2O加入到去离子水中配成硫酸亚铁水溶液;
(2)称取AgNO3加入到步骤(1)中所述的硫酸亚铁水溶液中,在常温常压下,通过快速还原反应得到Ag-Fe2(SO4)3-H2O反应体系;
(3)再向步骤(2)中制得的Ag-Fe2(SO4)3-H2O反应体系中加入FeSO4.7H2O,在空气中快速搅拌反应多个小时后即得AgFe3(SO4)2(OH)6粉体。
优选的是,步骤(1)中所述硫酸亚铁水溶液的浓度为0.01-0.4mol/L。
优选的是,步骤(2)中所述AgNO3的质量为0.10-0.5g。
优选的是,步骤(3)中添加的FeSO4.7H2O的质量为1-3g。
优选的是,步骤(3)中在空气中快速搅拌的速率为100-200转/分钟。
优选的是,步骤(3)中在空气中快速搅拌反应时间超过12h。
与现有技术相比,本发明的有益效果为:(1)实现了银铁矾可见光催化剂的简单合成,为铁矾的制备和应用开辟了新的领域。(2)本发明的方法具有实验操作简单、成本低廉,同时,获得的产物量大、产物可见光性能优异。
附图说明
图1为实施例1中获得的产物的XRD谱图;
图2为实施例1中产物的形态和化学组成分析;
图3为实施例1中获得的产物的光学性能。
具体实施方式
下面通过参考附图描述的实施例是示例性的,仅用于解释本发明,而不能解释为对本发明的限制。
一种制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法,包括以下步骤:
(1)将FeSO4.7H2O加入到去离子水中配成硫酸亚铁水溶液;
(2)称取AgNO3加入到步骤(1)中所述的硫酸亚铁水溶液中,在常温常压下,通过快速还原反应得到Ag-Fe2(SO4)3-H2O反应体系;
(3)再向步骤(2)中制得的Ag-Fe2(SO4)3-H2O反应体系中加入FeSO4.7H2O,在空气中快速搅拌反应多个小时后即得AgFe3(SO4)2(OH)6粉体。
AgNO3、FeSO4.7H2O和Fe2(SO4)3以及空气中的O2之间具有相互配合、缺一不可的关系。
步骤(1)中所述硫酸亚铁水溶液的浓度为0.01-0.4mol/L。
步骤(2)中所述AgNO3的质量为0.10-0.5g。
步骤(3)中添加的FeSO4.7H2O的质量为1-3g。
步骤(3)中在空气中快速搅拌的速率为100-200转/分钟。
步骤(3)中在空气中快速搅拌反应时间超过12h。
本发明的实施例1:
取0.2g AgNO3加入到100mL浓度为0.2mol/L的FeSO4.7H2O水溶液中,反应30分钟后,再加入0.3g FeSO4.7H2O,超声溶液和反应若干时间后即可获得目标产物。首先,利用X-衍射手段对产物结构进行分析后表明,产物的XRD谱图与块体AgFe3(SO4)2(OH)6的标准XRD谱图(PDF#41-1398)对应完好(见图1),说明实验得到的粉体为菱方结构的AgFe3(SO4)2(OH)6。接着,采用SEM手段对产物的形态和化学组成进行了分析,其结果如图2所示。由图2a可以看出,产物的形态多为圆片状聚集体,尺寸较大。对单个圆片进行面扫描和线扫描能谱分析结果表明,单个圆片主要是由Ag、Fe、S和O四种元素构成(见图2b)。线扫描结果初步表明,Ag:Fe:S三者比例约为0.83:4.81:2.8,接近于1:3:2,也可以说明产物组成为AgFe3(SO4)2(OH)6(见图2c)。基于上述部分实验结果,可以认为AgFe3(SO4)2(OH)6的形成过程如下:首先,Ag+被Fe2+快速还原成Ag,之后Ag又被Fe3+缓慢氧化成Ag+,最后,在含有Ag+、Fe3+和高浓度的SO4 2-的酸性环境中形成了AgFe3(SO4)2(OH)6。反应过程可如下两个式子表示。
利用公式可以来计算AgFe3(SO4)2(OH)6光带隙,其中h为普朗克常量,是 光的频率,Eg为光带隙能量值,α为吸光度,n对于间接带隙型半导体取0.5, 对于直接带隙型半导体2。以(αhν)n为纵坐标,hν为横坐标作图,对其中线性 区段进行拟合,得到一个线性方程,它在x轴截距即是带隙能量的大小。
首先,测得了黄色AgFe3(SO4)2(OH)6粉体的紫外-可见吸收光谱图(见3a), 然后,利用上述方法得到(αhν)0.5-hν曲线(见3b),可以估算出AgFe3(SO4)2(OH)6粉体的带隙约为1.9eV。最后,将一定量粉体分散于水中,外加一定强度的磁 场,约10分钟后,分散的产物将完全富集到瓶壁上,说明实验产物具有良好 的磁性能。
以上依据图式所示的实施例详细说明了本发明的构造、特征及作用效果,以上所述仅为本发明的较佳实施例,但本发明不以图面所示限定实施范围,凡是依照本发明的构想所作的改变,或修改为等同变化的等效实施例,仍未超出说明书与图示所涵盖的精神时,均应在本发明的保护范围内。
Claims (6)
1.一种制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法,其特征在于:包括以下步骤:
(1)将FeSO4.7H2O加入到去离子水中配成硫酸亚铁水溶液;
(2)称取AgNO3加入到步骤(1)中所述的硫酸亚铁水溶液中,在常温常压下,通过快速还原反应得到Ag-Fe2(SO4)3-H2O反应体系;
(3)再向步骤(2)中制得的Ag-Fe2(SO4)3-H2O反应体系中加入FeSO4.7H2O,在空气中快速搅拌反应多个小时后即得AgFe3(SO4)2(OH)6粉体。
2.根据权利要求1所述的制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法,其特征在于:步骤(1)中所述硫酸亚铁水溶液的浓度为0.01-0.4mol/L。
3.根据权利要求1所述的制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法,其特征在于:步骤(2)中所述AgNO3的质量为0.10-0.5g。
4.根据权利要求1所述的制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法,其特征在于:步骤(3)中添加的FeSO4.7H2O的质量为1-3g。
5.根据权利要求1所述的制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法,其特征在于:步骤(3)中在空气中快速搅拌的速率为100-200转/分钟。
6.根据权利要求1所述的制备AgFe3(SO4)2(OH)6可见光磁性催化剂的方法,其特征在于:步骤(3)中在空气中快速搅拌反应时间超过12h。
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