CN107008336B - 一种光催化材料SnO2@Fe2O3的制备及应用 - Google Patents
一种光催化材料SnO2@Fe2O3的制备及应用 Download PDFInfo
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Abstract
本发明提供一种利用氧化还原机理制备SnO2@Fe2O3纳米光催化复合材料的方法,包括:将纳米SnO2分散于液相介质中,得SnO2分散液;在还原剂存在的条件下,使SnO2分散液中纳米SnO2表面的Sn(IV)还原为锡的低氧化态,得SnO2还原液;将上述的SnO2还原液与Fe2O3溶液混合均匀,充分反应,分离产物,即得SnO2@Fe2O3纳米光催化复合材料。该方法操作简单,时间短,成本低,环境友好,重复性好,效率高,能快速有效的制备纳米光催化复合材料,具有普适性和规模生产价值。本发明制备的纳米光催化复合材料SnO2@Fe2O3具有良好的紫外‑可见吸收范围,大大提高了光催化降解效率,在治理水污染、处理有机废物领域具有广阔的应用前景。
Description
技术领域
本发明属于纳米光催化复合材料制备技术领域,特别涉及新型光催化材料SnO2@Fe2O3的制备及应用。
背景技术
如今,生活污水,工业废水农药废水等严重危害了人们的生活,甚至生命安全,但是传统污水处理方法只能通过过滤技术去除污水中的难溶物,砂子等污染物,然而对于可溶性有机废物的处理效率低且成本高,甚至达到无法处理的地步。光催化技术是利用太阳光的照射,将光能转化为化学能,促使大部分有机物与部分无机物转化为水和二氧化碳等小分子物质,进而达到净化环境的目的。它是一种高效,环保,节能的新技术。而当催化剂的粒径为纳米数量级时,它会显现出更优异的光催化性能,其大的比表面积会提高催化反应的速度。
然而现有的光催化复合材料在制备步骤中存在着繁琐、稳定性差、催化降解效率低等一系列问题。
SnO2具有可见光透光性好,电阻率低,化学性能稳定以及室温下抗酸碱能力强等优点,因此其可作为光催化材料。但纯态光催化材料在光催化方面很难满足所有要求,为了提高光催化活性和效率必须设计合成新型光催化剂。SnO2@Fe2O3纳米光催化复合材料在UV-VIS 范围具有优良的光催化活性,且表现出特定的显微结构,是一种潜在的新型高效光催化材料。
发明内容
为了克服上述不足,本发明采用一种界面氧化还原原位生长方法,该方法操作简单、时间短、成本低、环境友好、重复性好、效率高,具有普适性和规模化生产价值。
为了实现上述目的,本发明采用如下技术方案:
一种利用氧化还原机理制备SnO2@Fe2O3纳米光催化复合材料的方法,包括:
将纳米SnO2分散于液相介质中,得SnO2分散液;
在还原剂存在的条件下,使SnO2分散液中纳米SnO2表面的Sn(IV)还原为锡的低氧化态,得SnO2还原液;
将上述的SnO2还原液与Fe2O3溶液混合均匀,充分反应,分离产物,即得SnO2@Fe2O3纳米光催化复合材料。
优选的,所述液相介质为水或有机溶剂。
优选的,所述还原剂为能还原Sn(IV)的所有还原剂。
优选的,所述锡的低氧化态为0或+2价。
优选的,所述SnO2还原液与Fe2O3溶液在振荡、超声或搅拌条件下发生氧化还原反应。
优选的,所述纳米SnO2、Fe2O3的摩尔比为1:x(x=0.01~1)。
优选的,所述SnO2分散液的浓度为0.1~100mg/mL,
优选的,所述Fe2O3的浓度为0.1~100mg/mL。
优选的,所述分离产物的方法为离心、过滤、沉降或溶剂蒸发。
本发明还提供了任一上述的方法制备的SnO2@Fe2O3纳米光催化复合材料,所述SnO2@Fe2O3纳米光催化复合材料的粒径为至少有一维为1~100nm。
本发明还提供了上述催化剂复合材料在光催化处理生活污水,工业废水或农药废水中应用。
本发明的有益效果
(1)本申请的方法操作简单,时间短,成本低,环境友好,重复性好,效率高,能快速有效的制备纳米光催化复合材料,具有普适性和规模生产价值。
(2)二氧化锡的禁带宽度为3.5eV,吸收光均在紫外光区,而三氧化二铁的禁带宽度为2.2eV吸收光在可见光区。本发明制备的纳米光催化复合材料SnO2@Fe2O3拓宽了光谱吸收范围,具有良好的紫外-可见吸收,大大提高了光催化降解效率,有利于在治理水污染、处理有机废物领域的应用。
(3)本发明制备方法简单、处理效率高、实用性强,易于推广。
附图说明
构成本申请的一部分的说明书附图用来提供对本申请的进一步理解,本申请的示意性实施例及其说明用于解释本申请,并不构成对本申请的不当限定。
图1为SnO2@Fe2O3纳米光催化复合材料的X-射线衍射谱图。
图2为SnO2@Fe2O3纳米光催化复合材料的透射电镜图(图中比例尺为50nm)。
图3A为SnO2纳米材料的光降解亚甲基蓝紫外吸收图,B为SnO2@Fe2O3纳米光催化复合材料的光降解亚甲基蓝紫外吸收图(太阳光连续照射5h)。
图4测定纳米材料及其复合材料溶液在不同时间下的吸光度,将其与初始时刻溶液吸光度对比,获得亚甲基蓝的浓度与时间变化图。
具体实施方式
应该指出,以下详细说明都是例示性的,旨在对本申请提供进一步的说明。除非另有指明,本文使用的所有技术和科学术语具有与本申请所属技术领域的普通技术人员通常理解的相同含义。
除了纳米光催化复合材料制备存在差异,其应用方面光催化降解亚甲基蓝条件完全一致。
一种利用界面氧化还原原理制备纳米光催化复合材料SnO2@Fe2O3的方法,包括如下步骤:
1)将纳米材料分散在适宜的溶剂中,进行超声分散处理;
2)向上述分散好的溶液中加入还原剂,振荡、搅拌或超声使反应物表面高氧化态得到充分还原为宜;
3)向还原后溶液中加入含有纳米级Fe2O3的溶液,进行振荡、搅拌或超声使反应充分进行,然后将反应物进行离心分离、洗涤、干燥,即得SnO2@Fe2O3纳米光催化复合材料。
优选的是,步骤(1)中所述的纳米材料为SnO2纳米半导体材料,二氧化锡具有多种结构,从零维度的纳米颗粒,一维的纳米线、纳米棒、纳米带、纳米管,到三维的纳米球、纳米立方体等等。纳米材料不同的形状会产生不同性能和作用。
优选的是,步骤(2)中所述还原剂为能够还原Sn(IV)的任意还原剂。
本发明的原理为,所述纳米材料表面Sn一般是以+4氧化态形式存在,被适当的还原剂还原可将Sn(IV)还原为锡的低氧化态(+2、0),反应式为:
Sn4++2e-=Sn2+
Sn2++2e-=Sn
然后加入Fe2O3,Fe2O3中Fe(III)具有氧化性,将低价态的Sn氧化为稳定的Sn(IV)时Fe3+被还原为Fe2+。
在氧化还原位点处Fe2O3原位生长在纳米材料SnO2表面形成稳定的SnO2@Fe2O3异质结复合材料,如图2的电镜照片可以看出,异质结复合材料结合的比较紧密,有效的将双功能材料集于一体。
实施例1:
(1)将SnO2纳米颗粒分散在乙醇溶液中配成0.1mg/mL溶液。
(2)将步骤(1)分散后的溶液取4mL在超声功率50W下超声10min,加入8滴制备好的钠汞齐振荡10min。
(3)将步骤(2)溶液中钠汞齐移出,加入4滴2mg/mLFe2O3溶液于还原后的乙醇溶液中,超声8min,超声功率为50W。离心分离即得SnO2@Fe2O3纳米光催化复合材料,分散在乙醇中的TEM如图2所示,纳米材料的XRD分析如图1所示。
(4)将制备的SnO2纳米颗粒、SnO2@Fe2O3复合材料取2mg各自溶解在20mL亚甲基蓝(10mg/L)溶液中;
(5)将溶液在暗处振荡10min,使得光催化剂-污染物分子在水溶液中达到吸附-解吸平衡;
(6)将上述溶液在200W氙灯下照射,每隔1h时间,离心取上层清液3mL用紫外-可见分光光度计测量吸光度,不同时间下的吸光度曲线如图3A、3B所示。测定溶液在不同时间下的吸光度,将其与初始时刻溶液吸光度对比,获得亚甲基蓝的浓度与时间变化如图4所示。结果显示,5小时后纯态SnO2对亚甲基蓝的降解率为40%,SnO2@Fe2O3异质结光催化材料对亚甲基蓝的降解率达到60%。
上述(1)中SnO2纳米颗粒购于阿拉丁试剂公司。
实施例2:
(1)取SnO2纳米颗粒分散在乙醇溶液中配成0.1mg/mL溶液。
(2)将步骤(1)分散后的溶液取4mL在超声功率50W下超声8min,加入6滴4mg/ml 硼氢化钠溶液,振荡10min。
(3)将步骤(2)所得到的溶液离心分离,倒去上清液,然后加入4ml乙醇重新超声分散,再向其中加入4滴2mg/mLFe2O3溶液,超声反应。超声10min,超声功率为100W。过滤分离即得SnO2@Fe2O3纳米光催化复合材料。表明,SnO2@Fe2O3纳米光催化复合材料在不同超声功率和时间下能够稳定合成,为光催化降解有机物提供了原料。
(5)将SnO2纳米颗粒、SnO2@Fe2O3复合材料取2mg各自溶解在20mL亚甲基蓝 (10mg/L)溶液中;
(6)将溶液在暗处振荡10min,使得光催化剂-污染物分子在水溶液中达到吸附-解吸平衡;
(7)将上述溶液在200W氙灯下照射,每隔1h时间,离心取上层清液3mL用紫外-可见分光光度计测量吸光度,获得不同时间下的吸光度曲线。测定溶液在不同时间下的吸光度,将其与初始时刻溶液吸光度对比,获得亚甲基蓝的浓度与时间变化。结果显示,5小时后纯态 SnO2对亚甲基蓝的降解率为35%,SnO2@Fe2O3异质结光催化材料对亚甲基蓝的降解率达到 55%。
实施例3:
(1)取SnO2纳米颗粒分散在乙醇溶液中配成0.1mg/mL溶液。
(2)将步骤(1)分散后的溶液取4mL在超声功率50W下超声8min,加入8滴制备好的钠汞齐振荡10min。
(3)将步骤(2)溶液中钠汞齐移出,加入4滴2mg/mLFe2O3溶液于还原后的乙醇溶液中,超声10min,超声功率为50W。蒸发溶剂即得SnO2@Fe2O3纳米光催化复合材料。表明,SnO2@Fe2O3纳米光催化复合材料在不同超声功率和时间下,均能够稳定合成,为光催化降解有机物提供了原料。
(5)将SnO2纳米颗粒、SnO2@Fe2O3复合材料取2mg各自溶解在20mL亚甲基蓝 (10mg/L)溶液中;
(6)将溶液在暗处振荡10min,使得光催化剂-污染物分子在水溶液中达到吸附-解吸平衡;
(7)将上述溶液在200W氙灯下照射,每隔1h时间,离心取上层清液3mL用紫外-可见分光光度计测量吸光度,获得不同时间下的吸光度曲线。测定溶液在不同时间下的吸光度,将其与初始时刻溶液吸光度对比,获得亚甲基蓝的浓度与时间变化。结果显示,5小时后纯态 SnO2对亚甲基蓝的降解率为30%,SnO2@Fe2O3异质结光催化材料对亚甲基蓝的降解率达到 47%。
实施例4:
(1)将SnO2纳米带分散在乙醇溶液中配成0.1mg/mL溶液。
(2)将步骤(1)分散后的溶液取4mL在超声功率50W下超声10min,加入6滴4mg/ml硼氢化钠溶液,振荡10min。
(3)将步骤(2)所得到的溶液离心分离,倒去上清液,然后加入4ml乙醇重新超声分散,再向其中加入4滴2mg/mLFe2O3溶液,超声反应。超声5min,超声功率为100W。即得 SnO2@Fe2O3纳米光催化复合材料。表明,在不同超声功率和时间下,不同还原剂,不同形貌 SnO2利用该氧化还原方法均可稳定合成SnO2@Fe2O3纳米光催化复合材料。
(5)将SnO2纳米带、SnO2@Fe2O3复合材料分别取2mg各自溶解在20mL亚甲基蓝(10mg/L)溶液中;
(6)将溶液在暗处振荡10min,使得光催化剂-污染物分子在水溶液中达到吸附-解吸平衡;
(7)将上述溶液在200W氙灯下照射,每隔1h时间,离心取上层清液3mL用紫外-可见分光光度计测量吸光度。结果显示,5小时后纯态SnO2对亚甲基蓝的降解率为28%, SnO2@Fe2O3异质结光催化材料对亚甲基蓝的降解率达到45%。
以上所述仅为本申请的优选实施例而已,并不用于限制本申请,对于本领域的技术人员来说,本申请可以有各种更改和变化。凡在本申请的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本申请的保护范围之内。
Claims (8)
1.一种利用界面氧化还原原位生长法制备SnO2@Fe2O3纳米光催化复合材料的方法,其特征在于,包括:
将纳米SnO2分散于液相介质中,得SnO2分散液;
在还原剂存在的条件下,使SnO2分散液中纳米SnO2表面的正四价的Sn还原为锡的低氧化态,得SnO2还原液;
将所述的SnO2还原液与Fe2O3溶液混合均匀,充分反应,分离产物,即得SnO2@Fe2O3纳米光催化复合材料;
所述纳米SnO2、Fe2O3的摩尔比为1:0.01 ~ 1。
2.如权利要求1所述的一种利用界面氧化还原原位生长法制备SnO2@Fe2O3纳米光催化复合材料的方法,其特征在于,所述液相介质为水或有机溶剂。
3.如权利要求1所述的一种利用界面氧化还原原位生长法制备SnO2@Fe2O3纳米光催化复合材料的方法,其特征在于,所述还原剂为能还原正四价的Sn的所有还原剂。
4.如权利要求1所述的一种利用界面氧化还原原位生长法制备SnO2@Fe2O3纳米光催化复合材料的方法,其特征在于,所述锡的低氧化态为0或+2价。
5.如权利要求1所述的一种利用界面氧化还原原位生长法制备SnO2@Fe2O3纳米光催化复合材料的方法,其特征在于,所述SnO2还原液与Fe2O3溶液在振荡、超声或搅拌条件下发生氧化还原反应。
6.如权利要求1所述的一种利用界面氧化还原原位生长法制备SnO2@Fe2O3纳米光催化复合材料的方法,其特征在于,所述SnO2分散液的浓度为0.1~100mg/mL。
7.如权利要求1所述的一种利用界面氧化还原原位生长法制备SnO2@Fe2O3纳米光催化复合材料的方法,其特征在于,所述Fe2O3溶液的浓度为0.1~100mg/mL。
8.如权利要求1所述的一种利用界面氧化还原原位生长法制备SnO2@Fe2O3纳米光催化复合材料的方法,其特征在于,所述分离产物的方法为离心、过滤、沉降或溶剂蒸发。
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