CN107442139A - 用于高效降解龙胆紫的片状Z型SnS2/Bi2MoO6异质结光催化材料的制备方法 - Google Patents
用于高效降解龙胆紫的片状Z型SnS2/Bi2MoO6异质结光催化材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种用于高效降解龙胆紫的片状Z型SnS2/Bi2MoO6异质结光催化材料的制备方法,属于无机环保光催化材料的合成技术领域。本发明的技术方案要点为:用于高效降解龙胆紫的片状Z型SnS2/Bi2MoO6异质结光催化材料的制备方法,采用原位水热法使用微量的SnS2改良Bi2MoO6,两种半导体光催化剂复合形成新的片状Z型异质结,该种异质结有效促进光生电子空穴对的分离,从而显著提高异质结光催化材料的光催化活性。
Description
技术领域
本发明属于无机环保光催化材料的合成技术领域,具体涉及一种用于高效降解龙胆紫的片状Z型SnS2/Bi2MoO6异质结光催化材料的制备方法。
背景技术
随着工业的快速发展,各种有毒有害污染物不断进入人们的生活危害人类健康,利用太阳光降解有毒有害污染物变得越来越有意义,因此研制具有可见光催化活性的纳米材料成为环保领域研究的热点和焦点。
Bi2MoO6作为一种典型的奥里维里斯铋系半导体材料,在其相结构中,[O]2 -层把[Bi2O2]2+和[MoO4]2−紧密的连接在一起,是一种典型的二维层状材料。Bi2MoO6与Bi2WO6类似,但Bi2MoO6禁带宽度较窄,能更好地利用可见光,其催化效果也广泛应用在选择性催化丙烯、丁醇、石蜡等方面。但是单一的Bi2MoO6存在较多的缺陷,如量子产率较低、电荷分离和转移率较低、活性位点较少等。
SnS2是一种典型的CdI2型硫化物,正六边形薄片状结构,禁带宽度约1.91-2.35eV,合成成本低、无毒性、稳定性好、吸附性及可见光响应能力较强,因此备受人们关注,但光生电子和空穴易复合。
综上所述,利用上述两种材料的优点,采用原位水热法使用微量的SnS2改良Bi2MoO6,将两种半导体复合形成新型片状Z型异质结,该种异质结有较大的比表面积,减少电荷转移的距离和时间,有效促进光生电子空穴对的分离,从而显著地提高光催化活性。迄今为止,作为研究热点的Z型光催化剂已经由于较强的氧化还原能力及光生电荷分离后形成的空间优势被广泛用于研究污染物降解。目前,尚没有关于合成片状Z型SnS2/Bi2MoO6异质结光催化材料来提高光催化性能的相关报道。
发明内容
本发明解决的技术问题是提供了一种用于在太阳光照射下高效降解龙胆紫的片状Z型SnS2/Bi2MoO6异质结光催化材料的制备方法,该方法制得的SnS2/Bi2MoO6异质结光催化材料有效解决了光生载流子难分离的问题。
本发明为解决上述技术问题采用如下技术方案,用于高效降解龙胆紫的片状Z型SnS2/Bi2MoO6异质结光催化材料的制备方法,其特征在于具体步骤为:
(1)SnS2纳米片的制备
将SnCl4 .5H2O和硫脲溶解于去离子水中得到溶液A,再将溶液A转入反应釜中于180℃反应10h,然后自然冷却至室温,离心分离,用去离子水和无水乙醇洗涤多次后干燥得到SnS2纳米片待用;
(2)片状Z型SnS2/Bi2MoO6异质结光催化材料的制备
按照质量比m(SnS2):m(Bi2MoO6)=3-7:100的化学计量比分别称取SnS2纳米片、Bi(NO3)3 .5H2O和钼酸铵,将SnS2纳米片分散于无水乙醇中得到溶液B,将Bi(NO3)3 .5H2O溶解于硝酸溶液中得到溶液C,将钼酸铵溶解于去离子水中得到溶液D,再将溶液D加入到溶液C中并调节pH值为7-8得到溶液E,将溶液B加入到溶液E中并调节pH值为7-8得到溶液F,将溶液F转入反应釜中于160℃反应6h,冷却后将所得沉淀离心分离,洗涤,干燥即得到片状Z型SnS2/Bi2MoO6异质结光催化材料,该SnS2/Bi2MoO6异质结光催化材料是由平均直径为0.5μm的六边形纳米片及原位生长于其上的SnS2纳米片组成的平均长度为1.5μm、平均厚度为150nm的片状Z型异质结光催化材料。
进一步优选,步骤(1)中SnCl4 .5H2O与硫脲的质量比为0.7:1。
进一步优选,步骤(2)中硝酸溶液的摩尔浓度为2mol/L。
进一步优选,步骤(2)中SnS2与Bi2MoO6的化学计量比优选为m(SnS2):m(Bi2MoO6)=5:100。
本发明仅采用水热法合成片状Z型SnS2/Bi2MoO6异质结光催化材料,其具有较大的比表面积,能够有效利用可见光,形成异质结利于光生电子空穴更好的分离,模拟太阳光条件下降解染料龙胆紫表现出优异的光催化性能。本发明所使用的原料廉价易得,合成过程绿色环保,反应条件较为温和,适合规模化生产,有望产生良好的社会和经济效益。
附图说明
图1是实施例1制得的SnS2/Bi2MoO6异质结光催化材料的FESEM图;
图2是实施例1制得的SnS2/Bi2MoO6异质结光催化材料的HRTEM图;
图3是不同光催化材料在模拟太阳光照射下对龙胆紫的降解效率对比图;
图4是加入不同捕获剂后实施例1制得的SnS2/Bi2MoO6异质结光催化材料光催化降解龙胆紫的效果曲图;
图5是纯Bi2MoO6、纯SnS2和实施例1制得的Bi2MoO6/SnS2异质结光催化材料的XRD图谱;
图6是纯Bi2MoO6、纯SnS2和实施例1制得的Bi2MoO6/SnS2异质结光催化材料的UV-VisDRS图谱。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明,但不应该将此理解为本发明上述主题的范围仅限于以下的实施例,凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
(1)SnS2纳米片的合成
称取2.1g SnCl4 .5H2O和3g硫脲溶解到70mL水中,超声20min得到溶液A,将溶液A转移到反应釜(内衬为聚四氟乙烯)中,密封、置于烘箱中加热至180℃维持10h,反应釜在烘箱中自然冷却至室温后,离心分离得到沉淀,并用无水乙醇和去离子水洗涤数次,再于60℃真空烘干得到黄色粉末状SnS2纳米片;
(2)SnS2/Bi2MoO6异质结光催化材料的合成
分别称取一定量上述所制SnS2纳米片于30mL无水乙醇中超声分散20min得到溶液B,使质量比SnS2/Bi2MoO6分别为3wt%、5wt%和7wt%,称取2.2508g Bi(NO3)3·5H2O于25mL摩尔浓度为2mol/L的硝酸溶液中并搅拌至完全溶解得到溶液C,称取0.4096g (NH4)6Mo7O24·4H2O于10mL去离子水中溶解得到溶液D,将溶液D逐滴加入到溶液C中并用氨水调节pH=7.0,磁力搅拌30min得到溶液E,将溶液A逐滴加入到溶液E中并调节pH=7.0,搅拌30min得到溶液F,将溶液F转入反应釜中于160℃反应6h,将沉淀用水和无水乙醇洗涤3次,并于60℃干燥过夜得到SnS2/Bi2MoO6异质结光催化材料。
光催化活性评价:在PCX50B多通道光催化反应系统中进行,该反应仪放有旋片式5W光源1组(共9个)的LED灯作为光源,旋片式光源的特性是不同LED灯单位切换间隔可调,本实验均调为30s,反应瓶搅拌为磁力悬浮,外通冷却系统。在光催化反应系统中,龙胆紫模拟废水的初始浓度为20mg/L,溶液体积为50mL,催化剂用量为50mg。在光催化反应前,将含光催化剂的龙胆紫悬浮液超声分散5min,然后将石英反应瓶放入光催化反应系统中。仅开搅拌装置,在黑暗条件下搅拌吸附40min达到物理吸附和脱附平衡, 然后先开冷却系统再打开光源和旋片装置,每20min取一次样,所取样品体积约为3mL。将所取的样品溶液于10000r/min离心分离10min,取其上清液,用紫外分光光度计测上清液中的浓度,通过C/C0来判断龙胆紫的降解效果。其中,C0为吸附平衡后龙胆紫的浓度,C为反应时间为t时龙胆紫的浓度。
图1是本实施例制得的SnS2/Bi2MoO6异质结光催化材料的FESEM图,由图可以看出样品是由片状SnS2生长在片状Bi2MoO6上形成异质结,其中SnS2为自组装形成的直径约0.5μm的六边形薄纳米片,Bi2MoO6为表面光滑的无规则纳米片,长度一般在1.5μm,平均厚度约150nm左右;SnS2/Bi2MoO6异质结表面变得粗糙,且少量SnS2掺杂进Bi2MoO6后形貌发生改变,Bi2MoO6仍保持片状Bi2MoO6的形貌。
图2是本实例制得的SnS2/Bi2MoO6异质结光催化材料的HRTEM图,由图可以看出样品结晶良好,能观察到在Bi2MoO6表面原位生长出的片状SnS2晶格条纹,能观察到两种不同的晶格条纹,间距分别为0.315nm和0.223nm、0.27nm,分别对应SnS2的(100)晶面和Bi2MoO6的(132)和(200)晶面,并且能清晰观察到两种物质的边界,SnS2受Bi2MoO6影响形貌发生改变。表明SnS2与Bi2MoO6纳米片之间形成异质结构。
图3是模拟太阳光照射下不同质量比光催化剂对龙胆紫的降解效率对比图,由图可以看出,在没有光催化剂存在下,光照120min后龙胆紫几乎没有降解,表明龙胆紫分子具有很好的光稳定性。SnS2/Bi2MoO6机械混合样品和SnS2/Bi2MoO6异质结光催化材料与纯相比呈现增强的光降解活性,但是异质结光催化材料对龙胆紫的降解与物理混合材料和纯的Bi2MoO6、SnS2相比光催化效率明显提高,且5wt% SnS2/Bi2MoO6异质结光催化材料效果最好,在可见光下照射120min对龙胆紫的降解率达到了82%左右。
图4为加入不同捕获剂后SnS2/Bi2MoO6异质结光催化材料模拟太阳光降解龙胆紫效果曲图,从图中可以看出,在加入不同的捕获剂后,复合光催化剂对龙胆紫的光降解性能有所不同,其中,加入EDTA-2Na和异丙醇后模拟太阳光照射120min龙胆紫红几乎没有降解,而加入苯醌后,与不加捕获剂相比光催化性能稍有改变。表明本申请所制备的复合光催化剂在光催化降解龙胆紫的过程中,空穴与羟基自由基是主要的活性物种,而超氧自由基起辅助作用。
图5是纯SnS2、纯Bi2MoO6和制得的SnS2/Bi2MoO6片状光催化材料的XRD图谱,图中纯SnS2和纯Bi2MoO6各衍射峰位置分别与四方相SnS2(JCPDS 83-1705)和正交相Bi2MoO6(JCPDS71-2086)对应。从图中可以看出,2θ角在10.9o、28.3o、32.6o、47.2o和55.6o分别对应Bi2MoO6的(020)、(131)、(200)、(260)和(331)晶面的衍射峰,掺入少量的SnS2后,衍射峰没有发生明显的变化,但是随着SnS2投加量的增加,复合物受到SnS2在32.2o出现(001)面的影响,2θ角在32.6o对应的衍射峰强度明显增强,说明已有SnS2存在于Bi2MoO6中形成复合物。
图6为纯SnS2、纯Bi2MoO6和制得的5wt% SnS2/Bi2MoO6异质结光催化材料的UV-VisDRS图谱,由图可知纯SnS2几乎对整个可见光范围都有吸收,纯Bi2MoO6的吸收边缘为470nm左右,少量SnS2纳米片掺杂后,与纯的Bi2MoO6相比复合光催化材料的吸收边显著红移,且明显在可见光范围有吸收,说明SnS2可作为Bi2MoO6的感光剂。
以上实施例描述了本发明的基本原理、主要特征及优点,本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明原理的范围下,本发明还会有各种变化和改进,这些变化和改进均落入本发明保护的范围内。
Claims (4)
1.用于高效降解龙胆紫的片状Z型SnS2/Bi2MoO6异质结光催化材料的制备方法,其特征在于具体步骤为:
(1)SnS2纳米片的制备
将SnCl4 .5H2O和硫脲溶解于去离子水中得到溶液A,再将溶液A转入反应釜中于180℃反应10h,然后自然冷却至室温,离心分离,用去离子水和无水乙醇洗涤多次后干燥得到SnS2纳米片待用;
(2)片状Z型SnS2/Bi2MoO6异质结光催化材料的制备
按照质量比m(SnS2):m(Bi2MoO6)=3-7:100的化学计量比分别称取SnS2纳米片、Bi(NO3)3 .5H2O和钼酸铵,将SnS2纳米片分散于无水乙醇中得到溶液B,将Bi(NO3)3 .5H2O溶解于硝酸溶液中得到溶液C,将钼酸铵溶解于去离子水中得到溶液D,再将溶液D加入到溶液C中并调节pH值为7-8得到溶液E,将溶液B加入到溶液E中并调节pH值为7-8得到溶液F,将溶液F转入反应釜中于160℃反应6h,冷却后将所得沉淀离心分离,洗涤,干燥即得到片状Z型SnS2/Bi2MoO6异质结光催化材料,该SnS2/Bi2MoO6异质结光催化材料是由平均直径为0.5μm的六边形纳米片及原位生长于其上的SnS2纳米片组成的平均长度为1.5μm、平均厚度为150nm的片状Z型异质结光催化材料。
2.根据权利要求1所述的用于高效降解龙胆紫的片状Z型SnS2/Bi2MoO6异质结光催化材料的制备方法,其特征在于:步骤(1)中SnCl4 .5H2O与硫脲的质量比为0.7:1。
3.根据权利要求1所述的用于高效降解龙胆紫的片状Z型SnS2/Bi2MoO6异质结光催化材料的制备方法,其特征在于:步骤(2)中硝酸溶液的摩尔浓度为2mol/L。
4.根据权利要求1所述的用于高效降解龙胆紫的片状Z型SnS2/Bi2MoO6异质结光催化材料的制备方法,其特征在于:步骤(2)中SnS2与Bi2MoO6的化学计量比优选为m(SnS2):m(Bi2MoO6)=5:100。
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