CN107115893B - 一种硫化铟锡/方酸菁复合可见光催化剂的制备方法 - Google Patents
一种硫化铟锡/方酸菁复合可见光催化剂的制备方法 Download PDFInfo
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Abstract
本发明涉及一种硫化铟锡/方酸菁复合可见光催化剂的制备方法，包括步骤：硫化铟锡的制备、吲哚类方酸菁染料的合成和硫化铟锡/方酸菁染料复合光催化剂的制备。本发明的有益效果是：该制备方法较为简单，制备条件容易控制，所制备的硫化铟锡/方酸菁复合可见光催化剂为绿色环保高性能催化剂，无污染，催化效率高，具有一定的应用价值。
Description
技术领域
本发明属于光催化技术领域，涉及一种硫化铟锡/方酸菁复合可见光催化剂的制备方法。
背景技术
硫化铟锡是近期报道的具有可见光催化性能的三元硫化物半导体，其带隙为1.81eV，其价带电位为1.60eV，导带电位为-0.21eV。由于它的禁带宽度较窄，硫化铟锡在可见光区域内具有强烈的吸收，是具有广阔发展空间的新型光催化材料。然而光生电子空穴对很容易产生再结合，为了解决半导体材料共有的问题，我们用方酸菁染料敏化硫化铟锡，进一步增强它在可见光区域内的光吸收，提高光催化活性。
方酸菁染料作为一种特殊的有机功能型染料，由于分子中具有特殊的供体- 受体-供体(D-A-D)结构，所以方酸菁染料在可见-近红外区内拥有强烈的吸收性能，吸收波长在600nm左右。分子内的共轭结构大大提高了其光、热稳定性。另外方酸菁染料作为一种性能优异的近红外染料，也越来越多地被人们应用于光学记录、太阳能电池等光学领域。对称型吲哚类方酸菁示意如下：
本专利主要采用超声浸渍法敏化制备硫化铟锡/方酸菁的复合可见光催化剂。这种催化剂可应用于光催化技术中，可以快速有效地除去水中的有机污染物。
发明内容
本发明要解决的技术问题是：基于上述问题，本发明采用超声浸渍法敏化制备硫化铟锡/方酸菁复合可见光催化剂，这种催化剂可应用于光催化技术中，可以快速有效地除去水中的有机污染物
本发明解决其技术问题所采用的一个技术方案是：一种硫化铟锡/方酸菁复合可见光催化剂的制备方法，包括以下步骤：
(1)硫化铟锡的制备：将五水合四氯化锡、四水合三氯化铟溶于无水乙醇中，混合搅拌均匀，加入硫代乙酰胺，继续搅拌30min，转移至高压反应釜内， 160℃反应12小时，冷却，洗涤烘干；
(2)吲哚类方酸菁染料的合成：将N-2,3,3-三甲基吲哚和方酸加至三口烧瓶中，加入正丁醇和甲苯混合溶剂，连接好冷凝管和斯托克分水器，105～115℃加热回流10～12小时，冷却至室温，减压抽滤烘干，柱层析分离提纯；
(3)硫化铟锡/方酸菁染料复合光催化剂的制备：硫化铟锡和方酸菁分别加入乙醇，搅拌均匀后，方酸菁溶液逐滴滴加至硫化铟锡溶液中，搅拌12～14h，超声5～8h，抽滤洗涤烘干。
进一步地，步骤(1)中五水合四氯化锡、四水合三氯化铟、硫代乙酰胺和无水乙醇的摩尔比为1：4：8：1370，无水乙醇的密度为0.789g/cm3。
进一步地，步骤(2)中N-2,3,3-三甲基吲哚和方酸的摩尔比为2：1，正丁醇和甲苯的体积比为1：1～1：3。
进一步地，步骤(3)中方酸菁是硫化铟锡质量的10～50％。
本发明的有益效果是：该制备方法较为简单，制备条件容易控制，所制备的硫化铟锡/方酸菁复合可见光催化剂为绿色环保高性能催化剂，无污染，催化效率高，具有一定的应用价值。
附图说明
下面结合附图对本发明进一步说明。
图1是本发明实施例1制备得到的硫化铟锡的扫描电镜图；
图2是本发明实施例1制备得到的硫化铟锡/方酸菁复合可见光催化剂的扫描电镜图；
图3是本发明实施例1制备得到的硫化铟锡/方酸菁复合可见光催化剂的X 射线衍射图；
图4是本发明实施例1制备得到的硫化铟锡/方酸菁复合可见光催化剂光降解孔雀石绿的紫外可见吸收光谱随光照时间变化图。
具体实施方式
现在结合具体实施例对本发明作进一步说明，以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例1
(1)硫化铟锡的制备：称取0.4207g的五水合四氯化锡和1.4088g四水合三氯化铟，将它们溶解于96mL无水乙醇溶液中，搅拌至溶液澄清透明后，加入0.7212g硫代乙酰胺持续搅拌30min后转移入高压反应釜，在160℃的条件下反应12h，冷却洗涤烘干。
(2)对称型吲哚类方酸菁染料的合成：称取0.145g N-2,3,3-三甲基吲哚和0.052g方酸至三口烧瓶中，加入体积为20mL正丁醇和20mL甲苯混合溶剂，连接好冷凝管和斯托克分水器，在105℃条件下加热回流10h。反应结束后，待其冷却至室温减压抽滤烘干并采用柱层析法分离提纯。
(3)硫化铟锡/方酸菁复合光催化剂的制备：称量0.1g硫化铟锡于30mL 无水乙醇中，0.01g方酸菁30mL乙醇中，搅拌均匀后，再逐滴滴加方酸菁溶液至硫化铟锡中，持续搅拌12h使其完全混合均匀，在超声条件下反应5h，抽滤洗涤烘干。
实施例2
(1)硫化铟锡的制备：称取0.1728g的五水合四氯化锡和0.5786g四水合三氯化铟，将它们溶解于40mL无水乙醇溶液中，搅拌至溶液澄清透明后，加入0.2962g硫代乙酰胺持续搅拌30min后转移入高压反应釜，在160摄氏度的条件下反应12h，冷却洗涤烘干。
(2)对称型吲哚类方酸菁染料的合成：称取0.145g N-2,3,3-三甲基吲哚和0.052g方酸至三口烧瓶中，加入体积为20mL正丁醇和60mL甲苯混合溶剂，连接好冷凝管和斯托克分水器，在115℃条件下加热回流12h。反应结束后，待其冷却至室温减压抽滤烘干并采用柱层析法分离提纯。
(3)硫化铟锡/方酸菁复合光催化剂的制备：称量0.1g硫化铟锡于30mL 无水乙醇中，0.05g方酸菁150mL乙醇中，搅拌均匀后，再逐滴滴加方酸菁溶液至硫化铟锡中，持续搅拌14h使其完全混合均匀，在超声条件下反应8h，抽滤洗涤烘干。
采用日本JSM-6360A型扫描电子显微镜观察实施例1制备的硫化铟锡及硫化铟锡/方酸菁复合可见光催化剂的形貌，扫描电镜图如图1和图2所示，从图中可以看出，复合可见光催化剂中硫化铟锡花瓣状的表面负载有片状方酸菁染料。
实施例1所制备的硫化铟锡/方酸菁复合可见光催化剂的晶相结构由日本理学D/max2500PC自转X-射线衍射仪分析，其中，X射线为Cu靶Kα
电压40kV，电流100mA，步长为0.02°，扫描范围5°～80°。X射线衍射图谱如图3所示，由图可知，硫化铟锡为高结晶度的四方晶相结构，复合光催化剂中没有明显的方酸菁的峰值出现时是由于少量的方酸菁敏化于硫化铟锡物质。
应用例
将实施例1中制备的硫化铟锡/方酸菁作为光催化剂降解孔雀石绿溶液，其中孔雀石绿溶液浓度为20mg/L，取硫化铟锡/方酸菁光催化剂25mg，先暗反应30min使溶液达到吸附解吸平衡，再进行可见光催化反应，采用1000w氙灯作为光源，每隔一定时间用滴管抽取3ml反应液于离心管中，放入高速离心机中离心5min后，后用紫外-可见分光光度计测量光催化效果。
实施例1所制备的硫化铟锡/方酸菁复合可见光催化剂对孔雀石绿的降解性能如图4所示。由图4可见，25min内孔雀石绿几乎完全降解，可见硫化铟锡/ 方酸菁复合可见光催化剂具有较高的光催化活性和较快的光降解速率。
以上述依据本发明的理想实施例为启示，通过上述的说明内容，相关工作人员完全可以在不偏离本项发明技术思想的范围内，进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容，必须要根据权利要求范围来确定其技术性范围。
Claims (1)
1.一种硫化铟锡/方酸菁复合可见光催化剂的制备方法，其特征是：包括以下步骤：
(1)硫化铟锡的制备：将五水合四氯化锡、四水合三氯化铟溶于无水乙醇中，混合搅拌均匀，加入硫代乙酰胺，继续搅拌30min，转移至高压反应釜内，160℃反应12小时，冷却，洗涤烘干；
(2)吲哚类方酸菁染料的合成：将N-2,3,3-三甲基吲哚和方酸加至三口烧瓶中，加入正丁醇和甲苯混合溶剂，连接好冷凝管和斯托克分水器，105～115℃加热回流10～12小时，冷却至室温，减压抽滤烘干，柱层析分离提纯；
(3)硫化铟锡/方酸菁染料复合光催化剂的制备：硫化铟锡和方酸菁分别加入乙醇，搅拌均匀后，方酸菁溶液逐滴滴加至硫化铟锡溶液中，搅拌12～14h，超声5～8h，抽滤洗涤烘干；
所述的步骤(1)中五水合四氯化锡、四水合三氯化铟、硫代乙酰胺和无水乙醇的摩尔比为1：4：8：1370，无水乙醇的密度为0.789g/cm3；
所述的步骤(2)中N-2,3,3-三甲基吲哚和方酸的摩尔比为2：1，正丁醇和甲苯的体积比为1：1～1：3；
所述的步骤(3)中方酸菁是硫化铟锡质量的10～50％。
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