CN111686769A - 一种光催化剂及其制备方法和应用 - Google Patents
一种光催化剂及其制备方法和应用 Download PDFInfo
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Abstract
本发明属于光催化领域，具体涉及光催化剂及其制备方法以及应用。光催化剂为花球状结构、球形直径为0.5～1μm的BiOI。制备采用原位沉淀的方法制备具有花球状的BiOI单体材料。本发明的制备方法工艺简单、易于操控、成本低廉，构建了具有吸附和可见光光催化协同效应的BiOI特殊结构，在可见光下具有高效的吸附及光催化协同效应。对水体中的有害微生物和染料有机污染物具有高效的杀灭和吸附光降解效果，在水体净化和海洋防污等领域具有很好的实用价值和潜在的应用前景。
Description
技术领域
本发明属于光催化领域，具体涉及一种光催化剂及其制备方法和应用。
背景技术
1.光催化技术是一种利用光能进行物质转化的技术，自1 9 7 2年日本科学家Fujishima和Honda首次报道TiO2在紫外光照下可以光解水产生氢气和氧气以后，半导体光催化技术受到了越来越多的关注[1]。对于半导体材料来说，它们可以在光照条件下产生电子-空穴对，一部分电子和空穴在体相内或表面相遇而复合，另一部分电子迁移到半导体表面具有很强的还原能力，可以与吸附的氧结合，生成具有强氧化性的自由基；而迁移到半导体表面的空穴有很强的氧化能力，可以将吸附在半导体表面的OH-和H2O氧化，产生强氧化性的自由基，比如·OH、·HO2、H2O2和·O2-等[2]，可以直接与反应物发生作用并将其氧化分解，而且不产生二次污染。近年来，光催化技术的应用研究发展十分迅速，因其具有高效、无选择性、稳定性高、绿色无毒、无二次污染、能耗低、操作简便和低成本等突出优点，而且可以充分利用清洁无污染的太阳能，在污水处理、废气处理、空气净化、杀菌消毒、催化制氢、还原CO2等方面已经有广泛应用，并且效果良好。
2.近年来，人们对开发新型的可见光催化剂做了大量研究，其中包含了d0和d10电子构型的In3+、Ce3+、Bi3+、Ag+等。作为新型可见光响应的光催化剂，BiOX(X＝Cl，Br，I)铋系化合物是一类重要的半导体，由于[Bi2O2]2+与卤素层之间存在较强的内建电场，有助于电子-空穴对的有效分离，显现出较高的催化活性。
3.自2006年，Zhang等[3]用水热方法制备了BiOCl粉首次开发出了卤氧化物在光催化领域的应用后，BiOI因其较窄的禁带宽度(约1.9eV)能被可见光激发并在可见光下具有较高的催化活性从而作为一种新型可见光催化材料引起了越来越多的关注[4]。在采用不同方法条件下各种不同形貌的BiOI相继合成出来，比如常用的水热法、溶剂热法、微波水热法、声化学法。但这些方法中大多采用高温高压的条件，并且实验步骤也相对复杂[5-6]。所以能在常温常压下合成BiOI纳米材料是工业运用中不可避免的问题。比如曹等报道了一种能在常温下合成具有纳米化结构的BiOI材料[7]，但是在制备过程中需要加较大量的表面活性剂来控制BiOI的形貌。
发明内容
本发明的目的在于针对现有技术中存在的问题，提供一种光催化剂及其制备方法和应用。
本发明采用一下技术方案实施：
一种光催化剂，光催化剂为花球状结构、球形直径为0.5～1μm的BiOI。
一种光催化剂的制备方法，将Bi(NO3)3·5H2O分散于过量的乙二醇中，然后逐滴加入KI溶液，调节混合液pH值至5～9，混匀后，抽滤、洗涤和干燥即得到具有花球状结构的BiOI；；其中，KI与Bi(NO3)3·5H2O的物质的量之比为1：1～2。
所述分散采用超声分散10～60min，然后进行磁力搅拌10～60min。
所述采用浓度为0.1～5mol/L的NH3·H2O或NaOH调节混合液pH值。
所述调节pH值之后继续搅拌10～36h。
所述洗涤后在常压条件下干燥，温度为50～100℃，干燥时间为3～24h。
一种光催化剂的应用，所述光催化剂在降解染料中的应用。
一种光催化剂的应用，所述光催化剂在水体净化中的应用。
具有花球状结构的BiO I光催化剂用于对水体中有害微生物铜绿假单胞杆菌(P.aeruginosa)和染料污染物罗丹明的可见光催化杀灭和降解，采用氙灯作为光源，其波长范围为420～760nm；所述微生物浓度为106～108cfu/mL，所述罗丹明B的浓度为0～50mg/L，所述BiOI光催化剂的用量为0.051.5mg/mL。
本发明的有益效果：
本发明在常温不添加表面活性剂的情况下，采用原位沉淀的方法制备具有花球状的BiOI单体材料。与其他方法制备的BiOI纳米材料相比具有操作简单，成本低廉。同时这种特定结构的BiOI在具有高效的光催化的同时还表现出良好的吸附性能，其特有的吸附及光催化协同效应在光催化领域的实际应用具有重大意义；具体：
(1)本发明采用的制备方法工艺简单，易于控制、成本低廉。
(2)制备的花球状结构的BiOI单体材料对碱性染料具有很好的吸附性能，
在10～60min内可达到对染料污染物的饱和吸附，对罗丹明B的饱和吸附
量为10～100mg/g。
(3)制备的花球状结构的BiOI单体材料具有较大的比表面积和良好的可见
光吸收性能。
(4)制备的花球状结构的BiOI单体材料的吸附及可见光催化协同效应很显
著，在氙灯照射下，适量的BiOI光催剂对浓度为106～108cfu/mL的微生
物90～150min内杀灭率可达99％以上，对浓度为0～50mg/L的罗丹明B，
60～180min内实现完全吸附降解。
(5)制备的花球状BiOI单体材料表现出高效的吸附和光降解协同效应提高
了可见光催化活性，在水体净化和海洋防污等领域具有很好的实用价值和潜在的应用前景。
附图说明
图1为本发明所制备样品的X-射线衍射(XRD)图谱(其中横坐标为2θ(角度)，单位
为度；纵坐标为强度，单位为相对单位)。
图2为本发明所制备样品的扫描电子显微镜(FE-SEM)照片。
图3为本发明所制备的样品吸附及光催化协同降解反应中罗丹明B浓度随时间的变化曲线(其图中横坐标为时间，单位为min(分钟)；纵坐标为Ct/C0，C0为反应开始前罗丹明B初始浓度，Ct为反应时间为t时的罗丹明B浓度。
图4为本发明所制备的样品对铜绿假单胞菌的可见光光催化的杀灭实验(其中横
坐标为样品组(对照组、实验组(BiOI))；纵坐标为杀菌率，单位为％)。
具体实施方式
以下通过具体的实施例对本发明作进一步说明，有助于本领域的普通技术人员更全面的理解本发明，但不以任何方式限制本发明。
本发明通过常温原位沉淀法制备了具有花球状结构的BiOI单体光催化剂，该光催化剂不仅具有良好的可见光吸收性能，其特定的花球状结构在加快了光生载流子的分离，减小了光生电子-空穴对的复合几率，其特殊表面性质使其对碱性染料具有很好的吸附效果，在可见光下表现出高效的吸附及光催化协同效应，对水体中有害微生物和染料污染物具有高效的杀灭和吸附降解效果，在水体净化和海洋防污等领域具有很好的实用价值和潜在的应用前景。同时该单体光催化剂具有制备方法简单、价格低廉和重复性好等特点。
实施1具有花球状结构的BiOI单体材料的制备方法。
通过常温下原位沉淀的方法制备花球状结构的BiOI单体材料。称取10mmol Bi(NO3)3·5H2O加入到35mL乙二醇中，超声分散30min，然后磁力搅拌30min，逐滴加入35mL浓度为0.3mol/L的KI溶液，滴加完成后用2.0mol/L NH3·H2O溶液调节混合液的pH为7，继续搅拌24h。搅拌结束后，经过抽滤，再由乙醇和水依次洗涤，洗涤后60℃干燥6h即得到具有花球状状结构的BiOI单体材料(参见图1-2)。
由图1可知，所制备的BiOI具有四方晶体结构，且具有很高的纯度。
由图2可见，BiOI为呈花球状颗粒，结晶度较高，尺寸约为0.5～1μm，其花结构是由许多规则的二维纳米薄片交叉堆积而成，每个纳米片大小约为0.5μm，厚度约为20nm。这种花球状结构将具有较大的比表面积和良好的可见光吸收性能。
实施2具有花球状结构的BiOI单体材料的制备方法。
通过常温下原位沉淀的方法制备花球状结构的BiOI单体材料。称取10mmol Bi(NO3)3·5H2O加入到50mL乙二醇中，超声分散10min，然后磁力搅拌30min，逐滴加入50mL浓度为0.2mol/L的KI溶液，滴加完成后用2.0mol/L NH3·H2O溶液调节混合液的pH为8，继续搅拌24h。搅拌结束后，经抽滤，再由乙醇和水依次洗涤，洗涤后60℃干燥6h即得到具有花球状状结构的BiOI单体材料。
应用例1：具有花球状结构的BiOI光催化剂应用于染料污染物罗丹明B吸附可见光催化协同降解。
以500W氙灯作为光源，辅以滤光片滤掉紫外光，使其波长范围为420～760nm。将50mL 30mg/L的罗丹明B溶液加入到50mL反应器中，加入10mg本发明制备的光催化剂，分别在暗态和光照条件下进行吸附和光催化反应，反应过程中间隔一定时间取样，离心分离后取上层清液在紫外-可见分光光度计上测定554nm波长下罗丹明B溶液的吸光度，得到罗丹明B溶液的残余浓度，以此计算吸附降解率(参见图3)。
由图3可见，在黑暗条件下材料对罗丹明B有很好的吸附性能，其达到饱和吸附的时间在30min左右，吸附率可达到26％以上，吸附量为45mg/g。在可见光照下，本催化材料显示出较好的吸附光催化协同效应，在150min反应时间内对罗丹明B的吸附降解率接近100％。因此，具花球状结构的BiOI单体对罗丹明B具有良好的吸附性能，并且在可见光的条件下还表现出较好的吸附及光降解协同效应。
应用例2：具有花球状结构的BiOI光催化剂应用于水体中，对有害微生物铜绿假单胞杆菌的可见光杀灭。
以500W氙灯作为光源，辅以滤光片滤掉紫外光，使其波长范围为420～760nm。以铜绿假单胞杆菌(P.aeruginosa，8.0×108cfu/mL)评价花球状BiOI单体材料光催化剂的光催化杀菌性能。首先准备细菌悬液，将一定量的铜绿假单胞杆菌储存液接种到灭菌LB液体培养基中，然后将其置于38℃、150rpm的空气恒温摇床中，过夜培养。培养得到的细菌悬液离心后悬浮于0.01mol/LPBS(pH＝7.3)缓冲液中，得到浓度为8.0×108cfu/mL的铜绿假单胞杆菌悬液。光催化实验中取49.5mL灭菌0.01mol/L PBS(pH＝7.4)缓冲液加入到50mL反应器中，然后加入500μL细菌悬液，使反应液中细菌浓度为8.0×106cfu/mL，加入50mg本发明制备的光催化剂。暗态吸附达到平衡后进行光催化反应，反应过程中间隔一定时间取样，通过平板计数法确定细菌的存活率和杀菌率。
具体步骤为：取1.1mL反应液，用0.01mol/L PBS(pH＝7.3)缓冲液按照系列稀释法依次稀释几个梯度，然后从不同稀释倍数的溶液中取100μL至已经准备好的LB固体培养基上，将菌液均匀地涂抹在LB培养基上。将LB培养基倒置，放入电热恒温培养箱中38℃培养18h，通过计数培养基上长出的菌落个数，以及相应稀释倍数得出细菌浓度，以确定细菌的存活率和杀菌率。实验中每组实验均需平行测定4次，取平均值作为最后结果。空白实验作为对照实验(参见图4)。
由图4可见催化剂具有较大的比表面积和良好的可见光吸收性能，导致其可见光催化性能提高，具有良好的可见光催化杀菌性能。
Claims (8)
1.一种光催化剂，其特征在于：光催化剂为花球状结构、球形直径为0.5～1μm的BiOI。
2.一种权利要求1所述的光催化剂的制备方法，其特征在于：将Bi(NO3)3·5H2O分散于过量的乙二醇中，然后逐滴加入KI溶液，混合后，调节混合液pH值至5～9，混匀后，抽滤、洗涤和干燥即得到具有花球状结构的BiOI；其中，KI与Bi(NO3)3·5H2O的物质的量之比为1：1～2。
3.根据权利要求2所述的光催化剂的制备方法，其特征在于：所述分散采用超声分散10～60min，然后进行磁力搅拌10～60min。
4.根据权利要求2所述的光催化剂的制备方法，其特征在于：所述采用浓度为0.1～5mol/L的NH3·H2O或NaOH调节混合液pH值。
5.根据权利要求2所述的光催化剂的制备方法，其特征在于：所述调节pH值之后继续搅拌10～36h。
6.根据权利要求2所述的光催化剂的制备方法，其特征在于：所述洗涤后在常压条件下干燥，温度为50～100℃，干燥时间为3～24h。
7.一种权利要求1所述的光催化剂的应用，其特征在于：所述光催化剂在降解染料中的应用。
8.一种权利要求1所述的光催化剂的应用，其特征在于：所述光催化剂在水体净化中的应用。
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| CN114247455A (zh) * | 2022-01-10 | 2022-03-29 | 辽宁大学 | 一种负载型BiOI光催化材料的制备方法及应用 |
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