CN106362728B - 纳米片状Bi2Ga4O9的制备方法及应用 - Google Patents
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Abstract
本发明公开了一种纳米片状Bi2Ga4O9的制备方法,包括如下步骤:以氧化镓和碳酸钠为原料,首先利用固相法制备镓酸钠(NaGaO2)前驱体,然后以NaGaO2、氢氧化钠和六水合硝酸铋为原料,在180‑200℃恒温条件下水热反应12‑36h,将获得的沉淀洗涤、离心分离,在80℃的恒温条件下干燥8h,获得纳米片状Bi2Ga4O9,所述纳米片状Bi2Ga4O9可作为光催化剂使用。本发明的优点在于制备工艺简单易行、安全、能耗低,所制备的纳米片状Bi2Ga4O9对水中有机污染物具有良好的降解性能。
Description
技术领域
本发明属于新材料技术领域,具体涉及一种纳米片状Bi2Ga4O9光催化剂的制备方法。
背景技术
水中微量难降解有机污染物具有毒性大、生物降解性能差和处理难度大等特点,采用传统的废水处理方法很难使其彻底降解。如吸附法、电化学和膜过滤技术无法彻底去除污染物,会导致二次污染;生物处理法则因有机污染物对微生物的毒性限制了微生物的生长从而不能达到理想的降解效果。因此,研究高效的方法,用以处理难降解有机废水已成为现阶段环境保护技术领域亟待解决的一个难题。光催化技术可以将低密度的太阳光能转化为高密度的化学能,可以直接利用太阳光降解水体中的各类有机污染物,这为我们提供了一种治理环境污染的理想途径。光催化技术的核心是光催化材料,目前光催化材料的形貌调控已成为材料领域的研究热点之一,大量的研究也表明具备纳米片、纳米带或立方状的光催化材料如TiO2、BiOCl、BiOBr、BiVO4和Ag3PO4等对降解水体中有机污染物具有非常优异的光催化活性。由于部分铋系光催化材料具备可见光光催化性能,因而备受关注。
近年来学者们发现陶瓷半导体材料Bi2M4O9(M=Al3+、Fe3+、Ga3+)不仅具有良好的热稳定性、电化学和铁电性能,而且还具有良好的光催化性能。这类Bi2M4O9陶瓷半导体材料的制备过程大多为高温固相法,不仅需要消耗大量的热能,而且制备的Bi2M4O9半导体纯度不高,微观颗粒尺寸较大,影响了其性能。第一性原理理论计算表明Bi2Ga4O9半导体的导带主要由Bi6p、Ga4s和O2p轨道组成,价带主要由O2s和Ga3d轨道组成。Bi2Ga4O9结构中扭曲的八面体GaO6和四面体GaO4会影响其光催化性能(Inorganic chemistry, 2016, 55(10):4824-4835)。Bi2Ga4O9作为一种典型的陶瓷半导体材料,其光催化性能还鲜有报道。因此,通过形貌调控方式来研究Bi2Ga4O9半导体的光催化性能具有重要的理论。这不仅丰富了形貌调控理论内容,而且对于开发陶瓷半导体光催化具有重要的参考价值。
发明内容
针对上述现有技术存在的不足,本发明提供一种纳米片状Bi2Ga4O9的制备方法及应用,制备工艺简单、安全、能耗低,所制备的Bi2Ga4O9光催化剂纯度高、呈片状且光催化剂性能良好。
为实现上述目的,本发明采用以下技术方案:
纳米片状Bi2Ga4O9的制备方法,它包括以下步骤:
(1)按氧化镓和碳酸钠的摩尔比1:1称取氧化镓和碳酸钠,将其研磨混合均匀,850~900℃焙烧12~15h,自然冷却后获得NaGaO2前驱体;
(2)按Bi(NO3)3·6H2O和NaGaO2摩尔比1:(2~2.1)称取Bi(NO3)3·6H2O和NaGaO2,并按Bi(NO3)3·6H2O、超纯水和5mol/L氢氧化钠溶液1mmol:30mL:(0.25~0.32)mL的配比准备超纯水和氢氧化钠溶液,先把Bi(NO3)3·6H2O、NaGaO2和超纯水混合于100mL烧杯中,搅拌5-10min,然后加入5mol/L氢氧化钠溶液,搅拌15-20min得到前驱体悬浊液,将前驱体悬浊液转移至内衬为聚四氟乙烯的不锈钢反应釜中;
(3)将步骤(2)中装有悬浊液的反应釜置于烘箱中水热反应,水热反应温度为180-200℃,水热反应时间为12-36h,反应结束后,自然冷却到室温;
(4)将步骤(3)获得的沉淀洗涤、离心、干燥,获得纳米片状Bi2Ga4O9光催化剂,干燥温度为70-90℃。
纳米片状Bi2Ga4O9的制备方法,它包括以下步骤:
(1)按氧化镓和碳酸钠的摩尔比1:1称取氧化镓和碳酸钠,将其研磨混合均匀,900℃焙烧12h,自然冷却后获得NaGaO2前驱体;
(2)按Bi(NO3)3·6H2O和NaGaO2摩尔比1:2称取Bi(NO3)3·6H2O和NaGaO2,并按Bi(NO3)3·6H2O、超纯水和5mol/L氢氧化钠溶液1mmol:30mL:0.25mL的配比准备超纯水和氢氧化钠溶液,先把Bi(NO3)3·6H2O、NaGaO2和超纯水混合于100mL烧杯中,搅拌5-10min,然后加入5mol/L氢氧化钠溶液,搅拌15-20min得到前驱体悬浊液,将前驱体悬浊液转移至内衬为聚四氟乙烯的不锈钢反应釜中;
(3)将步骤(2)中装有悬浊液的反应釜置于烘箱中水热反应,水热反应温度为180-200℃,水热反应时间为12-36h,反应结束后,自然冷却到室温;
(4)将步骤(3)获得的沉淀洗涤、离心、干燥,获得纳米片状Bi2Ga4O9光催化剂,干燥温度为70-90℃。
步骤(4)中的干燥温度为80℃,干燥的时间为8h。
所述制备方法制备的纳米片状Bi2Ga4O9,所述纳米片状Bi2Ga4O9作为光催化剂。
与现有技术相比,本发明的有益效果:(1)本发明公开的纳米片状Bi2Ga4O9光催化剂制备方法工艺简单、安全、能耗低;(2)本发明公开的制备方法所所制备的纳米片状Bi2Ga4O9纯度高、结晶度好,且形貌为均一的纳米片;(3)本发明所制得的纳米片状Bi2Ga4O9具备良好的光催化活性,在环境领域具有良好的应用前景。
附图说明
图1 中(a)和(b)分别为实施例1和实施例2制备的纳米片状Bi2Ga4O9的X射线衍射图谱。
图2中(a)和(b)分别为实施例1和实施例2制备的纳米片状Bi2Ga4O9的扫描电子显微镜图。
图3中(a)和(b)分别为实施例1和实施例2制备的纳米片状Bi2Ga4O9在紫外光照射下对酸性红1的降解效果图。
具体实施方式
为使本发明的目的、技术方案及效果更加清楚、明确,以下参照附图对本发明进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。
纳米片状Bi2Ga4O9的制备方法,它包括以下步骤:
(1)按氧化镓和碳酸钠的摩尔比1:1称取氧化镓和碳酸钠,将其研磨混合均匀,850~900℃焙烧12~15h,自然冷却后获得NaGaO2前驱体;
(2)按Bi(NO3)3·6H2O和NaGaO2摩尔比1:(2~2.1)称取Bi(NO3)3·6H2O和NaGaO2,并按Bi(NO3)3·6H2O、超纯水和5mol/L氢氧化钠溶液1mmol:30mL:(0.25~0.32)mL的配比准备超纯水和氢氧化钠溶液,先把Bi(NO3)3·6H2O、NaGaO2和超纯水混合于100mL烧杯中,搅拌5-10min,然后加入5mol/L氢氧化钠溶液,搅拌15-20min得到前驱体悬浊液,将前驱体悬浊液转移至内衬为聚四氟乙烯的不锈钢反应釜中;
(3)将步骤(2)中已装有悬浊液的反应釜置于烘箱中水热反应,水热反应温度为180-200℃,水热反应时间为12-36h,反应结束后,自然冷却到室温;
(4)将步骤(3)获得的沉淀洗涤、离心、干燥,获得纳米片状Bi2Ga4O9光催化剂,干燥温度为70-90℃。
实施例1
纳米片状Bi2Ga4O9的制备方法,它包括以下步骤:
(1)按氧化镓和碳酸钠的摩尔比1:1称取氧化镓和碳酸钠,将其研磨混合均匀,850℃焙烧12h,自然冷却获得NaGaO2前驱体;
(2)按Bi(NO3)3·6H2O和NaGaO2摩尔比1:2称取Bi(NO3)3·6H2O和NaGaO2;并按Bi(NO3)3·6H2O、超纯水和5mol/L氢氧化钠溶液1mmol:30mL:0.25mL的配比准备超纯水和氢氧化钠溶液,先把Bi(NO3)3·6H2O、NaGaO2和超纯水混合于100mL烧杯中,搅拌5-10min,然后加入5mol/L氢氧化钠溶液,搅拌15-20min得到前驱体悬浊液,将前驱体悬浊液转移至内衬为聚四氟乙烯的不锈钢反应釜中;
(3)将步骤(2)中装有悬浊液的反应釜置于烘箱中水热反应(180℃,36h),反应结束后,自然冷却到室温;
(4)将步骤(3)获得的沉淀洗涤、离心、80℃干燥,获得纳米片状Bi2Ga4O9。
实施例2
纳米片状Bi2Ga4O9制备方法,它包括以下步骤:
(1)按氧化镓和碳酸钠的摩尔比1:1称取氧化镓和碳酸钠,将其研磨混合均匀,900℃焙烧15h,自然冷却获得NaGaO2前驱体;
(2)按Bi(NO3)3·6H2O和NaGaO2摩尔比1:2.1称取Bi(NO3)3·6H2O和NaGaO2;并按Bi(NO3)3·6H2O、超纯水和5mol/L氢氧化钠溶液1mmol:30mL:0.30mL的配比准备超纯水和氢氧化钠溶液,先把Bi(NO3)3·6H2O、NaGaO2和超纯水混合于100mL烧杯中,搅拌5-10min,然后加入5mol/L氢氧化钠溶液,搅拌15-20min得到前驱体悬浊液,将前驱体悬浊液转移至内衬为聚四氟乙烯的不锈钢反应釜中;
(3)将步骤(2)中装有悬浊液的反应釜置于烘箱中水热反应(200℃,12h),反应结束后,自然冷却到室温;
(4)将步骤(3)获得的沉淀洗涤、离心、90℃干燥,即得纳米片状Bi2Ga4O9。
本发明采用X射线衍射仪(Bruker D8 Advance)和扫描电子显微镜(FEI Quanta200)表征所获得的Bi2Ga4O9光催化剂的物相和形貌;
实施例1制得的纳米片状Bi2Ga4O9XRD图谱见图1(a),实施例2制得的纳米片状Bi2Ga4O9XRD图谱见图1(b),图1中纳米片状Bi2Ga4O9的XRD衍射峰位置与Bi2Ga4O9(JCPDS 76-2240)标准峰位置一一对应,说明所制备的样品为纯Bi2Ga4O9。实施例1制得的纳米片状Bi2Ga4O9SEM图见图2(a),实施例2制得的纳米片状Bi2Ga4O9SEM图见图2(b)。从图1-2可知所制备的Bi2Ga4O9纯度高、结晶度好,且形貌为纳米片。
本发明所制备的纳米片状Bi2Ga4O9的光催化活性是通过降解酸性红1染料溶液进行评价的,具体操作如下:
称取0.05g纳米片状Bi2Ga4O9样品于容积为50mL的石英试管中,加入50mL浓度为20mg/L酸性红1染料溶液模拟有机废水。首先在黑暗条件下搅拌30min使纳米片状Bi2Ga4O9充分分散于酸性红1溶液,然后开启300W高压汞灯光源,每隔15min取约5mL悬浊液样品,持续光照时间为60min。实验结果后离心所取的悬浊液样品,取其上清液并检测酸性红1的浓度。
将实施例1制得的纳米片状Bi2Ga4O9在降解初始浓度为20mg/L酸性红1的实验中,投加量为1.0g/L,光催化反应60min后酸性红1的降解率约为95.9%,说明该方法所制备的纳米片状Bi2Ga4O9具有良好的光催化降解有机物性能。
将实施例2制得的纳米片状Bi2Ga4O9在降解初始浓度为20mg/L酸性红1的实验中,投加量为1.0g/L,光催化反应60min后酸性红1的降解率约为96.7%,说明该方法所制备的纳米片状Bi2Ga4O9具有良好的光催化降解有机物性能。
实施例3
纳米片状Bi2Ga4O9制备方法,它包括以下步骤:
(1)按氧化镓和碳酸钠的摩尔比1:1称取氧化镓和碳酸钠,将其研磨混合均匀,870℃焙烧13h,自然冷却获得NaGaO2前驱体;
(2)按Bi(NO3)3·6H2O和NaGaO2摩尔比1:2.1称取Bi(NO3)3·6H2O和NaGaO2;并按Bi(NO3)3·6H2O、超纯水和5mol/L氢氧化钠溶液1mmol:30mL:0.32mL的配比准备超纯水和氢氧化钠溶液,先把Bi(NO3)3·6H2O、NaGaO2和超纯水混合于100mL烧杯中,搅拌5-10min,然后加入5mol/L氢氧化钠溶液,搅拌15-20min得到前驱体悬浊液,将前驱体悬浊液转移至内衬为聚四氟乙烯的不锈钢反应釜中;
(3)将步骤(2)中装有悬浊液的反应釜置于烘箱中水热反应(190℃,18h),反应结束后,自然冷却到室温;
(4)将步骤(3)获得的沉淀洗涤、离心、70℃干燥,即得纳米片状Bi2Ga4O9。
实施例4
纳米片状Bi2Ga4O9制备方法,它包括以下步骤:
(1)按氧化镓和碳酸钠的摩尔比1:1称取氧化镓和碳酸钠,将其研磨混合均匀,880℃焙烧14h,自然冷却获得NaGaO2前驱体;
(2)按Bi(NO3)3·6H2O和NaGaO2摩尔比1:2称取Bi(NO3)3·6H2O和NaGaO2;并按Bi(NO3)3·6H2O、超纯水和5mol/L氢氧化钠溶液1mmol:30mL:0.28mL的配比准备超纯水和氢氧化钠溶液,先把Bi(NO3)3·6H2O、NaGaO2和超纯水混合于100mL烧杯中,搅拌5-10min,然后加入5mol/L氢氧化钠溶液,搅拌15-20min得到前驱体悬浊液,将前驱体悬浊液转移至内衬为聚四氟乙烯的不锈钢反应釜中;
(3)将步骤(2)中装有悬浊液的反应釜置于烘箱中水热反应(185℃,24h),反应结束后,自然冷却到室温;
(4)将步骤(3)获得的沉淀洗涤、离心、85℃干燥,即得纳米片状Bi2Ga4O9。
以上所述的仅是本发明的优选实施方式,应当指出,对于本领域的技术人员来说,在不脱离本发明整体构思前提下,还可以作出若干改变和改进,这些也应该视为本发明的保护范围。
Claims (4)
1.纳米片状Bi2Ga4O9的制备方法,其特征在于,它包括以下步骤:
(1)按氧化镓和碳酸钠的摩尔比1:1称取氧化镓和碳酸钠,将其研磨混合均匀,850~900℃焙烧12~15h,自然冷却后获得NaGaO2前驱体;
(2)按Bi(NO3)3·6H2O和NaGaO2摩尔比1:(2~2.1)称取Bi(NO3)3·6H2O和NaGaO2,并按Bi(NO3)3·6H2O、超纯水和5mol/L氢氧化钠溶液1mmol:30mL:(0.25~0.32)mL的配比准备超纯水和氢氧化钠溶液,先把Bi(NO3)3·6H2O、NaGaO2和超纯水混合于100mL烧杯中,搅拌5-10min,然后加入5mol/L氢氧化钠溶液,搅拌15-20min得到前驱体悬浊液,将前驱体悬浊液转移至内衬为聚四氟乙烯的不锈钢反应釜中;
(3)将步骤(2)中装有悬浊液的反应釜置于烘箱中水热反应,水热反应温度为180-200℃,水热反应时间为12-36h,反应结束后,自然冷却到室温;
(4)将步骤(3)获得的沉淀洗涤、离心、干燥,获得纳米片状Bi2Ga4O9光催化剂,干燥温度为70-90℃。
2.根据权利要求1所述的纳米片状Bi2Ga4O9的制备方法,其特征在于:它包括以下步骤:
(1)按氧化镓和碳酸钠的摩尔比1:1称取氧化镓和碳酸钠,将其研磨混合均匀,900℃焙烧12h,自然冷却后获得NaGaO2前驱体;
(2)按Bi(NO3)3·6H2O和NaGaO2摩尔比1:2称取Bi(NO3)3·6H2O和NaGaO2,并按Bi(NO3)3·6H2O、超纯水和5mol/L氢氧化钠溶液1mmol:30mL:0.25mL的配比准备超纯水和氢氧化钠溶液,先把Bi(NO3)3·6H2O、NaGaO2和超纯水混合于100mL烧杯中,搅拌5-10min,然后加入5mol/L氢氧化钠溶液,搅拌15-20min得到前驱体悬浊液,将前驱体悬浊液转移至内衬为聚四氟乙烯的不锈钢反应釜中;
(3)将步骤(2)中装有悬浊液的反应釜置于烘箱中水热反应,水热反应温度为180-200℃,水热反应时间为12-36h,反应结束后,自然冷却到室温;
(4)将步骤(3)获得的沉淀洗涤、离心、干燥,获得纳米片状Bi2Ga4O9光催化剂,干燥温度70-90℃。
3.根据权利要求1所述的纳米片状Bi2Ga4O9的制备方法,其特征在于:步骤(4)中的干燥温度为80℃,干燥的时间为8h。
4.根据权利要求1-3任一所述制备方法制备的纳米片状Bi2Ga4O9,其特征在于:所述纳米片状Bi2Ga4O9作为光催化剂。
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