CN105964285B - 一种g-C3N4/Bi3TaO7表面复合光催化剂的制备方法 - Google Patents
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Abstract
本发明涉及复合光催化剂，特指一种g‑C3N4/Bi3TaO7表面复合光催化剂的制备方法，分别称取三聚氰胺和水热法制备的的Bi3TaO7，混合均匀后，置于马弗炉中550℃煅烧4h、收集样品，得到g‑C3N4/Bi3TaO7表面复合光催化剂。水热法制备的Bi3TaO7颗粒的粒径为20‑40nm，这种纳米尺寸的Bi3TaO7与三聚氰胺煅烧的过程中，Bi3TaO7能够很好的复合到生成的片状g‑C3N4表面，而且在g‑C3N4和Bi3TaO7界面上形成化学作用连接，有效的增强g‑C3N4/Bi3TaO7表面复合光催化剂光催化性能，也提高了复合光催化剂的稳定性。
Description
技术领域
本发明涉及复合光催化剂，特指一种以TaCl5、Bi(NO3)3·5H2O和三聚氰胺为原料来制备g-C3N4/Bi3TaO7表面复合光催化剂的方法，是一种制备工艺简单，成本低廉的方法。
背景技术
半导体材料因其环境友好、无毒无害、稳定性好的特性在解决能源危机和环境问题等方面的潜在应用价值而日益受到人们的关注；其中TiO2及Ti系化合物是研究较早的半导体光催化剂，然而，他们的禁带宽度都较大，只能对紫外光进行响应，而紫外光只占太阳光的4％-6％，因此，研究可见光响应光催化半导体材料意义重大。近年来，一些钽酸盐光催化剂(如Bi3TaO7，InTaO4等)因为在可见光下具有较好的光催化活性逐渐成为了人们研究的热点。Bi3TaO7具有萤石结构以及禁带宽度在2.74-2.86eV，而且其三维结构可以形成表面缺陷和氧空位， Bi3TaO7在可见光下显示出较好的光催化活性。然而，其光致电荷的分离效果，限制了Bi3TaO7的进一步应用。
半导体复合是提高电荷分离效率和增强光催化活性的有效途径。g-C3N4因具有类石墨结构以及合适的能带电位使其成为研究较多的复合半导体。最近，Liu 等人(Liu J,Liu Y,Liu N,et al.Metal-free efficient photocatalyst for stable visible watersplitting via a two-electron pathway[J].Science,2015,347(6225):970-974.) 合成碳量子点与氮化碳(C3N4)的复合材料作为光催化剂；Zhao等人(Zhao,J.； Ji,Z.；Shen,X.；Zhou,H.；Ma,L.,Facile synthesis of WO3nanorods/g-C3N4 composites with enhancedphotocatalytic activity.Ceram.Int.2015,41(4), 5600-5606.)制备了WO3纳米棒与g-C3N4复合光催化剂；Song等人(Song,C.；Fan, M.；Hu,B.；Chen,T.；Wang,L.；Shi,W.,Synthesis of a g-C3N4-sensitized and NaNbO3-substrated II-type heterojunctionwith enhanced photocatalytic degradation activity.CrystEngComm 2015,17(24),4575-4583.)制备了成功制备了NaNbO3和 g-C3N4复合材料，具有较好的活性。
迄今为止，尚未发现有人制备g-C3N4/Bi3TaO7复合材料。本发明采用水热法和固相法成功制备了g-C3N4/Bi3TaO7复合材料，所制备的g-C3N4/Bi3TaO7复合材料在环境、能源等领域有良好应用前景。
发明内容
本发明目的是提供一种使用水热法合成和固相反应法制备g-C3N4/Bi3TaO7表
面复合光催化剂的方法。
本发明通过以下步骤实现：
分别称取三聚氰胺和水热法制备的的Bi3TaO7，混合均匀后，置于马弗炉中 550℃煅烧4h、收集样品，得到g-C3N4/Bi3TaO7表面复合光催化剂。
所述的g-C3N4/Bi3TaO7表面复合光催化剂中g-C3N4所占的质量比为 10％-90％。
进一步地，所述的g-C3N4/Bi3TaO7表面复合光催化剂中g-C3N4所占的质量比为50％。
本发明采用水热法和固相反应法成功制备了g-C3N4/Bi3TaO7表面复合光催化剂，水热法制备的Bi3TaO7颗粒的粒径为20-40nm，这种纳米尺寸的Bi3TaO7与三聚氰胺煅烧的过程中，Bi3TaO7能够很好的复合到生成的片状g-C3N4表面，而且在g-C3N4和Bi3TaO7界面上形成化学作用连接，有效的增强g-C3N4/Bi3TaO7表面复合光催化剂光催化性能，也提高了复合光催化剂的稳定性。
所述Bi3TaO7的制备方法如下：
(1)将TaCl5和Bi(NO3)3·5H2O分别溶于乙醇溶液中，TaCl5与Bi(NO3)3·5H2O 摩尔比为3：5，分别搅拌均匀后，将TaCl5和Bi(NO3)3·5H2O溶液混合，继续搅拌至混合均匀。
(2)调节TaCl5和Bi(NO3)3·5H2O混合溶液的pH值为10，搅拌后，将以上混合溶液转移至耐高温反应釜，置于220℃烘箱中保持24h，之后冷却至室温，洗涤后干燥，得到纯相Bi3TaO7。
步骤(1)中，所述的乙醇的加入量以能溶解TaCl5和Bi(NO3)3·5H2O为准；所述分别搅拌的时间均为30min；所述继续搅拌的时间也为30min。
步骤(2)中，所述调节TaCl5和Bi(NO3)3·5H2O混合溶液的pH值指采用7mol·L-1的NaOH溶液进行调节；搅拌时间为30min；所述洗涤指依次用蒸馏水和乙醇洗涤3遍。
利用X-射线衍射(XRD)、场发射扫描电子显微镜(FESEM)、X光电子能谱仪(XPS)等仪器对产物进行形貌结构分析，以四环素溶液为目标染料进行光催化降解实验，通过紫外-可见分光光度计测量吸光度，以评估其光催化活性。
附图说明
图1为所制备的g-C3N4/Bi3TaO7的XRD衍射谱图，其中g-C3N4的含量分别为 0％、10％、30％、50％、70％、90％和100％(质量比)。
图2为所制备的不同含量g-C3N4/Bi3TaO7表面复合光催化剂的场发射扫描电镜图。
图3为所制备的不同含量g-C3N4/Bi3TaO7表面复合光催化剂的透射光谱图。
图4为所制备的不同含量g-C3N4/Bi3TaO7表面复合光催化剂的XPS谱图。
图5为所制备的不同含量g-C3N4/Bi3TaO7表面复合光催化剂可见光降解四环素活性图，其中a为纯的g-C3N4，b为纯的Bi3TaO7，c中g-C3N4含量为90％，d中 g-C3N4含量为10％，e中g-C3N4含量为70％，f中g-C3N4含量为30％，g中g-C3N4含量为50％。
实施例1 g-C3N4/Bi3TaO7表面复合光催化剂的制备
称取Bi3TaO7粉末0.5g，三聚氰胺质量分别为0.11g、0.428g、1g，2.34g和9g，将两者混合均匀后置于马弗炉中550℃煅烧4h，收集得到g-C3N4质量比为10％、 30％、50％、70％、90％的g-C3N4/Bi3TaO7表面复合光催化剂。
实施例2 g-C3N4/Bi3TaO7表面复合光催化剂的表征
如图1所示，不同含量的g-C3N4/Bi3TaO7表面复合光催化剂的XRD图谱显示，当g-C3N4的含量低于30％时，未发现其特征峰；当g-C3N4的含量高于30％时， g-C3N4的特征峰逐渐明显。
如图2和3所示，g-C3N4含量为50％时的g-C3N4/Bi3TaO7表面复合光催化剂的中， g-C3N4的为片状结构，厚度为10nm左右。
如图4所示，XPS图中可以看出有C、N、O、Ta、Bi元素的存在。
实施例3不同含量的g-C3N4/Bi3TaO7表面复合光催化剂的可见光催化活性实验
(1)配制浓度为10μg/L的四环素溶液，将配好的溶液置于暗处。
(2)称取不同含量的g-C3N4/Bi3TaO7表面复合光催化剂50mg，分别置于光催化反应器中，加入100mL步骤(1)所配好的目标降解液，磁力搅拌60min待复合光催化剂分散均匀后，打开水源，光源，进行光催化降解实验。
(3)每15min吸取反应器中的光催化降解液，离心后用于紫外-可见吸光度的测量。
(4)由图5可见所制备的纳米复合光催化剂具有优异的可见光催化活性，尤其是g-C3N4的含量为50％的样品，与纯的Bi3TaO7相比，90min内四环素的降解活性提高了1.8倍。
Claims (5)
1.一种g-C3N4/Bi3TaO7表面复合光催化剂的制备方法，其特征在于：分别称取三聚氰胺和水热法制备的Bi3TaO7，混合均匀后，置于马弗炉中煅烧后收集样品，得到g-C3N4/Bi3TaO7表面复合光催化剂；所述的g-C3N4/Bi3TaO7表面复合光催化剂中g-C3N4所占的质量比为50％，与纯的Bi3TaO7相比，90min内四环素的降解活性提高了1.8倍；所述煅烧指550℃煅烧4h。
2.如权利要求1所述的一种g-C3N4/Bi3TaO7表面复合光催化剂的制备方法，其特征在于：水热法制备的Bi3TaO7颗粒的粒径为20-40nm，这种纳米尺寸的Bi3TaO7与三聚氰胺煅烧的过程中，Bi3TaO7能够很好的复合到生成的片状g-C3N4表面，而且在g-C3N4和Bi3TaO7界面上形成化学作用连接，有效的增强g-C3N4/Bi3TaO7表面复合光催化剂光催化性能，也提高了复合光催化剂的稳定性。
3.如权利要求1所述的一种g-C3N4/Bi3TaO7表面复合光催化剂的制备方法，其特征在于所述Bi3TaO7的制备方法如下：
(1)将TaCl5和Bi(NO3)3·5H2O分别溶于乙醇溶液中，TaCl5与Bi(NO3)3·5H2O摩尔比为3：5，分别搅拌均匀后，将TaCl5和Bi(NO3)3·5H2O溶液混合，继续搅拌至混合均匀；
(2)调节TaCl5和Bi(NO3)3·5H2O混合溶液的pH值为10，搅拌后，将以上混合溶液转移至耐高温反应釜，置于220℃烘箱中保持24h，之后冷却至室温，洗涤后干燥，得到纯相Bi3TaO7。
4.如权利要求3所述的一种g-C3N4/Bi3TaO7表面复合光催化剂的制备方法，其特征在于：步骤(1)中，所述的乙醇的加入量以能溶解TaCl5和Bi(NO3)3·5H2O为准；所述分别搅拌的时间均为30min；所述继续搅拌的时间也为30min。
5.如权利要求3所述的一种g-C3N4/Bi3TaO7表面复合光催化剂的制备方法，其特征在于：步骤(2)中，所述调节TaCl5和Bi(NO3)3·5H2O混合溶液的pH值指采用7mol·L-1的NaOH溶液进行调节；搅拌时间为30min；所述洗涤指依次用蒸馏水和乙醇洗涤3遍。
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| CN105195201A (zh) * | 2015-10-16 | 2015-12-30 | 江苏大学 | Ta2O5/g-C3N4杂化可见光光催化剂的制备及应用 |
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| CN105195201A (zh) * | 2015-10-16 | 2015-12-30 | 江苏大学 | Ta2O5/g-C3N4杂化可见光光催化剂的制备及应用 |
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