CN106238088B - 一种高分散性g-C3N4/TiO2光触媒无机水溶胶制备方法 - Google Patents
一种高分散性g-C3N4/TiO2光触媒无机水溶胶制备方法 Download PDFInfo
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Abstract
本发明公开了一种高分散性g‑C3N4/TiO2光触媒无机水溶胶制备方法，属功能材料领域。该方法将g‑C3N4/TiO2光触媒在搅拌情况下以一定比例加入到含有无机分散剂的水溶液中，添加少量胶溶剂并调节悬浮液pH值，然后经剪切乳化和搅拌处理，得到稳定的高分散性g‑C3N4/TiO2光触媒中性无机水溶胶。制备工艺流程简单，操作简便，不使用有机分散剂和溶剂，制备成本低，制备得到的光触媒水溶胶分散性和稳定性高，适合制备光触媒浆液及涂层剂，有利于光触媒在涂覆材料领域中应用。
Description
技术领域
本发明涉及一种稳定的高分散性纳米g-C3N4/TiO2光触媒无机水溶胶制备方法。属于建筑涂层材料领域。
背景技术
纳米TiO2由于特有的表面效应、小尺寸效应、量子效应和宏观量子隧道效应，表现出独特的光电性能。其化学性质稳定，且无毒价廉，独特的颜色效应、光催化作用及紫外线屏蔽等功能，使它在涂料、化妆品、废水处理、杀菌及环保等方面有着广阔的应用前景。但纳米TiO2比表面积大、表面能高，在使用过程中极易发生粒子团聚严重影响了其应用。因此，寻求有效的分散方法是克服纳米 TiO2颗粒团聚、拓展应用领域的关键所在。近年来，有关纳米TiO2颗粒的分散研究多采用有机表面分散剂对纳米TiO2进行改性，通过产生静电稳定和空间位阻作用，提高其在水中的分散稳定性，其分散效果较好，可获得低粘度悬浮液。但由于TiO2光催化氧化作用的无选择性，导致在使用过程中容易产生对体系中的有机组分(基底)腐蚀。因此如何通过控制纳米TiO2粉体在介质中的胶体特性、悬浮液的pH值以及分散剂种类等因素制备高稳定、高分散、低粘度的悬浮液，分散剂的选取和用量是一个重要的关键因素。
目前，TiO2水溶胶主要存在两方面的问题，(1)TiO2未经掺杂改性，只能被紫外线激发而产生自洁效应，难以利用太阳光中大量的可见光；(2)溶胶制备主要采用有机钛源：钛酸丁酯、异丙醇钛等，通过水解法等实现溶胶的制备。原料成本较高、成膜后容易分解析气、以及反应时间较长等，制备效率较低，且有机溶剂对人体和环境也有一定的危害性，直接涂覆TiO2酸性溶胶会对水泥基材造成破坏。本发明利用低成本制备的石墨相氮化碳(g-C3N4)和商品纳米TiO2为原料，采用机械化学法制备得到具有可见光活性的g-C3N4/TiO2光触媒，并在此基础上制备一种高分散性g-C3N4/TiO2光触媒近中性的无机水溶胶，为解决以上问题提供一个良好方案，目前未见相关文献报道。
发明内容
针对目前制备分散良好的纳米TiO2基稳定水溶胶技术难点，本发明的目的在于提供一种简便的、低成本、高稳定、高分散、改性TiO2中性水溶胶制备方法。
制备高稳定、高分散、合适粘度的g-C3N4/TiO2悬浮液是胶态成型的关键，为实现上述目标，通过对控制粉体在介质中的胶体特性、分散剂种类和用量、pH 值及混合方式等因素，对TiO2基粉体在水中分散时进行研究，实现高分散性、高稳定性g-C3N4/TiO2水溶胶制备。
为实现本发明目的，技术方案如下：
(1)、商品纳米二氧化钛(锐钛矿)经共轭分子g-C3N4的表面杂化改性后，制备得到可见光活性的g-C3N4/TiO2光触媒；
(2)、在100ml水中依次加入分散剂六偏磷酸钠和硅酸钠，分散剂加入量为 0.1～0.5wt％，搅拌溶解完全；
(3)、在步骤(2)上述溶液中逐步加入g-C3N4/TiO2光触媒粉体，加入量为 1～3wt％，然后滴加1～3wt％的H2O2溶液，剪切乳化，进行胶溶过程；
(4)、用盐酸或氢氧化钠溶液调节悬浮液的pH至7～8，继续搅拌分散，得到 g-C3N4/TiO2光触媒水溶胶。
本发明采用改性g-C3N4/TiO2光触媒作为原料，采用无机分散剂六偏磷酸钠和硅酸钠、H2O2作为胶溶剂，制备了可见光催化活性的g-C3N4/TiO2光触媒水溶胶。试验证明，制备的g-C3N4/TiO2水溶胶光触媒活性组分分布均匀，溶胶的稳定性好，较长时间(大于3个月)存放后不会沉淀。合成的水溶胶接近中性、亲水性强、低粘度，可以很好地涂覆于建筑物表面，并且具有较好的光催化能力和自清洁性能，为建筑材料表面实现自清洁提供基础。
本发明创新点在于：1、以水作溶剂，不使用有机分散剂和溶剂，体系中不含有机成分，既降低成本又环保、安全，更加适合较大规模的生产。2、悬浮体系各组分加入顺序是：首先加入双组份分散剂六偏磷酸钠和硅酸钠，搅拌溶解完全后再逐渐加入g-C3N4/TiO2光触媒粉末，最后加入少量胶溶剂H2O2；在此过程中，分散剂种类和用量、pH值及加料顺序等均对TiO2基粉体在水中分散产生影响。纳米粒子的分散稳定性是其发挥功能的关键，本方法将纳米级改性二氧化钛微粒均匀分散在中性水溶液中，配合机械分散法加快胶溶过程，缩短分散时间，溶胶稳定且不发生团聚，操作简单，体系稳定分散效果持久，是一种方便、快捷地制备g-C3N4/TiO2水溶胶的新方法，利用此水溶胶在基片表面成膜，不经过高温处理，即可拥有较好的可见光催化活性，具有良好的去除室内VOC功能。
附图说明
图1为本发明样品接触角测量结果，图中，A-H2O、B-1wt％-g-C3N4/TiO2水溶胶、 C-3wt％-g-C3N4/TiO2水溶胶；
图2为本发明样品透射电镜照片，图中，a-TiO2、b-g-C3N4、c-3wt％-g-C3N4/TiO2、d-3wt％-g-C3N4/TiO2高分辨透射电镜照片；
图3为本发明样品XRD图谱和拉曼光谱，图中，e–本发明样品XRD图谱，f–本发明样品拉曼光谱；e图中1为g-C3N4，2为5wt％-g-C3N4/TiO2，3为TiO2； f图中，1为3wt％-g-C3N4/TiO2，2为TiO2；
图4为本发明样品紫外-可见漫反射光谱和交流阻抗谱，图中，g–本发明样品紫外-可见漫反射光谱，g图中，1为3wt％-g-C3N4/TiO2，2为TiO2；h–本发明样品交流阻抗谱；
图5为本发明样品的光触媒降解亚甲基蓝染料催化活性，图中，i–在紫外光下(15W汞灯)光触媒降解亚甲基蓝染料催化活性；j–在可见光下(500W氙灯、 420nm滤光片)光触媒降解亚甲基蓝染料催化活性。
具体实施方式
为对本发明进行更好地说明，举实施例如下：
实施例1
所述高分散性g-C3N4/TiO2光触媒无机水溶胶制备方法通过如下方法实现：
(1)、商品纳米二氧化钛(锐钛矿)经共轭分子g-C3N4的表面杂化改性后，制备得到可见光活性的g-C3N4/TiO2光触媒；
(2)、在100ml水中依次加入双组份分散剂六偏磷酸钠和硅酸钠，分散剂加入量为0.1～0.5wt％，搅拌30min溶解完全；
(3)、在步骤(2)上述溶液中逐步加入g-C3N4/TiO2光触媒粉体，加入量为 1～3wt％，滴加1～3wt％的H2O2溶液，剪切乳化10min，进行胶溶过程；
(4)、用盐酸或氢氧化钠溶液调节悬浮液的pH至7～8，继续搅拌分散30min，得到g-C3N4/TiO2光触媒水溶胶。
检测结果见表1、2、3。
表1水溶胶样品的表观粘度
| 样品名称 | 本发明3wt％-g-C3N4/TiO2 | 本发明1wt％-g-C3N4/TiO2 | H2O |
| 粘度(mPa·S) | 20～30 | 10～16 | 10～14 |
表1光触媒样品主要物性指标
表3水溶胶主要性能指标
Claims (1)
1. g-C3N4/TiO2光触媒无机水溶胶制备方法，其特征为，通过以下步骤实现：
(1)、纳米二氧化钛经共轭分子g-C3N4的表面杂化改性后，制备得到可见光活性的g-C3N4/TiO2 光触媒；
(2)、在100 ml水中依次加入双组份分散剂六偏磷酸钠和硅酸钠，分散剂加入量为0.1~0.5wt%，搅拌溶解完全；
(3)、在步骤（2）上述溶液中逐步加入g-C3N4/TiO2 光触媒粉体，加入量为1~3wt%，然后滴加1~3wt% 的H2O2溶液，剪切乳化，进行胶溶过程；
（4）、用盐酸或氢氧化钠溶液调节悬浮液的pH至7~8，继续搅拌分散，得到g-C3N4/TiO2光触媒水溶胶。
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