CN114425375B - Ni12P5/TpPa-1-COF光催化剂及其制备方法和在光催化分解水中的应用 - Google Patents
Ni12P5/TpPa-1-COF光催化剂及其制备方法和在光催化分解水中的应用 Download PDFInfo
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Abstract
本发明涉及Ni12P5/TpPa‑1‑COF及其制备方法和在光催化水分解中的应用。将Ni12P5的DMF分散液加入到TpPa‑1‑COF的反应体系中，进行溶剂热反应，所得产物离心，分别用四氢呋喃和丙酮洗涤，真空干燥，得到目标产物。将催化剂超声分散在抗坏血酸水溶液中，向溶液中通入氮气除去氧气，在可见光下(λ≥420nm)进行催化反应，可以实现在可见光下高效催化水分解制氢。
Description
技术领域
本发明属于催化制氢领域，尤其涉及Ni12P5/TpPa-1-COF光催化剂及其在光催化水分解中的应用。
背景技术
氢能以其可再生、环保和高能量密度等优点被认为是化石能源的替代品。特别是近年来，一些具有半导体特性的新材料被研究作为析氢光催化剂，如有机聚合物g-C3N4和金属-有机框架(MOFs)。共价有机框架(COFs)作为一种新兴的晶体和多孔材料，近年来表现出了良好的可见光催化产氢活性。然而，在所有的COF基光催化剂中，为了实现高析氢速率，需要使用贵金属助催化剂。因此，设计和合成无贵金属COF基高效催化H2O的光催化剂具有广阔的应用前景。
发明内容
本发明的目的是利用溶剂热反应将Ni12P5与TpPa-1-COF复合，得到一种新型材料。该材料在催化水分解制氢中具有良好的应用前景。
为了实现上述目的，本发明采用的技术方案是：Ni12P5/TpPa-1-COF光催化剂，制备方法包括如下步骤：
1)将适量Ni12P5溶于DMF中，通过超声得到均匀的黑色悬浮液；
2)将Ni12P5的DMF分散液加入到TpPa-1-COF的反应体系中，进行溶剂热反应，所得产物离心，分别用四氢呋喃和丙酮洗涤，真空干燥，得到目标产物。
上述的Ni12P5/TpPa-1-COF光催化剂，步骤1)中，所述Ni12P5晶体的制备方法包括如下步骤：取乙酸镍和PPh3，研磨均匀后放入管式炉中，抽真空后通入N2并重复若干次，进行煅烧，冷却到室温后洗涤，并真空干燥得到Ni12P5晶体。
进一步地，上述的Ni12P5/TpPa-1-COF光催化剂，步骤1)中，所述煅烧是在通N2的情况下进行的，煅烧温度为370℃，煅烧时间为1h。
进一步地，上述的Ni12P5/TpPa-1-COF光催化剂，步骤1)中，所述煅烧时的升温速率为2℃/min。
进一步地，上述的Ni12P5/TpPa-1-COF光催化剂，步骤2)中，按质量比，Ni12P5:TpPa-1-COF＝1:5
进一步地，上述的Ni12P5/TpPa-1-COF光催化剂，步骤2)中，TpPa-1-COF的反应体系为：三甲酰间苯三酚，对苯二胺和乙酸水溶液的混合体系。
进一步地，上述的Ni12P5/TpPa-1-COF光催化剂，步骤2)中，所述溶剂热反应是，于120℃下加热72h。
上述的Ni12P5/TpPa-1-COF光催化剂在光催化水分解制氢中的应用。
进一步地，上述的应用，方法如下：将Ni12P5/TpPa-1-COF光催化剂超声分散于溶有牺牲剂的水溶液中，向溶液中通入氮气除去氧气，在可见光下进行催化反应。
进一步地，上述的应用，所述牺牲剂为抗坏血酸。
本发明的有益效果是：通过简单的磷化法合成Ni12P5，利用溶剂热法在DMF的Ni12P5分散溶液中原位生长TpPa-1-COF。制备得到了一种具有良好光催化活性的催化剂Ni12P5/TpPa-1-COF，该催化剂可以实现在可见光下高效催化水分解制氢。
附图说明
图1是TpPa-1-COF与Ni12P5/TpPa-1-COF复合物的固体紫外-可见漫反射光谱图。
图2是Ni12P5/TpPa-1-COF复合物的透射电子显微镜图(a)和高分辨透射电子显微镜图(b)。
图3是可见光下(λ≥420nm)Ni12P5/TpPa-1-COF复合物催化水分解制氢示意图。
图4是可见光下(λ≥420nm)TpPa-1-COF,Ni12P5/TpPa-1-COF催化水分解产氢对比图。
具体实施方式
实施例1
(一)Ni12P5纳米颗粒的制备
将385mg乙酸镍和2360mg PPh3，在研钵中仔细研磨均匀，放在小坩埚中。将小坩埚放入管式炉，抽真空后通入N2并重复这个步骤两次，在通N2的情况下，以2℃/min是升温速率升温至370℃，并在370℃下进行煅烧，时间1h。冷却到室温后用甲苯和乙醇先后各洗涤产物三次，并真空干燥24h，得到15mg黑色产物Ni12P5纳米颗粒。
(二)Ni12P5/TpPa-1-COF的制备方法如下
向史朗克真空管中加入63mg三甲酰间苯三酚(Tp)，48mg对苯二胺(Pa-1)和0.5ml3M乙酸水溶液，将22.2mg Ni12P5分散到3ml DMF中，超声均匀后，加入到管中。混合均匀后进行三次冻融脱气循环。随后将史朗克真空管置于烘箱中120℃条件下反应72h。冷却至室温后过滤以获得产物，并使用四氢呋喃对产物进行洗涤。使用无水丙酮浸泡所得产物72h，期间更换丙酮6次。将所得Ni12P5/TpPa-1-COF在真空条件下干燥。
对比例TpPa-1-COF的制备
将63mgTp，48mg Pa-1加入史朗克真空管中，超声30min。超声结束后依次加入3mlDMF，0.5ml 3M乙酸，混合均匀后进行三次冻融脱气循环。随后将史朗克真空管置于烘箱中120℃条件下反应72h。冷却至室温后过滤以获得产物，并使用四氢呋喃对产物进行洗涤。使用无水丙酮浸泡所得产物72h，期间更换丙酮6次。将所得TpPa-1-COF真空干燥。
检测结果
图1是TpPa-1-COF和Ni12P5/TpPa-1-COF的固体紫外-可见漫反射光谱。通过对比TpPa-1-COF和Ni12P5/TpPa-1-COF的光谱图可以确定Ni12P5与TpPa-1-COF的复合有效拓宽了TpPa-1-COF对可见光的吸收范围。
图2是Ni12P5/TpPa-1-COF复合物的透射电子显微镜图(a)和高分辨透射电子显微镜图(b)。由图2中(a)可以看出，Ni12P5的粒径较小，约为10nm左右，TpPa-1-COF的形貌为由纳米棒组成的花朵状的团簇。Ni12P5纳米颗粒均匀的分散在TpPa-1-COF表面，并与TpPa-1-COF紧密结合。如图2中(b)可以看出，所测的晶格条纹之间的距离约为0.1858nm，对应于Ni12P5的(312)晶面。
实施例2 Ni12P5/TpPa-1-COF光催化剂催化水分解制氢
方法如下：该反应在石英反应器中进行，以300W氙灯作为光源模拟太阳光。将催化剂Ni12P5/TpPa-1-COF(10mg)超声分散于100mL浓度为0.005M抗坏血酸的水溶液中，向反应体系中通入高纯氮气30分钟以除去氧气，然后在可见光(λ≥420nm)照射下反应6h。在反应过程中采用气相色谱法每30分钟检测一次生成氢气的量。参比实验中，以TpPa-1-COF代替Ni12P5/TpPa-1-COF作为催化剂。
图3是可见光下Ni12P5/TpPa-1-COF光催化剂催化水分解制氢示意图。实验结果如图4，当TpPa-1-COF作催化剂时，6h产氢量仅为0.9884mmol·g-1。而Ni12P5/TpPa-1-COF作催化剂时，催化活性显著提高，产氢量随着反应时间的增加呈线性上升，反应6h未见活性衰减，6h产氢总量高达12.08mmol·g-1。由此可见，当Ni12P5与TpPa-1-COF复合后，Ni12P5作为一种有效的非贵金属助催化剂，可以极大地促进光生电子从COF向Ni12P5的转移，Ni12P5/TpPa-1-COF的催化活性高、稳定性好、制备方法简单，在光催化水分解制氢领域具有良好的应用前景。
Claims (6)
1.Ni12P5/TpPa-1-COF光催化剂，其特征在于，制备方法包括如下步骤：
1)将适量Ni12P5溶于DMF中，通过超声得到均匀的黑色悬浮液；
2)将Ni12P5的DMF分散液加入到TpPa-1-COF的反应体系中，进行溶剂热反应，所得产物离心，分别用四氢呋喃和丙酮洗涤，真空干燥，得到目标产物；
步骤1)中，所述Ni12P5晶体的制备方法包括如下步骤：取乙酸镍和PPh3，研磨均匀后放入管式炉中，抽真空后通入N2并重复若干次，进行煅烧，冷却到室温后洗涤，并真空干燥得到Ni12P5晶体；
步骤1)中，所述煅烧是在通N2的情况下进行的，煅烧温度为370℃，煅烧时间为1h；
步骤2)中，按质量比，Ni12P5:TpPa-1-COF＝1:5；
步骤2)中，TpPa-1-COF的反应体系为：三甲酰间苯三酚，对苯二胺和乙酸水溶液的混合体系。
2.根据权利要求1所述的Ni12P5/TpPa-1-COF光催化剂，其特征在于，步骤1)中，所述煅烧时的升温速率为2℃/min。
3.根据权利要求2所述的Ni12P5/TpPa-1-COF光催化剂，其特征在于，步骤2)中，所述溶剂热反应是，于120℃下加热72h。
4.权利要求1所述的Ni12P5/TpPa-1-COF光催化剂在光催化水分解制氢中的应用。
5.根据权利要求4所述的应用，其特征在于，方法如下：将权利要求1所述的Ni12P5/TpPa-1-COF光催化剂超声分散于溶有牺牲剂的水溶液中，向溶液中通入氮气除去氧气，在可见光下进行催化反应。
6.根据权利要求5所述的应用，其特征在于，所述牺牲剂为抗坏血酸。
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