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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