CN111151302A - 一种共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备方法 - Google Patents
一种共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备方法 Download PDFInfo
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Abstract
本发明涉及一种共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备,包括步骤:硫化镉纳米棒的制备、共价有机框架材料COF(TpPa‑2)的制备和共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备。本发明的有益效果是:该制备方法较为简单,制备条件容易控制,所制备的共价有机框架材料掺杂棒状硫化镉复合光催化剂具有无污染,催化效率高等优点,具有一定的应用价值。
Description
技术领域
本发明属于纳米材料制备及应用技术领域,涉及一种共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备方法。
背景技术
多孔材料的发展经历了从无机多孔材料到有机-无机杂化多孔材料,发展到近年来成为研究前沿之一的有机多孔材料,多孔材料由于其独特的孔结构性质,在气体储存与分离、多相催化、药物释放、能量储存、光电材料和化学传感器等应用领域引起了人们的广泛关注。多孔材料按照不同的分类标准,可以分为微孔、介孔和大孔材料,无机多孔材料、有机多孔材料和有机-无机杂化多孔材料以及无定形、结晶性多孔材料等。近几十年来,由于对材料性能要求的不断提升,传统的无机多孔材料如活性炭、沸石、介孔硅以和多孔石墨烯等已经无法满足人们日益发展的能源和环境需求,科学工作者们对多孔材料研究的重心逐渐转移到新型有机多孔材料的开发上来。相比于传统无机多孔材料的难以功能化和无机-有机杂化多孔材料较差的稳定性,有机多孔材料的出现非常好地弥补了这些缺陷。
共价有机框架材料(Covalent Organic Frameworks,COFs),利用有机小分子基于动态共价键聚合形成有序规整的结晶性聚合物。COFs是一类新型多孔有序的有机聚合物,将刚性构件与二维(2D)或三维(3D)结构通过动态共价键连接,形成具有可预测拓扑结构的结晶性有机多孔材料。COFs可以通过改变构筑单元来精准调节孔的大小、结构以及相应功能。由于结晶性的COFs材料与传统的无定型多孔材料相比具有很多优点,使其成为研究的热点,在多孔材料当中占有着非常重要的地位。在各种类型的半导体光催化剂中,具有适当带隙(2.4eV)的硫化镉为了克服光生载流子快速复合和光致腐蚀等缺点,在改性研究方面进行了许多研究,包括复合其他半导体材料。
本发明拟采用高度稳定的COF(TpPa-2)作为用于负载硫化镉纳米棒的基质,COFs的p-π共轭2D晶体框架可以有效地帮助有效的电荷转移,从而稳定纳米颗粒并最终抑制纳米颗粒的重组。通过溶剂热法来制备一种共价有机框架材料掺杂棒状硫化镉复合光催化剂,所制备的光催化剂表现出显著增强的染料降解效率。
发明内容
本发明要解决的技术问题是:基于上述问题,本发明提供一种共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备方法。
本发明解决其技术问题所采用的一个技术方案是:一种共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备方法,包括以下步骤:
(1)硫化镉纳米棒的制备:将4.66 g Cd(NO3)2·4H2O与3.45 g硫脲同时溶于70 mL乙二胺中,在室温下搅拌30 min。将上述混合物转移到聚四氟乙烯内衬不锈钢高压釜中,在160℃下持续反应24 h,当反应釜冷却至室温后,用去离子水和无水乙醇反复洗涤所得产物,并在60 ℃下干燥8 h。
(2)共价有机框架材料COF(TpPa-2)的制备:在50 mL schlenk管加入均三甲苯和二恶烷溶剂混合溶剂,加入63 mg 1,3,5-三甲醛基间苯三酚和61 mg 2,5-二甲基对苯二胺,超声30min使其分散均匀,在0.5 mL的3M乙酸存在下,反应温度在120℃下进行72小时,回收产物用DMF和丙酮洗涤,60℃下干燥12小时。
(3)共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备:准确称取的步骤(1)所制备硫化镉和步骤(2)制备的COF(TpPa-2)材料,分别加入到20mL无水乙醇中,超声1 h。悬浮液在室温下搅拌1 h,将硫化镉悬浮液逐滴滴加到COF(TpPa-2)悬浮液中,超声1 h后室温下搅拌24 h。离心收集,用水和乙醇依次清洗,最后将所得产物在60 ℃下干燥24小时即所制得的共价有机框架材料掺杂棒状硫化镉复合光催化剂。
进一步地,所述的步骤(2)中1,3,5-三甲醛基间苯三酚与2,5-二甲基对苯二胺的摩尔比为2:3。
进一步地,所述的步骤(2)中均三甲苯和二恶烷溶剂混合溶剂的体积比为1:1。
进一步地,所述的步骤(3)中COF(TpPa-2):硫化镉质量比分别为40 wt%~60 wt%。
本发明的有益效果是:该制备方法较为简单,制备条件容易控制,所制备的共价有机框架材料掺杂棒状硫化镉复合光催化剂具有无污染,催化效率高等优点,具有一定的应用价值。
附图说明
下面结合附图对本发明进一步说明。
图1是本发明实施例1制备得到的共价有机框架材料掺杂棒状硫化镉复合光催化剂的扫描电镜图;
图2是本发明实施例1制备得到的共价有机框架材料掺杂棒状硫化镉复合光催化剂的X射线衍射图;
图3是本发明实施例1制备得到的共价有机框架材料掺杂棒状硫化镉复合光催化剂降解孔雀石绿(MG)的活性图。
具体实施方式
现在结合具体实施例对本发明作进一步说明,以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例1
(1)硫化镉纳米棒的制备:将4.66 g Cd(NO3)2·4H2O与3.45 g硫脲同时溶于70 mL乙二胺中,在室温下搅拌30 min。将上述混合物转移到聚四氟乙烯内衬不锈钢高压釜中,在160℃下持续反应24 h,当反应釜冷却至室温后,用去离子水和无水乙醇反复洗涤所得产物,并在60 ℃下干燥8 h。
(2)共价有机框架材料COF(TpPa-2)的制备:在50 mL schlenk管加入均5 mL三甲苯和5 mL二恶烷溶剂混合溶剂,加入63 mg 1,3,5-三甲醛基间苯三酚和61 mg 2,5-二甲基对苯二胺,超声30min使其分散均匀,在0.5 mL的3M乙酸存在下,反应温度在120℃下进行72小时,回收产物用DMF和丙酮洗涤,60℃下干燥12小时。
(3)共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备:准确称取步骤(1)制备的硫化镉0.1 g和步骤(2)制备的COF(TpPa-2)材料0.04 g,分别加入到20mL无水乙醇中,超声1 h。悬浮液在室温下搅拌1 h,将硫化镉悬浮液逐滴滴加到COF(TpPa-2)悬浮液中,超声1 h后室温下搅拌24 h。离心收集,用水和乙醇依次清洗,最后将所得产物在60 ℃下干燥24小时即所制得的共价有机框架材料掺杂棒状硫化镉复合光催化剂。
实施例2
(1)硫化镉纳米棒的制备:将4.66 g Cd(NO3)2·4H2O与3.45 g硫脲同时溶于70 mL乙二胺中,在室温下搅拌30 min。将上述混合物转移到聚四氟乙烯内衬不锈钢高压釜中,在160℃下持续反应24 h,当反应釜冷却至室温后,用去离子水和无水乙醇反复洗涤所得产物,并在60 ℃下干燥8 h。
(2)共价有机框架材料COF(TpPa-2)的制备:在50 mL schlenk管加入均5 mL三甲苯和5 mL二恶烷溶剂混合溶剂,加入63 mg 1,3,5-三甲醛基间苯三酚和61 mg 2,5-二甲基对苯二胺,超声30min使其分散均匀,在0.5 mL的3M乙酸存在下,反应温度在120℃下进行72小时,回收产物用DMF和丙酮洗涤,60℃下干燥12小时。
(3)共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备:准确称取步骤(1)制备的硫化镉0.1 g和步骤(2)制备的COF(TpPa-2)材料0.06g,分别加入到20mL无水乙醇中,超声1 h。悬浮液在室温下搅拌1 h,将硫化镉悬浮液逐滴滴加到COF(TpPa-2)悬浮液中,超声1 h后室温下搅拌24 h。离心收集,用水和乙醇依次清洗,最后将所得产物在60 ℃下干燥24小时即所制得的共价有机框架材料掺杂棒状硫化镉复合光催化剂。
实施例1-2所制备的共价有机框架材料掺杂棒状硫化镉复合光催化剂的扫描电镜图如图1所示。从图1可以看出,本实施方式制备的共价有机框架材料掺杂棒状硫化镉复合光催化剂的形貌为多孔结构表面包覆棒状硫化镉,且分布较为均匀。
实施例1-2所制备的共价有机框架材料掺杂棒状硫化镉复合光催化剂的X射线衍射图谱如图2所示。本发明制备的共价有机框架材料掺杂棒状硫化镉复合光催化剂的XRD衍射图中可看到在24.81˚,26.51˚,28.18˚,36.62˚和43.68˚是CdS的特征衍射峰。由于与硫化镉相比,共价有机框架材料用量的相对较少,在混合物中未观察到对应于共价有机框架材料COF(TpPa-2)的(100)面的强烈衍射峰。由于COF(TpPa-2)的衍射峰宽而强烈,因此可以证明硫化镉与COF(TpPa-2)复合在一起,并且未改变自身晶型。
用所制备的共价有机框架材料掺杂棒状硫化镉复合光催化剂来催化降解孔雀石绿(MG)溶液,按照下述步骤进行:
分别称取20 mg不同催化剂放入试管中,加入50 mL 20mg/L MG溶液,用带有420 nm滤光片的500 W氙灯作为光源,进行光催化降解反应。暗反应时间为1h ,光照以后,每隔20min取次样,并在5000 rpm 条件下高速离心,取上层清液用紫外可见分光光度计测其浓度变化。由图3可见,在120分钟内孔雀石绿降解率以达到97%,可见所制备的共价有机框架材料掺杂棒状硫化镉复合光催化剂具有较高的光催化活性。
以上述依据本发明的理想实施例为启示,通过上述的说明内容,相关工作人员完全可以在不偏离本项发明技术思想的范围内,进行多样的变更以及修改。本项发明的技术性范围并不局限于说明书上的内容,必须要根据权利要求范围来确定其技术性范围。
Claims (4)
1.一种共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备方法,其特征在于,包括以下步骤:
(1)硫化镉纳米棒的制备:将4.66 g Cd(NO3)2·4H2O与3.45 g硫脲同时溶于70 mL乙二胺中,在室温下搅拌30 min;将上述混合物转移到聚四氟乙烯内衬不锈钢高压釜中,在160℃下持续反应24 h,当反应釜冷却至室温后,用去离子水和无水乙醇反复洗涤所得产物,并在60 ℃下干燥8 h;
(2)共价有机框架材料COF(TpPa-2)的制备:在50 mL schlenk管加入均三甲苯和二恶烷溶剂混合溶剂,加入63 mg 1,3,5-三甲醛基间苯三酚和61 mg 2,5-二甲基对苯二胺,超声30min使其分散均匀,在0.5 mL的3M乙酸存在下,反应温度在120℃下进行72小时,回收产物用DMF和丙酮洗涤,60℃下干燥12小时;
(3)共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备:准确称取的步骤(1)所制备硫化镉和步骤(2)制备的COF(TpPa-2)材料,分别加入到20mL无水乙醇中,超声1 h,悬浮液在室温下搅拌1 h,将硫化镉悬浮液逐滴滴加到COF(TpPa-2)悬浮液中,超声1 h后室温下搅拌24 h;离心收集,用水和乙醇依次清洗,最后将所得产物在60 ℃下干燥24小时即所制得的共价有机框架材料掺杂棒状硫化镉复合光催化剂。
2.根据权利要求1所述的一种共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备方法,其特征是:所述的步骤(2)中1,3,5-三甲醛基间苯三酚与2,5-二甲基对苯二胺的摩尔比为2:3。
3.根据权利要求1所述的一种共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备方法,其特征是:所述的步骤(2)中均三甲苯和二恶烷溶剂混合溶剂的体积比为1:1。
4.根据权利要求1所述的一种共价有机框架材料掺杂棒状硫化镉复合光催化剂的制备方法,其特征是:所述的步骤(3)中COF(TpPa-2):硫化镉质量比分别为40 wt%~60 wt%。
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