CN115010952B - 一种类梭形MIL-101(Fe)二十面体的制备方法及其光催化性能 - Google Patents
一种类梭形MIL-101(Fe)二十面体的制备方法及其光催化性能 Download PDFInfo
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Abstract
本发明公开一种类梭形MIL‑101(Fe)二十面体的制备方法及其光催化性能,类梭形MIL‑101(Fe)的制备特点是以N,N‑二甲基甲酰胺DMF为溶剂,加入六水合氯化铁、对苯二甲酸和一定量的乙酸,溶剂热反应后离心洗涤干燥,即可制备出类梭形MIL‑101(Fe)光催化剂。催化剂制备方法环保,简单,成本低廉,产品纯净,在可见光下利用过硫酸盐高级氧化工艺能够很好去除水中有机污染物,催化剂具有良好的应用前景。
Description
技术领域
本发明涉及一种光催化剂领域,具体是一种类梭形MIL-101(Fe)二十面体的制备方法及其光催化性能。
背景技术
金属有机框架(MOFs)是一种以多齿有机配体为连接体,以无机金属离子或金属氧簇为节点构建的多孔杂化材料。MOFs基材料由于具有比表面积大、化学稳定性好、孔隙率高和活性位点分布均匀等独特性质,已被应用于许多领域,如气体储存、药物输送、催化和分离。由于Fe在地壳矿物中含量丰富,而且环境友好,通常是催化反应的活性中心,因此,铁基MOFs(Fe-MOFs)备受关注。
刘建新等人报道了一种纺锤状MIL-101(Fe)(申请公布号:CN113292734A),其通过改变N,N-二甲基甲酰胺(DMF)和水的比例控制MIL-101(Fe)的形貌;刘宏利等人报道了一种多孔纳米线型的MIL-101(Fe)(申请公布号:CN112934271A),其通过在合成MIL-101(Fe)的前驱液中加入多元醇来调节MIL-101(Fe)的形貌。
调研表明,迄今尚未有类梭形MIL-101(Fe)作为活化过硫酸盐光催化材料的报道。
发明内容
本发明的目的在于提供一种类梭形MIL-101(Fe)二十面体的制备方法及其光催化性能及其光催化性能,通过采用乙酸当作调节剂,经过简单的溶剂热反应,制备了类梭形MIL-101(Fe)光催化剂,其具有优异的光催化性能,另一方面,乙酸当作竞争配体配位到MIL-101(Fe)中,与用乙酸调控之前的MIL-53(Fe)相比,我们所合成的类梭形MIL-101(Fe)光催化剂的活性,提高了3.03倍,类梭形MIL-101(Fe)具有良好的应用前景。
本发明的目的可以通过以下技术方案实现:
一种类梭形MIL-101(Fe)二十面体的制备方法,所述制备方法包括以下步骤:
步骤一:室温下,将六水合氯化铁和对苯二甲酸加入盛有DMF溶液的烧杯中,搅拌5分钟后得到第一混合溶液。
步骤二:在第一混合溶液中加入乙酸后进行搅拌,搅拌10分钟至溶解均匀,得到第二混合溶液。
步骤三:将第二混合溶液转移到聚四氟乙烯内衬中,洗涤、离心、干燥,得到产物为类梭形MIL-101(Fe)。
进一步的,所述第二混合溶液转移到聚四氟乙烯内衬中,在170℃恒温溶剂热反应24小时。
进一步的,所述类梭形MIL-101(Fe)的光催化性能检测将纯相不规则MIL-53(Fe)和类梭形MIL-101(Fe)光催化剂降解含有TC-HCL的抗生素废水溶液,分别加入TC-HCL水溶液,避光搅拌30min,加入过硫酸钠,之后开启氙灯光源在可见光照射下。
进一步的,所述光催化性能将不规则MIL-53(Fe)和类梭形MIL-101(Fe)光催化剂进行催化降解反应,上清液用分光光度计检测,根据Lambert–Beer定律,有机物特征吸收峰强度的变化,定量计算其浓度变化。
本发明的有益效果:
1、本发明类梭形MIL-101(Fe)光催化剂材料,制备方法简易、成本低廉、形貌均匀;
2、本发明类梭形MIL-101(Fe)光催化剂材料在可见光下利用过硫酸盐高级氧化工艺能够很好降解盐酸四环素(TC-HCL)废水溶液。
附图说明
下面结合附图对本发明作进一步的说明。
图1是本发明光催化剂的X射线衍射(XRD)图;
图2是本发明MIL-53(Fe)为不规则形貌;
图3是本发明类梭形MIL-101(Fe)光催化剂形貌;
图4是本发明不规则MIL-53(Fe)和类梭形MIL-101(Fe)光催化剂对盐酸四环素(TC-HCL)抗生素废水溶液降解活性的对比图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
一种类梭形MIL-101(Fe)二十面体的制备方法及其光催化性能,结合图1、图3和图4所示,制备方法包括以下步骤:
步骤一:室温下,将4.05g的六水合氯化铁和1.236g的对苯二甲酸加入盛有45mLDMF溶液的烧杯中,搅拌5分钟后得到第一混合溶液。
步骤二:在第一混合溶液中加入5mL乙酸,搅拌10分钟至溶解均匀,得到第二混合溶液。
步骤三:将第二混合溶液转移到聚四氟乙烯内衬中,在170℃恒温溶剂热反应24小时,之后经过洗涤、离心、干燥,得到产物为类梭形MIL-101(Fe)。
一种类梭形光催化剂的光催化性能,光催化性能检测步骤如下:
S1:分别将纯相不规则MIL-53(Fe)和类梭形MIL-101(Fe)光催化剂降解含有TC-HCL的抗生素废水溶液样品。
S2:分别称取样品各20mg,分别加入200mLTC-HCL水溶液,其中TC-HCL浓度均为40mg/L,先避光搅拌30min,使抗生素在催化剂表面达到吸附/脱附平衡。
S3:加入过硫酸钠,之后开启氙灯光源在可见光照射下,使不规则MIL-53(Fe)和类梭形MIL-101(Fe)光催化剂进行催化降解反应,上清液用分光光度计检测。
S4:根据Lambert–Beer定律,有机物特征吸收峰强度的变化,可以定量计算其浓度变化。
S5:当吸光物质相同、厚度相同时,用吸光度的变化直接表示溶液浓度的变化,因为TC-HCL在357nm处有一个特征吸收峰,所以可以利用此波长下吸光度的变化来衡量溶液中TC-HCL的浓度变化。
如图4所示,(图4中的横坐标为可见光光照射时间;纵坐标为经过可见光光照射一段时间后测量的TC-HCL浓度值与TC-HCL的初始浓度的比值;C0为TC-HCL的初始浓度,Ct为经过可见光照射一段时间后测量的TC-HCL浓度,t为时间),类梭形MIL-101(Fe)光催化剂的活性,相较于未处理的不规则MIL-53(Fe)提高了3.03倍,类梭形MIL-101(Fe)光催化剂能有效催化降解TC-HCL抗生素废水溶液,催化活性优于纯相不规则MIL-53(Fe)催化剂。
如图1、图2和图4所示,纯相不规则MIL-53(Fe)的制备流程:
室温下,在烧杯中,将4.05g的六水合氯化铁和1.236g的对苯二甲酸加入盛有50mLDMF溶液的烧杯中,搅拌15分钟,然后转移到聚四氟乙烯内衬中,在170℃恒温溶剂热反应24小时;洗涤、离心、干燥,产物即为不规则MIL-53(Fe)。
在本说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。
Claims (3)
1.一种类梭形MIL-101(Fe)二十面体的制备方法,其特征在于,所述制备方法包括以下步骤:
步骤一:室温下,将4.05g六水合氯化铁和1.236g对苯二甲酸加入盛有DMF溶液的烧杯中,搅拌5分钟后得到第一混合溶液;
步骤二:在第一混合溶液中加入5mL乙酸后进行搅拌,搅拌10分钟至溶解均匀,得到第二混合溶液;
步骤三:将第二混合溶液转移到聚四氟乙烯内衬中,在170℃恒温溶剂热反应24小时,洗涤、离心、干燥,得到产物为类梭形MIL-101(Fe)。
2.根据权利要求1所述的一种类梭形MIL-101(Fe)二十面体的制备方法,其特征在于,所述类梭形MIL-101(Fe)的光催化性能检测将纯相不规则MIL-53(Fe)和类梭形MIL-101(Fe)光催化剂降解含有TC-HCL的抗生素废水溶液,分别加入TC-HCL水溶液,避光搅拌30min,加入过硫酸钠,之后开启氙灯光源在可见光下照射。
3.根据权利要求2所述的一种类梭形MIL-101(Fe)二十面体的制备方法,其特征在于,所述光催化性能将不规则MIL-53(Fe)和类梭形MIL-101(Fe)光催化剂进行催化降解反应,上清液用分光光度计检测,根据Lambert–Beer定律和有机物特征吸收峰强度的变化,定量计算其浓度变化。
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