CN111661876A - 一种花瓣状二维硫化钼纳米材料的制备方法及其应用 - Google Patents
一种花瓣状二维硫化钼纳米材料的制备方法及其应用 Download PDFInfo
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Abstract
本发明提供了一种花瓣状二维硫化钼纳米材料的制备方法及其应用,以钼酸钠二水化合物为钼源,以硫代乙酰胺为硫源,采用水热法结合真空冷冻干燥制备二维硫化钼纳米材料,制备工艺流程为:制备混合液→搅拌→水热反应→冷冻干燥→花瓣状二维硫化钼。通过以上工艺制备的二维硫化钼为花瓣状,尺寸为100nm~150nm,厚度为10nm~20nm。本发明制备的花瓣状二维硫化钼纳米材料可以高效吸附水中四环素。
Description
技术领域
本发明属于环境材料合成技术领域,具体涉及一种花瓣状二维硫化钼纳米材料的制备方法,及其吸附水体中四环素的应用。
背景技术
硫化钼作为一种近年来新兴的一种二维材料而引起了学者们的广泛研究关注,因为其具有独特的物理化学性质,所以硫化钼在电化学、材料、润滑等领域被广泛研究应用。硫化钼物理结构为六方晶系层状,层与层之间依靠微弱的范德华力连接,因此润滑性能很高,因此在润滑领域中应用较为广泛,可用作固体润滑剂。MoS2具有耐酸碱腐蚀的特性,在空气中稳定化学性质稳定,氧化温度为320℃,且不溶于有机溶剂。二维纳米硫化钼比普通硫化钼具有更优异的性质,纳米硫化钼具有更大的比表面积,较强的吸附能力,润滑能力明显提高等。因此,二维纳米硫化钼的制备研究成为了研究热点。
目前,纳米二维硫化钼的制备方法主要包括:水热法、沉积法、机械和液相剥离法、溶液法等,以及研究应用较少的模板法、超声波法、熔盐法等。
沉积法是利用高温使固体前驱体升华成气态并伴随有化学反应的发生,然后冷凝沉积在基体表面上。此方法制备出的二维硫化钼具有较好的质量,但是需要工艺较为复杂,成本比较高;机械剥离法制备的硫化钼效率较低并且质量较差;溶液法在常温常压下的设备中经过的化学反应制备出二维硫化钼,此法制备的产物中MoS2纯度低,容易有杂质。水热法成本较低,制备出的硫化钼质量较高,但硫化钼层数不易控制。
如今,抗生素对水体的污染引起了社会的广泛关注,残留在水体中的抗生素不仅会对水体生态环境造成破坏从而危害水体中生物及微生物安全,并且会随食物链进入人类身体中,最终将危害人体健康,因此减少排入水体中的抗生素量及去除水体中残留的抗生素成为了迫切需要解决的环境问题。目前已经有多种方法应用于去除水中残留的抗生素,例如光催化、吸附等方法。利用吸附剂的高效吸附能力,直接投加吸附剂到污染水体中,吸附剂有效的吸附水体中残留的抗生素,例如四环素。吸附剂比表面积大越大吸附性能相对越高。
因此,本发明在在上述背景下进一步研究,研究出一种花瓣状硫化钼纳米材料的制备方法,并研究了本方法合成的二维硫化钼对水中四环素的吸附效果。
发明内容
本发明目的之一在于以水热法为制备手段,制备出一种花瓣状二维硫化钼纳米材料,质量以及分散性较好,制备工艺步骤简单,成本较低。
本发明目的之二在于制备出的二维硫化钼可吸附水体中的四环素,且吸附效率较高。
本发明的技术方案是:
一种花瓣状二维硫化钼纳米材料的制备方法,其特征在于,包括如下步骤:
将硫代乙酰胺和钼酸钠二水化合物溶于去离子水中并搅拌混合均匀,然后将混合液转移到聚四氟乙烯衬里的高压反应釜中,并将反应釜放入烘箱中进行水热反应,反应结束后离心收集反应釜中黑色产物,并用去离子水和乙醇洗涤,然后将黑色产物用真空冷冻干燥机冷冻干燥,得到层状MoS2。
所述的硫代乙酰胺、钼酸钠二水化合物和去离子水的用量比例为0.45g:0.72g:80mL。
所述搅拌方式为磁力搅拌,搅拌时间为10min。
所述水热反应的温度为200℃,反应时间为24小时。
真空冷冻干燥的温度为-60℃,干燥时间为24小时。
本发明所述制备方法制备出的二维硫化钼形貌为花瓣状,尺寸为100nm~150nm,厚度为10nm~20nm。
本发明所述制备方法得到的二维硫化钼纳米材料用于吸附水中四环素的用途。
本发明的有益效果为:
本发明所述制备二维硫化钼纳米材料的方法,制备出的硫化钼具有质量以及分散性较好、制备工艺步骤简单、成本较低等优点。并且可以高效吸附水中的四环素。
附图说明
图1为本发明所述方法制备花瓣状二维硫化钼纳米材料的流程图;
图2为本发明二维硫化钼纳米材料的SEM图;
图3为本发明二维硫化钼纳米材料的XRD图;
图4本发明二维硫化钼纳米材料的TEM图;
图5本发明二维硫化钼纳米材料吸附四环素考察图。
具体实施方式
下面结合具体实施实例对本发明做进一步说明,一种花瓣状二维硫化钼纳米材料的制备工艺流程如图1所示。
四环素吸附活性评价:取100mL 20mg/L的四环素溶液加入反应瓶中并且避光放置,测定其初始吸光度值,取30mg样品加入反应瓶并加入一个磁子,设定反应器温度为25℃,通空气量为2mL/min,开启磁力搅拌(转速设定为700rpm/min),每间隔十分钟取一次样并通过紫外-可见分光光度计测定其吸光度,根据标准曲线(c=(A+0.00892)/0.03093)换算出四环素浓度,并通过公式:Q=(C0-C)V/m算出其吸附容量Q,其中C0为四环素的初始浓度,C为达到吸附平衡时的四环素溶液的浓度,V为溶液的体积,m为加入的样品的质量。
实施例1:
(1)称取0.45g硫代乙酰胺和0.72g钼酸钠二水加入到80ml的去离子水中,搅拌至完全溶解,形成无色透明溶液。
(2)将(1)中得到的无色透明溶液分装到两个规格为100ml的聚四氟乙烯反应釜中,每个反应釜中溶液为40ml,然后将反应釜放到烘箱中进行水热反应。烘箱温度设定为200℃,反应时间设定为24小时。
(3)烘箱冷却至室温后,将反应釜从烘箱中取出并用无水乙醇和去离子水洗涤产物,无水乙醇和去离子水至少各洗三次,将所得样品放入真空冷冻干燥箱中干燥,温度设定为-60度,干燥后取出即得到二维硫化钼。
(4)按照以上工艺制备出的二维硫化钼形貌为花瓣状,尺寸为100nm~150nm,厚度为10nm~20nm。样品的SEM图如图2所示,图中片状硫化钼呈明显弯曲,非平整二维片状,形状与花瓣类似,且大小均匀,说明材料合成成功。
XRD衍射谱图如图3所示,硫化钼峰形结构与标准卡片中PDF#77-1545对应,说明合成的材料确实是硫化钼;
TEM图如图4所示,说明合成材料厚度较薄,且单个片状硫化钼边缘较厚,黑色不透明区域为大量二维薄片叠加所的结果。
(5)考察上述工艺流程制备出的样品吸附性能,结果如图5所示,样品吸附率为70.2%。
Claims (7)
1.一种花瓣状二维硫化钼纳米材料的制备方法,其特征在于,包括如下步骤:
将硫代乙酰胺和钼酸钠二水化合物溶于去离子水中并搅拌混合均匀,然后将混合液转移到聚四氟乙烯衬里的高压反应釜中,并将反应釜放入烘箱中进行水热反应,反应结束后离心收集反应釜中黑色产物,并用去离子水和乙醇洗涤,然后将黑色产物用真空冷冻干燥机冷冻干燥,得到层状MoS2。
2.根据权利要求1所述的一种花瓣状二维硫化钼纳米材料的制备方法,其特征在于,所述的硫代乙酰胺、钼酸钠二水化合物和去离子水的用量比例为0.45g:0.72g:80mL。
3.根据权利要求1所述的一种花瓣状二维硫化钼纳米材料的制备方法,其特征在于,所述搅拌方式为磁力搅拌,搅拌时间为10min。
4.根据权利要求1所述的一种花瓣状二维硫化钼纳米材料的制备方法,其特征在于,所述水热反应的温度为200℃,反应时间为24小时。
5.根据权利要求1所述的一种花瓣状二维硫化钼纳米材料的制备方法,其特征在于,真空冷冻干燥的温度为-60℃,干燥时间为24小时。
6.一种花瓣状二维硫化钼纳米材料,其特征在于,是根据权利要求1~6任一项所述制备方法得到,二维硫化钼形貌为花瓣状,尺寸为100nm~150nm,厚度为10nm~20nm。
7.将权利要求6所述的花瓣状二维硫化钼纳米材料用于吸附水中四环素的用途。
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