CN113292100A - 一种单层二硫化钼的制备及表面改性方法 - Google Patents
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
本发明公开了一种单层二硫化钼的制备及改性方法。其特征在于将自制钼源溶解到有机溶剂中,加入反应催化剂,并置于恒温烘箱发生反应,自然冷却后经离心、洗涤、真空烘箱干燥即可获得疏水性单层二硫化钼。本发明制得的二硫化钼借助有机物控制二硫化钼层间距,借助溶剂热法改变二硫化钼的表面性质(疏水性)。本发明首次在全有机环境中合成单层二硫化钼并对其表面改性,与反应物接触阻力较低,该方法制备过程操作简便,条件温和,成本低廉,可重复性高,具有良好的应用前景。
Description
技术领域
本发明属于二硫化钼的制备及表面改性技术领域,具体涉及在纯有机环境下将有机溶剂小分子穿插到多层二硫化钼中形成单层二硫化钼同时对其表面改性的制备方法。
背景技术
二硫化钼(MoS2)是一种层状结构的过渡金属硫化物,层与层之间通过范德华力相互堆叠,层间距为0.62nm(如Geim AK,Grigorieva I V.Van der Waalsheterostructures.Nature,2013,499(7459):419-425.),其独特的结构特点及过渡金属化学性能使其广泛应用于润滑、电池电容器、传感器、半导体以及工业催化等方面。随着研究的深入,研究者们发现少层甚至单层的亚结构二硫化钼有着优异的摩擦、润滑剂催化性能:经化学或机械方法制备的少层/单层二硫化钼材料具有更好的电催化性能及电池容量(如Lembke D,Kis A.Breakdown of High-Performance Monolayer MoS2 Transistors.ACSNano 2012,6,10070-10075.)。第二物种插层后的宽间距二硫化钼(≥0.69nm),凭借其宽的反应物分子传输通道,在传统油品加氢催化方面表现出较大的潜力。目前,少层或单层二硫化钼的制备方法如化学气相沉积法(Hong,Sungwook,Shen,et al.Chemical VaporDeposition Synthesis of MoS2 Layers from the Direct Sulfidation of MoO3Surfaces Using Reactive Molecular Dynamics Simulations.J.Phys.Chem.C,2018,122,7494-7503.)、剥落法(如Venkata Subbaiah,Saji K,Tiwari A.Atomically ThinMoS2:A Versatile Nongraphene 2D Material.Adv.Funct.Mater.2016,26,2046-2069.)、自分解法(Shi Y,Zhou W,Lu A Y,et al.van der Waals Epitaxy of MoS2 Layers UsingGraphene As Growth Templates.Nano Lett.2012,12,2784–2791.)等操作复杂,条件严苛(高温或惰性气氛保护),限制了其大规模生产。此外,现有方法制备的二硫化钼材料亲水的界面特性致使其在催化、润滑领域与有机溶剂及树脂基体相容性较差,极大影响其优异性能的发挥。目前,二硫化钼表面改性:表面有机包覆(有机小分子改性、聚合物改性)、沉淀反应包覆、插层改性等方法,即利用表面吸附或化学反应将有机改性分子集团修饰到粉体表面或通过离子交换反应、特征吸附等将离子或单体穿插入二硫化钼层间。但现有改性方法合成过程繁琐,成本较大,大范围工业化改性的研究还在试探阶段。
发明内容
本发明涉及一种简单的单层二硫化钼的制备及表面改性方法,在全有机环境下,将有机物穿插到二硫化钼层间中,调节层间距获得单层结构,同时获得具有疏水-亲油特点的界面性质,减少催化材料在有机相反应中对分子的扩散及传质限制。与其他方法相比,该方法合成步骤简单,条件温和,合成成本低,可重复性强,具有良好的应用前景。
针对本发明中单层二硫化钼制备及其改性方法,包括以下步骤:
(1)将四硫代钼酸铵溶解到有机溶剂中,均匀混合;加入催化剂,继续混合,形成均一的分散液;
(2)将上述步骤(1)中得到的分散液转移到反应釜中,升温反应;
(3)反应结束后冷却至室温,分离产物得到具有有机物插层的亲油性单层二硫化钼。
步骤(1)中的四硫代钼酸铵的制备方法按文献[无机盐工业,2007(05):12-15.]所述,自制获得。
步骤(1)中所述有机溶剂为苯胺、乙二胺及环己胺溶液中的一种或几种,所述的催化剂为尿素、硫脲中的一种或几种,所述的四硫代钼酸铵与有机溶剂及催化剂的摩尔比为1:(2~6):(1~3)。
步骤(1)中所有操作均在室温下进行,并始终保持搅拌。
步骤(2)中所述的反应釜为具有特氟龙内衬的50mL晶化釜,晶化釜的填充度为70%~80%,所述的升温反应温度为170~200℃,反应时间为10~20小时。
步骤(3)中所述的分离操作为离心、洗涤、干燥,所用清洗液为无水乙醇和去离子水。
本发明的优点在于:
1.全有机环境下合成疏水性单层二硫化钼催化材料,有机物拓宽层间距的同时控制二硫化钼的生长尺寸,得到的二硫化钼颗粒大小均匀,尺寸较小。
2.本发明制备的二硫化钼材料层间距距离大,活性位点与反应物接触及传质阻力低。
3.本发明制备的二硫化钼材料具有较好的疏水性,极大提高了二硫化钼与有机体系的相容性。
4.本发明制备的二硫化钼材料工艺简单,条件温和,生产效率高,周期短,制备过程安全,适合大批量生产,具有广阔的应用前景。
附图说明
图1为疏水性单层二硫化钼材料的X射线衍射(XRD)图。
图2为疏水性单层二硫化钼材料的扫描电镜(SEM)图。
图3为疏水性单层二硫化钼材料的透射电镜(TEM)图。
图4为疏水性单层二硫化钼材料的接触角(空气-水、空气-油)图。
图5为疏水性单层二硫化钼材料的X射线光电子能谱(XPS)图。
图6为疏水性单层二硫化钼材料的拉曼光谱(Raman)图。
具体实施方式
为使得本申请相关催化剂制备过程,特点,优势更加清晰,现将结合附图对技术方案进行完整描述。需说明的是,本发明提及的实施例为本实验部分实施例,而非全部实施例;本发明提及的原料均通过商业途径购买,未提及的操作及合成过程为本领域技术人员熟知的工艺步骤或制备方法。在任何不超出本发明的构思和范畴的改动,均在本发明范围内。
实施例1:
取3.25g四硫代钼酸铵溶解到20mL乙二胺溶剂中,混合均匀后加入1.92g硫脲作,均匀混合后转移到50mL晶化釜中,在170℃恒温烘箱中保持20小时。自然冷却后,将产物先后用无水乙醇、去离子水进行离心,洗涤五次,真空干燥后得到疏水性单层二硫化钼材料,将其记为Solvo-II-1。
实施例2:
取3.25g四硫代钼酸铵在室温下溶解到20ml环己胺溶剂中,混合均匀后加入1.92g尿素,均匀混合后转移到50mL晶化釜,在180℃恒温烘箱中保持20小时。自然冷却后,将产物先后用无水乙醇、去离子水进行离心,洗涤五次,真空干燥后得到疏水性单层二硫化钼材料,将其记为Solvo-III-1。
实施例3:
取1.625g四硫代钼酸铵在室温下溶解到20mL苯胺溶剂中,混合均匀后加入1.92g硫脲,均匀混合后转移到50mL晶化釜,在200℃恒温烘箱中保持20小时。自然冷却后,将产物先后用无水乙醇、去离子水进行离心,洗涤五次,真空干燥后得到疏水性单层二硫化钼材料,将其记为Solvo-IV-1。
对上述样品进行X射线衍射表征,由图1可以发现,三个温度段获得的二硫化钼样品均出现二硫化钼14.4°(002),33.2°(100)及58.5°(110)晶面的XRD特征衍射峰。其中(002)峰的强弱与二硫化钼堆叠层数正相关,可知得按照本发明方法得到的系列二硫化钼样品为少层或单层结构。以样品Solvo-II-1样品为典型,对样品进行了扫描电镜、透射电镜、接触角和X-射线元素分析表征及分析。
图2为Solvo-II-1样品的扫描电镜图,可以发现本发明方法合成的二硫化钼样品呈现颗粒小球状,粒径在100nm左右。
图3为Solvo-II-1样品的透射电镜图,从图3可以得知二硫化钼层间距在0.7~1.05nm,远超过二硫化钼层间距0.62nm,说明通过本发明所述合成方法,二硫化钼的层间距被拓宽,获得单层结构。
图4为Solvo-II-1样品的接触角测试,从图4可知,该方法合成的样品呈现极强的疏水性。
图5为Solvo-II-1样品的X射线光电子能谱测试,从图5可知,Solvo-II-1样品的Mo3d图谱可以分为Mo 3d3/2(231.4eV)和Mo 3d5/2(228.1eV),S 2p图谱可以分为S 2p3/2(161.4eV)与S 2p1/2(162.2eV),这都与MoS2的XPS结合能相吻合。
选择样品Solvo-II-1,Solvo-III-1,及Solvo-IV-1与多层商用二硫化钼进行拉曼光谱表征,结果如图6所示。商用二硫化钼出现拉曼振动峰E2g 1(409cm-1)及A1g(383cm-1),两峰的与二硫化钼自身的堆叠层数正相关(Advanced Functional Materials,22(2012)1385-1390;Applied Physics Letters,100(2012)1271),本发明所制的疏水性二硫化钼材料并未出现上述两个特征峰,说明上述样品的确为单层。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围内。
Claims (7)
1.一种单层二硫化钼的制备及表面改性方法,其步骤如下:
(1)将四硫代钼酸铵在室温下溶解到有机溶剂中,均匀混合;加入催化剂,继续搅拌,形成均一的分散液;
(2)将上述步骤(1)中得到的分散液转移到反应釜中,升温反应;
(3)反应结束后冷却至室温,分离产物得到疏水性单层二硫化钼材料。
2.根据权利要求1所述的一种单层二硫化钼的制备及表面改性方法,其特征在于,步骤(1)中所述有机溶剂为苯胺、乙二胺及环己胺中的一种或几种;所述的催化剂为尿素、硫脲中的一种或几种。
3.根据权利要求1所述的一种单层二硫化钼的制备及表面改性方法,其特征在于,步骤(1)中所述的四硫代钼酸铵与有机溶剂及催化剂的摩尔比为1:(2~6):(1~3)。
4.根据权利要求1所述的一种单层二硫化钼的制备及表面改性方法,其特征在于,步骤(2)中所述的反应釜为具有特氟龙内衬的50ml晶化釜,晶化釜的填充度为70%~80%。
5.根据权利要求1所述的一种单层二硫化钼的制备及表面改性方法,其特征在于,步骤(2)中所述的升温反应温度为170~200℃,反应时间为10~20小时。
6.根据权利要求1所述的一种单层二硫化钼的制备及表面改性方法,其特征在于,步骤(3)中所述的分离产物操作为离心,洗涤和干燥。
7.一种如权利要求1~6任一项所述方法制备的疏水性单层二硫化钼,其特征在于所述二硫化钼粒径在80~100nm,有机物插层后层间距在0.77~1.0nm,空气-水接触角大于100°,获得单层结构及疏水的界面特性。
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