CN105271417B - 一种油溶性二硫化钨纳米微粒的制备方法 - Google Patents
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Abstract
本发明公开了一种油溶性二硫化钨纳米微粒的制备方法,其以二硫代钨酸铵为单源前驱体,在表面修饰剂存在条件下于180‑400℃恒温反应30分钟以上获得;其中,表面修饰剂为碳原子数在6~40之间的直链、或支链脂肪酸或脂肪胺中的至少一种。本发明方法在反应体系中不引入任何需要除去的离子,反应副产物仅为氨气,氧气和水蒸气,无有毒污染物排放。本制备方法具有工艺、设备简单、原料廉价易得、成本低,产率高等特点,适合大规模的工业生产。所制备出的二硫化钨纳米微粒粒径均一,具有良好的油溶性,在润滑油纳米添加剂等领域具有广阔的应用前景。
Description
技术领域
本发明属于新型功能纳米材料制备技术领域,具体涉及一种油溶性二硫化钨纳米微粒的制备方法。
背景技术
二硫化钨纳米微粒在润滑材料、催化剂等领域具有广泛的用途。目前其制备主要是以通过焙烧热分解四硫代钨酸铵来制备二硫化钨纳米微粒(Chem. Mater., 2011, 23(17), pp 3879–3885、Advanced Materials, 200113(4), pp283–286、ChemicalCommunications, 2003 (8): 980-981.)。这种制备方法的主要缺点是热解中间体四硫代钨酸铵的过程中生成无色、剧毒、酸性硫化氢气体,不仅对操作人员造成危害,而且还对环境造成极大的污染。另一个制约纳米微粒应用的技术瓶颈是其分散性,这是由于纳米微粒表面能高,易团聚、难以在液体介质中分散,从而制约了其大规模的应用。
发明内容
本发明目的在于克服现有技术缺陷,提供一种反应条件温和、操作简便安全、适合规模化生产的油溶性二硫化钨纳米微粒的制备方法,制得的二硫化钨纳米微粒纯度高、在有机溶剂中具有良好的分散性、稳定性。
为实现上述目的,本发明采用如下技术方案:
一种油溶性二硫化钨纳米微粒的制备方法,其以二硫代钨酸铵为单源前驱体,在表面修饰剂存在条件下于180-400℃恒温反应30分钟以上获得;其中,表面修饰剂为碳原子数在6~40之间的直链、或支链脂肪酸或脂肪胺中的至少一种。
单源前驱体二硫代钨酸铵和表面修饰剂有一定的添加范围,否则制备不出二硫化钨或者制备出来的二硫化钨难以分散。具体的,二硫代钨酸铵与表面修饰剂的添加比例为1g:3-50g。
所涉及的合成工艺如下所示:
所涉及的化学方程式如下所示:
本发明方法以二硫代钨酸铵为单源前驱体同时提供钨源和硫源,在表面修饰剂存在条件下加热分解二硫代钨酸铵即得到所述的油溶性二硫化钨纳米微粒。在反应体系中不引入任何需要除去的阴离子,反应副产物仅为氧气、氨气和水蒸汽,可轻易除去,极大地降低了制备成本。相较于现有的普遍采用高温热解四硫代钨酸铵的制备方法,避免了剧毒硫化氢气体的放出,提供了制备油溶性二硫化钨纳米微粒的一种新思路。
本发明制备方法反应条件温和、操作简便安全、对环境无污染,具有工艺设备简单、原料廉价易得、成本低,产率高等特点,适合大规模的工业化生产。所制备出的二硫化钨纳米微粒粒径均一,具有良好的油溶性,在润滑油纳米添加剂等领域具有广阔的应用前景。
附图说明
图1为实施例1制得的油溶性二硫化钨纳米微粒的XRD图;
图2为实施例1制得的油溶性二硫化钨纳米微粒的XPS图;
图3为实施例1制得的油溶性二硫化钨纳米微粒的TEM图。
具体实施方式
以下结合实施例对本发明的技术方案作进一步地详细介绍,但本发明的保护范围并不局限于此。
实施例1
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵,20g油胺,10g十八烯,将上述混合液加热到360℃,恒温反应1h。然后用乙醇和正己烷离心洗涤产物,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
制得的油溶性二硫化钨纳米微粒的XRD图见图1。图中,32.765°,49.687°,58.424°处的衍射峰与二硫化钨的标准卡片相完全一致(JCPDF卡片号,08-0237),分别对应二硫代钨酸铵的特征衍射晶面(100),(105),(1 1 0)。说明所制备的二硫化钨成功的制备,且为二维片层结构。
制得的油溶性二硫化钨纳米微粒的XPS图见图2。图中W4f5/2 和W4f7/2分别对应为二硫化钨,同时S2p3/2的峰位同样证明了二硫化钨的成功制备,和图1所证明的结论一致。说明通过二硫代钨酸铵的热解可以成功制备出二硫化钨,且产品纯度较高,无任何杂质的出现。
制得的油溶性二硫化钨纳米微粒的透射电子显微镜图见图3。由图3可以看出,所制备的二硫化钨纳米微粒粒径均匀,平均粒径约为16nm。高分辨图像表明所合成的样品结晶良好且为片层结构。在聚α烯烃6基础油和酯类油癸二酸二异辛酯中,分别配置油溶性WS2纳米微粒添加浓度3.0wt% 的溶液,静置2个月未见沉淀析出。
实施例2
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵和20g油酸,将上述混合液加热到360℃,恒温反应40分钟。然后用乙醇和正己烷离心洗涤产物,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
实施例3
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵和20g十八胺,将上述混合液加热到360℃,恒温反应1h。然后用乙醇和正己烷离心洗涤产物,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
实施例4
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵和20g油胺,将上述混合液加热到330℃,恒温反应1h。然后用乙醇和正己烷离心洗涤产物,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
实施例5
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵,20g油胺,10g十八烯,将上述混合液加热到330℃,恒温反应1h。然后用乙醇和正己烷混合液离心洗涤,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
实施例6
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵,20g油酸,10g十八烯,将上述混合液加热到360℃,恒温反应30分钟。然后用乙醇和正己烷混合液离心洗涤,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
实施例7
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵,26g十九酸和4g油胺,将上述混合液加热到360℃,恒温反应1h。然后用乙醇和正己烷混合液离心洗涤,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
实施例8
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵,20g十六酸,将上述混合液加热到360℃,恒温反应1h。然后用乙醇和正己烷混合液离心洗涤,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
实施例9
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵,20g十七胺,将上述混合液加热到280℃,恒温反应1h。然后用乙醇和正己烷混合液离心洗涤,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
实施例10
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵,20g油胺和10g油酸,将上述混合液加热到400℃,恒温反应40分钟。然后用乙醇和正己烷混合液离心洗涤,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
实施例11
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵,20g正辛胺,将上述混合液加热到360℃,恒温反应1h。然后用乙醇和正己烷混合液离心洗涤,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
实施例12
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵,20g油胺和10g十八胺,将上述混合液加热到400℃,恒温反应40分钟。然后用乙醇和正己烷混合液离心洗涤,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
实施例13
一种油溶性二硫化钨纳米微粒的制备方法,具体为:
在500ml烧瓶中加入4g二硫代钨酸铵,20g十八胺和10g油酸,将上述混合液加热到400℃,恒温反应1h。然后用乙醇和正己烷混合液离心洗涤,得到的黑色固体即为目标产物油溶性二硫化钨纳米微粒。
上述实施例2至13制得的油溶性二硫化钨纳米微粒经XRD、XPS和透射电子显微镜检测发现:所得产物纯度较高,确实为二硫化钨纳米微粒,且尺寸均匀,平均粒径在16nm左右,呈二维片层结构。在聚α烯烃6基础油和酯类油癸二酸二异辛酯中,分别配置油溶性WS2纳米微粒添加浓度3.0wt% 的溶液,静置2个月未见沉淀析出。
Claims (1)
1.一种油溶性二硫化钨纳米微粒的制备方法,其特征在于,以二硫代钨酸铵为单源前驱体,在表面修饰剂存在条件下于180-400℃恒温反应30分钟以上获得;其中,表面修饰剂为碳原子数在6~40之间的直链、或支链脂肪酸或脂肪胺中的至少一种;
二硫代钨酸铵与表面修饰剂的添加比例为1g:3-50g。
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