CN106423218A - 一种二硫化钼/碳纳米复合材料的合成方法 - Google Patents
一种二硫化钼/碳纳米复合材料的合成方法 Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/40—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
本发明公开了一种用腐植酸精钾制备二硫化钼/碳复合材料的合成方法,属于无机非金属材料领域,将可溶性钼盐四水合钼酸铵溶于水,再向其中加入腐植酸精钾,将以上两者的混合溶液反向滴定到硝酸中,调整pH到1‑3之间,制得沉淀。然后利用熔融盐焙烧法,在氩气等惰性气氛下焙烧,发生碳热反应,制得长度在100nm左右的纳米棒负载在碳膜上的复合结构。本发明的优点在于工艺简单,成本低廉,使用生物质材料腐植酸精钾为碳源,直接合成了负载型的纳米复合结构。
Description
技术领域
本发明属于无机非金属新材料研发技术领域,具体公开一种涉及二硫化钼/碳纳米复合材料的共沉淀及熔融盐焙烧的合成方法。
背景技术
二硫化钼具有类似石墨的层状结构和稳定的物理化学性质,广泛应用于固体润滑剂、储氢材料、电池电极材料、催化材料等。纳米级二硫化钼材料,因其吸附能力强、催化反应活性高等特点被用作煤炭液化、煤炭热解、石油中加氢脱硫、除硫去氮的催化剂。但是由于纳米粒子粒度尺寸小,表面能高,粒子之间容易发生团聚,纳米材料在介质中的分散和稳定成为限制其在工业应用的主要问题之一。为了改善纳米二硫化钼粒子的团聚,近年来,石墨烯或氧化石墨烯成为人们研究的热点。目前,制备石墨烯的方法主要有机械剥离法、还原氧化石墨法、外延生长法及金属催化法等合成方法。然而,石墨烯表面呈现稳定惰性,难溶解于溶剂中,更难与其他有机或无机材料均匀地复合。因此,制备石墨烯复合材料,大多是先将氧化石墨烯与纳米材料复合,再将复合后的材料还原得到石墨烯复合材料。这种制备步骤繁琐,产物性能往往难以满足应用需求,因此,有必要开发一种直接获得石墨烯负载单分散纳米粒子的制备方法。
目前制备纳米粒子/石墨烯的主要方法有化学还原法、电化学沉积法、热蒸发法、水热法、溶胶-凝胶法等。一些研究表明,选择合适碳源和合成条件可以直接获得负载的石墨烯。腐植酸是一种天然大分子有机化合物,主要由风化煤或者褐煤采用“碱溶酸沉”的方法获得。腐植酸具有不确定的分子量,其上含有羧基、羟基、酚羟基、醌基、甲氧基等多种活性官能团。它具有良好的吸收、络合、交换等功能。
发明内容
本发明的目的是:为了证明选择合适的碳源,可以直接获得二硫化钼/碳纳米复合材料。提出了采用腐植酸精钾络合金属钼离子,进一步将其与硫酸钠混合研磨后焙烧,制备二硫化钼/碳纳米复合材料的方法。
本发明的技术方案为:一种二硫化钼/碳纳米复合材料的合成方法,该合成方法包括以下步骤:(1)配置0.25M的四水合七钼酸铵溶液40ml,再向其中加入2g腐植酸精钾,将两者混合并搅拌成混合溶液,备用;(2)配置0.5M的硝酸溶液100ml,将步骤(1)中搅拌得到的混合溶液逐滴滴加到0.5M的硝酸溶液中,调节溶液的pH为1-3之间,静置一段时间后得到沉淀物,备用;(3)将步骤(2)中制备好的沉淀物冻干,与无水硫酸钠按1:10的质量比混合研磨,在Ar气气氛下,在600℃或700℃或800℃条件下,以10℃/min的升温梯度焙烧3h,自然冷却到室温,获得二硫化钼/碳纳米复合材料的前驱体,备用;(4)将步骤(3)中得到的前驱体用水和无水乙醇各离心洗涤五遍,最后保存在无水乙醇中;将产物在50℃下干燥得到二硫化钼/碳纳米复合材料的粉体。利用腐植酸精钾“碱溶酸沉”的特点,在熔融盐焙烧体系中采用腐植酸精钾这种生物质材料作为碳源合成二硫化钼/碳纳米复合材料,所述腐植酸钾购买自新疆双龙腐植酸公司。
有益效果:本发明提供了一种直接获得二硫化钼/碳纳米复合材料的方法,利用从风化煤中提取出来的腐植酸精钾这种既廉价又高效的生物质材料作为碳源,实现最大程度的资源利用,最终达到了环境保护,资源高值化利用的目的。
附图说明
图1:本发明制备方法的T=600℃时二硫化钼/碳纳米复合材料的X射线(XRD)图谱;
图2:本发明制备方法的T=600℃时二硫化钼/碳纳米复合材料的透射电子显微镜图谱(TEM);
从图1的X射线图谱可以知道,T=600℃时得到的材料是二硫化钼/碳纳米复合材料。从图2的透射电子显微镜的图像可以看出,所得到的二硫化钼/碳纳米复合材料为100nm左右的纳米棒均匀的负载在碳膜表面上的形貌。由此看出,选择合适的碳源-腐植酸精钾,可以直接获得二硫化钼/碳纳米复合材料。
具体实施方式
实施例1、配置0.25M的(NH4)6Mo7O24·4H2O溶液40ml,再向其中加入2g腐植酸精钾,再配置0.5M的HNO3溶液100ml。在磁力搅拌的条件下,将(NH4)6Mo7O24·4H2O与腐植酸精钾混合溶液缓慢反向滴加到HNO3溶液中。将以上浑浊液静置后,吸出上层的水,然后将沉淀物进行冻干,取1g冻干后的腐植酸精钾-钼酸前驱体与10g无水硫酸钠以1:10的质量比进行混合研磨,然后在Ar气气氛下,600℃条件下,以10℃/min升温梯度焙烧3h,自然冷却到室温,再用水和乙醇分别对样品进行离心洗涤各五遍,最后将样品保存在乙醇中,50℃烘干得到硫化钼/碳纳米复合材料
实施例2、配置0.25M的(NH4)6Mo7O24·4H2O溶液40ml,再向其中加入2g腐植酸精钾,再配置0.5M的HNO3溶液100ml。在磁力搅拌的条件下,将(NH4)6Mo7O24·4H2O与腐植酸精钾混合溶液缓慢反向滴加到HNO3溶液中。将以上浑浊液静置后,吸出上层的水,然后将沉淀物进行冻干,取1g冻干后的腐植酸精钾-钼酸前驱体与10g无水硫酸钠以1:10的质量比进行混合研磨,然后在Ar气气氛下,700℃条件下,以10℃/min升温梯度焙烧3h,自然冷却到室温,用水和乙醇分别对样品进行离心洗涤各五遍,最后将样品保存在乙醇中,50℃烘干得到硫化钼/碳纳米复合材料。
实施例3、配置0.25M的(NH4)6Mo7O24·4H2O溶液40ml,再向其中加入2g腐植酸精钾,再配置0.5M的HNO3溶液100ml。在磁力搅拌的条件下,将(NH4)6Mo7O24·4H2O与腐植酸精钾混合溶液缓慢反向滴加到HNO3溶液中。将以上浑浊液静置后,吸出上层的水,然后将沉淀物进行冻干,取1g冻干后的腐植酸精钾-钼酸前驱体与10g无水硫酸钠以1:10的质量比进行混合研磨,然后在Ar气气氛下,800℃条件下,以10℃/min升温梯度焙烧3h,自然冷却到室温,再用水和乙醇分别对样品进行离心洗涤各五遍,最后将样品保存在乙醇中,50℃烘干得到硫化钼/碳纳米复合材料。
上述实验所用腐植酸钾购买自新疆双龙腐植酸公司。
结论:通过选择合适的碳源-腐植酸精钾,直接获得了二硫化钼/碳纳米复合材料,其形貌为100 nm左右的纳米棒均匀的负载在碳膜表面上。
本发明的主要技术内容是以四水合钼酸铵和廉价的腐植酸精钾混合溶液为原料,反向滴定到硝酸中,制得沉淀。再与无水硫酸钠混合研磨,利用熔融盐焙烧法,经过碳热反应,将无水硫酸钠既作为模版剂,又作为硫源,获得了100nm左右的纳米棒均匀的负载在碳膜表面上的二硫化钼/碳纳米复合材料。
Claims (2)
1.一种二硫化钼/碳纳米复合材料的合成方法,该合成方法包括以下步骤:
(1)配置0.25M四水合七钼酸铵40ml,再向其中加入2g腐植酸精钾,将两者混合并搅拌成混合溶液,备用;
(2)配置0.5 M的硝酸溶液100ml,将步骤(1)中搅拌得到的混合溶液逐滴滴加到0.5M的硝酸溶液中,调节溶液的pH为1-3之间,静置一段时间后得到沉淀物,备用;
(3)将步骤(2)中制备好的沉淀物冻干,与无水硫酸钠按1:10的质量比混合研磨,在Ar气气氛下,在600℃或700℃或800℃条件下,以10℃/min的升温梯度焙烧3h,自然冷却到室温,获得二硫化钼/碳纳米复合材料的前驱体,备用;
(4)将步骤(3)中得到的前驱体用水和无水乙醇各离心洗涤五遍,最后保存在无水乙醇中;将产物在50℃下干燥得到二硫化钼/碳纳米复合材料的粉体。
2.根据权利要求1所述的共沉淀法制备二硫化钼/碳纳米复合材料的方法,其特征在于:所述腐植酸钾购买自新疆双龙腐植酸公司。
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