CN110560107A - 一种Ni-MoS2/RGO/Ti3C2复合材料的制备方法 - Google Patents
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 16
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- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 31
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- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 7
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Abstract
本发明公开了一种Ni‑MoS2/RGO/Ti3C2复合材料的制备方法，包括将氧化石墨烯、Ti3C2纳米粉体、钼酸钠、Ni(OH)2粉末在醇溶剂中超声分散均匀，然后加入硫脲超声分散混匀，将反应液置于反应釜内进行保温反应，保温反应结束后回收中间产物，将中间产物置于加热炉内隔氧条件下进行退火处理，即可制得所述Ni‑MoS2/RGO/Ti3C2复合材料。上述制得的复合催化剂，通过氧化石墨烯、Ti3C2、MoS2组装在纳米多孔镍的外表面，形成独特的三维多孔结构的复合材料，使得催化剂的比表面积大大被提升，可促进光生载流子的有效分离，实现二硫化钼较高性能的光解水制氢性能。
Description
技术领域
本发明涉及光解水催化剂制备技术领域，具体涉及一种Ni-MoS2/RGO/Ti3C2复合材料的制备方法。
背景技术
氢能源是非常环保的新能源，目前世界各国均对光解水制氢进行了大量的研究，也制备出了各式各样的光解水催化剂。如Ni-MoS2/RGO纳米复合催化剂等等，这些新式催化剂虽然能够在一定程度上提升光催化效率，但是其提高率有限，还难以满足实际使用的需求，因此，有必要提供一种性能更为优良的催化剂的制备方法。
发明内容
本发明的目的是提供一种Ni-MoS2/RGO/Ti3C2复合材料的制备方法，其光解制氢效果好。
本发明采取的技术方案具体如下：
一种Ni-MoS2/RGO/Ti3C2复合材料的制备方法，其特征在于：
包括将氧化石墨烯、Ti3C2纳米粉体、钼酸钠、Ni(OH)2粉末在醇溶剂中超声分散均匀，然后加入硫脲超声分散混匀，将反应液置于反应釜内进行保温反应，保温反应结束后回收中间产物，将中间产物置于加热炉内隔氧条件下进行退火处理，即可制得所述Ni-MoS2/RGO/Ti3C2复合材料。
具体的方案为：
先量取12ml氨水溶液加入100ml硝酸镍水溶液中，然后在加入100ml的尿素水溶液，搅拌混匀，90℃水浴加热反应3h，反应结束后，过滤、洗涤、干燥回收得到Ni(OH)2粉末；硝酸镍水溶液和尿素素水溶液中硝酸镍与尿素的摩尔比为1:2；
将氧化石墨烯加入200ml醇溶液中，超声分散混匀，然后再加入Ti3C2纳米粉体，超声分散混匀，配制得到A溶液，A溶液中Ti3C2的含量为0.5mg/ml、氧化石墨烯的含量为3.0mg/ml；
量取30ml上述A溶液，称取2.42g的钼酸钠、2.0g Ni(OH)2粉末依次投入里面，超声分散混匀，然后加入3.5g的硫尿脲，超声分散混匀，得到混合反应液，将混合反应液转移至反应釜内进行保温反应，保温反应的温度为100℃，时间为10h，保温反应结束后，过滤、洗涤、干燥回收中间产物，然后将中间产物置于加热炉内惰性气氛或真空条件下进行退火处理，退火处理的温度为500℃，时间3h，退火处理后即可制得所述Ni-MoS2/RGO/Ti3C2复合材料。
上述制得的复合催化剂，通过氧化石墨烯、Ti3C2、MoS2组装在纳米多孔镍的外表面，形成独特的三维多孔结构的复合材料，使得催化剂的比表面积大大被提升，可促进光生载流子的有效分离，实现二硫化钼较高性能的光解水制氢性能。并且石墨烯、Ti3C2与MoS2的复合拓展了催化剂的可见光吸收范围和吸收强度，利用石墨烯优异的电子传递性能，从而大幅度降低光生电子空穴对的复合率，因而极大地提高了催化剂的光催化活性。并且，Ti3C2、MoS2、纳米多孔镍之间形成N-P异质结结构，进一步大大提高了复合材料的光催化活性，该复合光催化材料在可见光区具有较强的光吸收特性，能够高效利用自然光，高效率的进行光水解。
具体实施方式
为了使本发明的目的及优点更加清楚明白，以下结合实施例对本发明进行具体说明。应当理解，以下文字仅仅用以描述本发明的一种或几种具体的实施方式，并不对本发明具体请求的保护范围进行严格限定。
下述各实施例中，如无特别说明，所用试剂和药品均通过商业途径购买得到。
实施例1
先量取12ml氨水溶液(25％，质量浓度)加入100ml硝酸镍水溶液中，然后在加入100ml 的尿素水溶液，搅拌混匀，90℃水浴加热反应3h，反应结束后，过滤、洗涤、干燥回收得到 Ni(OH)2粉末；硝酸镍水溶液和尿素素水溶液中硝酸镍与尿素的摩尔比为1:2；
将氧化石墨烯加入200ml醇溶液(50％，质量浓度)中，超声分散混匀，然后再加入Ti3C2纳米粉体，超声分散混匀，配制得到A溶液，A溶液中Ti3C2的含量为0.5mg/ml、氧化石墨烯的含量为3.0mg/ml；
量取30ml上述A溶液，称取2.42g的钼酸钠(Na2MoO4·2H2O)、2.0g Ni(OH)2粉末依次投入里面，超声分散混匀，然后加入3.5g的硫脲，超声分散混匀，得到混合反应液，将混合反应液转移至反应釜内进行保温反应，保温反应的温度为100℃，时间为10h，保温反应结束后，过滤、洗涤、干燥回收中间产物，然后将中间产物置于加热炉内真空条件下进行退火处理，退火处理的温度为500℃，时间3h，退火处理后即可制得所述Ni-MoS2/RGO/Ti3C2复合材料。
实施例2
先量取12ml氨水溶液(25％，质量浓度)加入100ml硝酸镍水溶液中，然后在加入100ml 的尿素水溶液，搅拌混匀，90℃水浴加热反应3h，反应结束后，过滤、洗涤、干燥回收得到 Ni(OH)2粉末；硝酸镍水溶液和尿素素水溶液中硝酸镍与尿素的摩尔比为1:2；
将氧化石墨烯加入200ml醇溶液(50％，质量浓度)中，超声分散混匀，配制得到A溶液， A溶液中氧化石墨烯的含量为3.0mg/ml；
量取30ml上述A溶液，称取2.42g的钼酸钠(Na2MoO4·2H2O)、2.0g Ni(OH)2粉末依次投入里面，超声分散混匀，然后加入3.5g的硫脲，超声分散混匀，得到混合反应液，将混合反应液转移至反应釜内进行保温反应，保温反应的温度为100℃，时间为10h，保温反应结束后，过滤、洗涤、干燥回收中间产物，然后将中间产物置于加热炉内真空条件下进行退火处理，退火处理的温度为500℃，时间3h，退火处理后即可制得所述Ni-MoS2/RGO/Ti3C2复合材料。
实施例3
将上述实施例1、2制备的复合催化剂在MC-SPH2O全自动光催化全解水实验测试系统上进行性能检测。将实施例1、2中制备的复合催化剂分别组装到光解水系统中；通入高纯氮气 30min，排除反应体系中的溶解氧和管路中的空气；检查系统，打开恒温循环水，启动氙灯光源(功率300W)，用CUT400滤去紫外光，检测光照12h复合催化剂的光催化分解水制氢的活性。氢气含量采用联机气相色谱仪在线检测，TCD检测器，TDX-01气相填充柱，光解水产氢结果如表1所示。
表1催化剂的可见光光解水制氢的结果
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以作出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。本发明中未具体描述和解释说明的结构、装置以及操作方法，如无特别说明和限定，均按照本领域的常规手段进行实施。
Claims (2)
1.一种Ni-MoS2/RGO/Ti3C2复合材料的制备方法，其特征在于：
包括将氧化石墨烯、Ti3C2纳米粉体、钼酸钠、Ni(OH)2粉末在醇溶剂中超声分散均匀，然后加入硫脲超声分散混匀，将反应液置于反应釜内进行保温反应，保温反应结束后回收中间产物，将中间产物置于加热炉内隔氧条件下进行退火处理，即可制得所述Ni-MoS2/RGO/Ti3C2复合材料。
2.根据权利要求1所述Ni-MoS2/RGO/Ti3C2复合材料的制备方法，其特征在于：
先量取12ml氨水溶液加入100ml硝酸镍水溶液中，然后在加入100ml的尿素水溶液，搅拌混匀，90℃水浴加热反应3h，反应结束后，过滤、洗涤、干燥回收得到Ni(OH)2粉末；硝酸镍水溶液和尿素素水溶液中硝酸镍与尿素的摩尔比为1:2；
将氧化石墨烯加入200ml醇溶液中，超声分散混匀，然后再加入Ti3C2纳米粉体，超声分散混匀，配制得到A溶液，A溶液中Ti3C2的含量为0.5mg/ml、氧化石墨烯的含量为3.0mg/ml；
量取30ml上述A溶液，称取2.42g的钼酸钠、2.0g Ni(OH)2粉末依次投入里面，超声分散混匀，然后加入3.5g的硫尿脲，超声分散混匀，得到混合反应液，将混合反应液转移至反应釜内进行保温反应，保温反应的温度为100℃，时间为10h，保温反应结束后，过滤、洗涤、干燥回收中间产物，然后将中间产物置于加热炉内惰性气氛或真空条件下进行退火处理，退火处理的温度为500℃，时间3h，退火处理后即可制得所述Ni-MoS2/RGO/Ti3C2复合材料。
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| CN113441160A (zh) * | 2021-07-30 | 2021-09-28 | 陕西科技大学 | 一种氢氧化镍/碳化钛光热催化材料及其制备方法和应用 |
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| CN112010291A (zh) * | 2020-09-03 | 2020-12-01 | 郑州工程技术学院 | 一种镍掺杂二硫化钼/石墨烯三维复合材料的制备方法及应用 |
| CN113441160A (zh) * | 2021-07-30 | 2021-09-28 | 陕西科技大学 | 一种氢氧化镍/碳化钛光热催化材料及其制备方法和应用 |
| CN113441160B (zh) * | 2021-07-30 | 2023-06-16 | 陕西科技大学 | 一种氢氧化镍/碳化钛光热催化材料及其制备方法和应用 |
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