CN108067280A - 一种硫化镍/类石墨烯碳氮化合物复合催化剂的制备方法 - Google Patents

一种硫化镍/类石墨烯碳氮化合物复合催化剂的制备方法 Download PDF

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CN108067280A
CN108067280A CN201711177629.3A CN201711177629A CN108067280A CN 108067280 A CN108067280 A CN 108067280A CN 201711177629 A CN201711177629 A CN 201711177629A CN 108067280 A CN108067280 A CN 108067280A
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董玉明
张会珍
赵辉
赵云霏
赵爽
赵娜
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Abstract

本发明目的是为了缓解日益严重的能源短缺和环境污染问题，通过温和的原位光沉积法制备了不含贵金属的硫化镍/类石墨烯碳氮化合物复合催化剂，用于高效地光催化分解水产氢。本发明以类石墨烯碳氮化合物为光敏剂，醋酸镍作为镍源，硫脲作为硫源制得硫化镍/类石墨烯碳氮化合物复合催化剂。此制备方法简单高效、低碳环保、成本低廉，且催化剂的光催化产氢速率高。因而，此硫化镍/类石墨烯碳氮化合物复合催化剂在光催化产氢领域具有很好的工业化应用前景。

Description

一种硫化镍/类石墨烯碳氮化合物复合催化剂的制备方法
技术领域
本发明提出硫化镍/类石墨烯碳氮化合物复合催化剂的简便制备方法，属于材料科学技术领域和光催化制氢领域。
背景技术
随着能源困境和环境污染问题日益严峻，开发绿色可再生能源已经引起了极大的关注。氢能源具有燃烧值高、产物清洁无污染、可再生等优点，可作为化石能源的替代物，进而有助于减轻环境问题。利用太阳光在催化剂的作用下分解水制氢，可以将太阳能转化为化学能(氢能)，有效地把太阳能储存起来，具有非常高的研究价值。开发具有良好稳定性和光活性的光催化剂是光催化制氢领域的关键。
类石墨烯碳氮化合物(又称为g-C3N4)是一种由碳、氮两种元素组成的共价化合物，热稳定性及化学稳定性好，禁带宽度较窄，可以吸收可见光。并且其原料廉价易得，制备方法简单。然而，纯g-C3N4在光催化分解水制氢系统中，光生电子和空穴很容易发生复合，产氢活性低。在g-C3N4纳米片表面负载金属硫化物纳米颗粒可以有效地抑制光生载流子的复合，从而提高光催化产氢活性。
本发明制备的硫化镍/类石墨烯碳氮化合物复合催化剂，具有优良的光催化产氢活性和稳定性。据我们所知，本实验采用的光沉积方法在g-C3N4表面负载硫化镍，尚未见文献报道。
发明内容
本发明目的是为了缓解日益严重的能源短缺和环境污染问题，通过温和的原位光沉积法制备了不含贵金属的簇状的硫化镍/类石墨烯碳氮化合物复合催化剂，用于高效地太阳能分解水产氢。此制备方法简单高效、低碳环保、成本低廉，且催化剂的光催化产氢速率高、稳定性好。
本发明提供一种硫化镍/类石墨烯碳氮化合物复合催化剂的简便制备方法，可以通过以下技术方案实现：
(1)称取适量硫脲放入坩埚中加盖，在550℃空气气氛下加热2小时，升温速率为2℃/min.将所得的黄色粉末研磨后放入不加盖的坩埚中，在500℃下加热2小时，升温速率仍为2℃/min.最后，得到的淡黄色粉末即为类石墨烯碳氮化合物(又可称为g-C3N4，为纳米片结构)；
(2)在25ml的单口圆底烧瓶中，加入一定量的类石墨烯碳氮化合物，醋酸镍(作为镍源)和硫脲(作为硫源)，再加入适量水和乙醇，超声使其分散混合均匀。通入40分钟氮气除去反应体系中的氧气，然后置于氙灯下进行光照；
(3)反应结束后，使用离心将固体分离，用去离子水和乙醇洗涤数次，将所得固体放于真空干燥箱进行干燥，得到灰黑色固体物质即为硫化镍/类石墨烯碳氮化合物复合催化剂。
本发明的显著优点在于：g-C3N4是一种廉价易得、无毒、稳定性好的吸光材料，且具有合适的禁带宽度。硫化镍原料来源丰富，价格便宜，可以有效促进光生载流子的分离；使用光沉积的方法制得硫化镍/类石墨烯碳氮化合物复合催化剂，相比其他方法，本发明的方法简单高效，且节能环保；硫化镍纳米粒子均匀的分散在g-C3N4纳米片上，且尺寸很小，大约为几到十几纳米，暴露出的活性原子的数目多，原子利用率高，具有优异的产氢活性和稳定性。
附图说明
图1是实施例1所得类石墨烯碳氮化合物和硫化镍/类石墨烯碳氮化合物复合催化剂的高分辨率的XPS光谱。
图2是实施例1所得类石墨烯碳氮化合物和硫化镍/类石墨烯碳氮化合物复合催化剂的透射电镜图片和高分辨率透射电镜图片。
图3是实施例1所得类石墨烯碳氮化合物和硫化镍/类石墨烯碳氮化合物复合催化剂的能量色散X射线能谱。
图4是实施例1所得类石墨烯碳氮化合物和硫化镍/类石墨烯碳氮化合物复合催化剂在可见光下的光催化产氢性能图。
图5是实施例1所得类石墨烯碳氮化合物和硫化镍/类石墨烯碳氮化合物复合催化剂在太阳光下的光催化产氢性能图。
具体实施方式
下面结合一些实例和附图对本发明做进一步的说明，但本发明的应用不限于此。
实施例1
(1)称取20g硫脲放入坩埚中加盖，在550℃空气气氛下加热2小时，升温速率为2℃/min.将所得的黄色粉末研磨后放入不加盖的坩埚中，在500℃下加热2小时，升温速率仍为2℃/min.最后，得到的淡黄色粉末即为类石墨烯碳氮化合物；
(2)在25mL的单口圆底烧瓶中，加入20mg类石墨烯碳氮化合物，12.5mg醋酸镍，38mg硫脲，4mL无水乙醇，6mL超纯水，超声处理5min使其分散混合均匀。通入40分钟氮气除去反应体系中的氧气。
(3)将烧瓶放于300W氙灯下，照射20min后，使用离心将固体分离，用去离子水洗涤两次，乙醇洗涤一次，将所得固体放于真空干燥箱，80℃干燥过夜，得到灰白色固体物质即为硫化镍/类石墨烯碳氮化合物复合催化剂。所制备的硫化镍/类石墨烯碳氮化合物复合催化剂中硫化镍的质量百分含量为0.76wt％。
将制备的复合催化剂进行高分辨率的XPS光谱(图1)，透射电镜和高分辨率的透射电镜(图2)及能量色散X射线能谱(图3)。
实施例2
取实施例1中制备的硫化镍/类石墨烯碳氮化合物复合催化剂5mg置于25mL圆底烧瓶中，加入1mL三乙醇胺(98％)，9mL水；超声处理5min,用氮气脱气40min除去反应体系中的氧气；将圆底烧瓶放于300W氙灯，400nm滤光片下光照，反应结束后，用热导-气相色谱仪检测反应生成的氢气。该催化剂的产氢速率约为800μmol g-1h-1，且反应30个小时后，产氢速率没有明显下降(图4)。
实施例3
取实施例1中制备的硫化镍/类石墨烯碳氮化合物复合催化剂5mg置于25mL圆底烧瓶中，加入1mL三乙醇胺(98％)，9mL水；超声处理5min，用氮气脱气40min除去反应体系中的氧气；将圆底烧瓶放于自然太阳光下照射2h，产氢速率约为1000μmol g-1h-1(图5)。
由上述各实例可以看出，本发明所制备的硫化镍/类石墨烯碳氮化合物复合催化剂具有合成方法简单、产氢速率高、稳定性好等优点，在光催化产氢领域具有很好的工业化应用前景。

Claims (1)

1.一种硫化镍/类石墨烯碳氮化合物复合催化剂的简单高效的制备方法，其特征在于按照如下方案进行：
(1)称取适量硫脲放入坩埚中加盖，在550℃空气气氛下加热2小时，升温速率为2℃/min.将所得的黄色粉末研磨后放入不加盖的坩埚中，在500℃下加热2小时，升温速率仍为2℃/min.最后，得到的淡黄色粉末即为类石墨烯碳氮化合物(又可称为g-C3N4，为纳米片结构)；
(2)在25mL的单口圆底烧瓶中，加入一定量的类石墨烯碳氮化合物，醋酸镍(作为镍源)和硫脲(作为硫源)，再加入适量水和乙醇，超声使其分散混合均匀。通入40分钟氮气除去反应体系中的氧气，然后置于氙灯下进行光照；
(3)反应结束后，使用离心将固体分离，用去离子水和乙醇洗涤数次，将所得固体放于真空干燥箱进行干燥，得到灰黑色固体物质即为硫化镍/类石墨烯碳氮化合物复合催化剂。
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CN109526981A (zh) * 2018-12-18 2019-03-29 华南农业大学 一种纳米复合材料g-C3N4/Ni及其制备方法与应用
CN109759087A (zh) * 2019-01-16 2019-05-17 安徽大学 一种NiS/MgAl-LDH光催化剂及其制备方法和应用
CN110652988A (zh) * 2019-09-25 2020-01-07 三峡大学 超细双金属硫化物微球负载NiS薄膜的制备方法及其应用
CN112473717A (zh) * 2020-11-30 2021-03-12 江南大学 一种镍单原子/功能化石墨相氮化碳复合催化剂
CN112547107A (zh) * 2020-12-04 2021-03-26 江南大学 一种α-Fe2O3/Ni@2D g-C3N4催化剂的制备方法
CN113600220A (zh) * 2021-06-23 2021-11-05 宁夏大学 氮化碳高负载分散NiS光催化降解材料及制备方法
CN114392763A (zh) * 2022-01-29 2022-04-26 中国科学院东北地理与农业生态研究所 四角管状CN/NiS复合光催化剂制备方法

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