CN115301266A - 一种类石墨相氮化碳/聚苯胺/硫化镍异质结构光催化剂及其制备方法 - Google Patents
一种类石墨相氮化碳/聚苯胺/硫化镍异质结构光催化剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种g‑C3N4‑PANI‑NiS异质结构光催化剂的制备方法，包括：(1)g‑C3N4纳米片的制备：将碳氮源放置于带盖的陶瓷坩埚中于马弗炉中进行煅烧，得到淡黄色g‑C3N4粉末，再把g‑C3N4粉末置于瓷舟于管式炉中空气气氛下进行二次煅烧，将合成的样品用去离子水和无水乙醇洗涤三次，在真空干燥箱里干燥过夜后进行研磨得到白色g‑C3N4纳米片；(2)g‑C3N4‑PANI的制备：将苯胺分散在0.1mol/L的HCl溶液中，加入适量的过硫酸铵和g‑C3N4纳米片到上述混合液中，在冰浴下进行连续搅拌，得到的绿色沉淀即为产物；(3)将g‑C3N4‑PANI超声分散在去离子水中，依次加入镍源和硫源和适量的三乙醇胺，超声得到分散均匀的的悬浮液，将悬浮液于光催化反应器中在室温下用氙灯进行辐照后，得到g‑C3N4‑PANI‑NiS异质结构光催化剂。上述方法制得的g‑C3N4‑PANI‑NiS异质结构光催化剂在光催化析氢方面的具有良好的应用。
Description
技术领域
本发明涉及一种光催化材料，具体涉及一种g-C3N4-PANI-NiS异质结构光催化剂的制备方法，属于材料合成技术领域。
背景技术
人类赖以生存的化石能源是不可持续能源，其储存是有限的。随着全球工业的快速发展，化石燃料的短缺导致了对现代社会能源需求日益增长的严重关注，同时化石燃料的燃烧也造成环境问题日益突出，因此发展低成本的清洁可持续能源具有重要意义。自从1972年Fujishima所发表的开创性论文以来，人们发现半导体光催化技术可以分解水产生氢气，将低密度的太阳能转换为高密度的氢能形式储存。从能源利用和环境保护两个方面来看，氢能是一种能量高且燃烧无污染的可再生能源，可谓是21世纪的理想能源。因此，开发氢能源刻不容缓。
非金属聚合物半导体石墨相氮化碳(g-C3N4)因其具有前驱体来源广泛、制备方法简单、环境友好无重金属污染、光化学稳定性高、且能带结构适合光催化产氢/产氧等优点而在光催化分解水领域得到了积极广泛的研究。然而，g-C3N4载流子分离率低、水氧化驱动力弱及可见光吸收有限的瓶颈问题一直得不到有效的解决，这也严重限制了g-C3N4光催化全分解水的发展。为了克服这些问题，各种策略被用来来提高g-C3N4的光催化产氢效率，包括调节尺寸大小、形态、电子结构、金属或非金属沉积以及异质结构的构造等。其中，建立异质连接型光催化系统是促进光生成电子-空穴对的电荷分离的有效方法。
聚苯胺(PANI)是一种P型导电聚合物，在可见光范围内具有较高的光吸收系数和高电子迁移率，在光催化领域受到广泛关注。PANI和g-C3N4都具有∏共轭结构，两者更可能相容形成复合材料。聚苯胺(PANI)包覆于g-C3N4的表面时，不仅提高了g-C3N4的太阳能利用率，同时为其光生电子-空穴对的分离提供“传输通道”，促进了光生载流子的分离，从而提高其光催化性能。
在光催化产氢过程中，在光催化剂表面引入助催化剂是提高光催化性能的最有效方法之一，因为它具有加速界面电子转移、抑制光激发电荷重组和增加有效活性位点的优点。NiS作为一种过渡金属硫系化物，具有优异的电化学性能和良好的电导率，是光催化析氢反应中的有效助催化剂。此外，与其他非贵金属相比，NiS在质子还原过程中与吸附在表面的水形成Ni-H键时的活化能较低，将促进氢吸附还原-解吸过程，从而显著增强光催化制氢反应。
发明内容
采用热聚合法合成g-C3N4纳米片，再利用化学氧化聚合法以苯胺为单体，过硫酸铵为氧化剂在酸性介质中将合成的聚苯胺(PANI)包覆在g-C3N4纳米片上制得g-C3N4-PANI，然后利用光沉积法将NiS负载在g-C3N4-PANI上制备了g-C3N4-PANI-NiS光催化剂，发现所制备的g-C3N4-PANI-NiS光催化剂的在可见光下的光催化析氢性能高达7.818mmol/g-1h-1。
本发明提供了g-C3N4-PANI-NiS复合光催化剂的制备方法，其特征在于，该方法包括以下步骤：
(1)g-C3N4纳米片的制备：将碳氮源放置于带盖的陶瓷坩埚中于马弗炉中进行煅烧，得到淡黄色g-C3N4粉末，再把g-C3N4粉末置于瓷舟于管式炉中空气气氛下进行二次煅烧，将合成的样品用去离子水和无水乙醇洗涤三次，在真空干燥箱里干燥过夜后进行研磨得到白色g-C3N4纳米片；
(2)g-C3N4-PANI的制备：将苯胺分散在稀盐酸溶液中，加入适量的过硫酸铵和g-C3N4纳米片到上述混合液中，在冰浴下进行连续搅拌，得到的绿色沉淀即为产物；
(3)g-C3N4-PANI-NiS的制备：将g-C3N4-PANI超声分散在去离子水中，依次加入镍源和硫源和适量的三乙醇胺，超声得到分散均匀的的悬浮液，将悬浮液于光催化反应器中在室温下用氙灯进行辐照后，得到g-C3N4-PANI-NiS复合光催化剂并干燥。
在上述制备方法中，所述步骤(1)中，碳氮源可选为单胺、二氰二胺、三聚氰胺、尿素或硫脲。
在上述制备方法中，所述步骤(1)中，第一次煅烧温度为300～1000℃，再次煅烧温度为100～500℃。
在上述制备方法中，所述步骤(2)中，搅拌时间为1～10h。
在上述制备方法中，所述步骤(2)中，稀盐酸浓度为0.05-0.5mol/L。
在上述制备方法中，所述步骤(3)中，超声时间为0.5～2h。
在上述制备方法中，所述步骤(3)中，镍源可选为硝酸镍、氯化镍、硫酸镍、溴化镍或羟基镍。
在上述制备方法中，所述步骤(3)中，硫源为硫脲、硫代乙酰胺、半胱氨酸等。
在上述制备方法中，所述步骤(3)中，辐照时间为10～60min。
在上述制备方法中，所述步骤(3)中，干燥温度为50～80℃。
采用本技术制备的g-C3N4-PANI-NiS复合光催化剂制备过程简单，具有良好的光催化活性。
附图说明
图1是本发明实施例1所制得的g-C3N4-PANI-NiS复合光催化剂的XRD图
图2是本发明实施例1所制得的g-C3N4-PANI-NiS复合光催化剂的光催化析氢性能图。
具体实施方式
下面结合实施例对本发明的技术方案做进一步说明。
本发明提出一种高性能g-C3N4-PANI-NiS复合光催化剂制备方法，其特征在于，所述方法采用热聚合法g-C3N4纳米片，再采用利用化学氧化聚合法以苯胺为单体，过硫酸铵为氧化剂在酸性介质中将合成的聚苯胺(PANI)包覆在g-C3N4纳米片上制得g-C3N4-PANI，然后利用光沉积法将NiS分别负载在g-C3N4-PANI上制备了g-C3N4-PANI-NiS复合光催化剂，包括以下步骤和内容：
(1)碳氮源可选为单胺、二氰二胺、三聚氰胺、尿素或硫脲等。
(2)将碳氮源置于瓷舟中，于管式炉中空气气氛下煅烧，煅烧温度为300～1000℃，制得g-C3N4纳米片。
(3)将苯胺分散在0.05-0.5mol/L的HCl溶液中，加入适量的过硫酸铵和g-C3N4纳米片到上述混合液中，在冰浴下进行连续搅拌，制得g-C3N4-PANI。
(4)镍源可选为硝酸镍、氯化镍、硫酸镍、溴化镍或羟基镍等，硫源为硫脲、硫代乙酰胺、半胱氨酸等，将g-C3N4-PANI超声分散在去离子水中，依次加入镍源和硫源和适量的三乙醇胺，超声得到分散均匀的的悬浮液，将悬浮液于光催化反应器中在室温下用氙灯进行辐照后，收集并在80℃下干燥得到g-C3N4-PANI-NiS复合光催化剂。
总之，用本技术能得到高性能的g-C3N4-PANI-NiS复合光催化剂。
实施例1：称取20g尿素，放置于带盖的陶瓷坩埚中，在马弗炉中以2℃/min的升温速率升到550℃并保温4h制得g-C3N4粉末，研磨后称取10g g-C3N4粉末置于瓷舟中并转移到管式炉中，在空气氛围下以2℃/min的升温速率升到450℃并保温6h制得g-C3N4纳米片，用移液枪取50μL的苯胺分散在20mL 0.1mol/L的HCl溶液中，再称取0.08g过硫酸铵和5g g-C3N4纳米片加入该混合液中，将混合液在冰浴下连续搅拌8h制得g-C3N4-PANI，称取20mg g-C3N4-PANI分散在4mL去离子水中，超声分散0.5h，依次加入1mL 0.1M Ni(NO3)2·6H2O溶液，1mL 0.1M硫脲溶液，4mL三乙醇胺后，再次超声得到分散均匀得悬浮液，将悬浮液转移到光催化反应器中，抽取30min真空后，在室温下用氙灯对混合溶液进行辐照30min后制得g-C3N4-PANI-NiS复合光催化剂。
所合成的g-C3N4-PANI-NiS复合光催化剂制备过程简单，具有良好的光催化活性。
Claims (2)
1.一种g-C3N4-PANI-NiS异质结构光催化剂的制备方法，其特征在于，该方法包括以下步骤：
(1)g-C3N4纳米片的制备：将碳氮源放置于带盖的陶瓷坩埚中于马弗炉中进行煅烧，得到淡黄色g-C3N4粉末，再把g-C3N4粉末置于瓷舟于管式炉中空气气氛下进行二次煅烧，将合成的样品用去离子水和无水乙醇洗涤三次，在真空干燥箱里干燥过夜后进行研磨得到白色g-C3N4纳米片；
(2)g-C3N4-PANI的制备：将苯胺分散在稀盐酸溶液中，加入适量的过硫酸铵和g-C3N4纳米片到上述混合液中，在冰浴下进行连续搅拌，得到的绿色沉淀即为产物；
(3)g-C3N4-PANI-NiS的制备：将g-C3N4-PANI超声分散在去离子水中，依次加入镍源和硫源和适量的三乙醇胺，超声得到分散均匀的的悬浮液，将悬浮液于光催化反应器中在室温下用氙灯进行辐照后，得到g-C3N4-PANI-NiS复合光催化剂并干燥。
2.按照权利要求1所述的制备方法，其特征在于，
步骤(1)中，碳氮源可选为单胺、二氰二胺、三聚氰胺、尿素或硫脲；步骤(1)中，第一次煅烧温度为300～1000℃，再次煅烧温度为100～500℃；步骤(2)中，搅拌时间为1～10h；步骤(2)中，稀盐酸浓度为0.05-0.5mol/L；步骤(3)中，超声时间为0.5～2h；步骤(3)中，镍源可选为硝酸镍、氯化镍、硫酸镍、溴化镍或羟基镍；步骤(3)中，硫源为硫脲、硫代乙酰胺、半胱氨酸等；步骤(3)中，辐照时间为10～60min；步骤(3)中，干燥温度为50～80℃。
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