CN112156806A - 一种快速制备碘钾共掺杂氮化碳的方法及其产品和应用 - Google Patents
一种快速制备碘钾共掺杂氮化碳的方法及其产品和应用 Download PDFInfo
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- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 title claims abstract description 147
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000008367 deionised water Substances 0.000 claims abstract description 44
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 44
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 30
- 239000011630 iodine Substances 0.000 claims abstract description 30
- 238000000227 grinding Methods 0.000 claims abstract description 20
- ZVAKTWSQIIRIIH-UHFFFAOYSA-N [K].[I] Chemical compound [K].[I] ZVAKTWSQIIRIIH-UHFFFAOYSA-N 0.000 claims abstract description 14
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims description 56
- 229920000877 Melamine resin Polymers 0.000 claims description 34
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 34
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 21
- 229910052700 potassium Inorganic materials 0.000 claims description 21
- 239000011591 potassium Substances 0.000 claims description 21
- 239000000919 ceramic Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 8
- 230000015556 catabolic process Effects 0.000 claims description 5
- 238000006731 degradation reaction Methods 0.000 claims description 5
- 239000011941 photocatalyst Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 230000000593 degrading effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 229910001868 water Inorganic materials 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
本发明是一种快速制备碘钾共掺杂氮化碳的方法及其产品和应用,准确称量三聚氰胺、碘化钾以及去离子水溶剂,将三聚氰胺以及碘化钾加入去离子水中,在一定温度下搅拌蒸干。将上述产物研磨粉碎之后放入带盖坩埚中于马弗炉中进行焙烧,然后自然冷却。将焙烧产物与单质碘加入去离子水中之后于行星式球磨机中研磨一段时间,过滤、洗涤、干燥之后即得碘钾共掺杂氮化碳。采用本发明提出的制备方法得到的碘钾共掺杂氮化碳,禁带宽度适中,光生电子与空穴的分离效率高,光催化降解亚甲基蓝效果好,且操作简单,步骤少,原料易得,成本低,适合放大化生产。
Description
技术领域
本发明属于纳米材料制备领域,具体涉及一种快速制备碘钾共掺杂氮化碳的方法及其产品和应用。
背景技术
光催化技术是近年来迅速发展起来的可以利用太阳能进行环境净化和能源转化的新技术。其一般能带间隙适中,在太阳光的照射下,其电子能发生跃迁,从而形成高能的光生电子与光生空穴对,当与空气中的氧气以及水接触时,能发生氧化还原反应生成超氧自由基、羟基自由基等活跃自由基,这些自由基可以降解污染物、杀灭细菌与病毒等。相比于其他技术,光催化技术安全、高效无二次污染,污染物被彻底氧化分解为CO2、H2O等无害产物。但是,现有的光催化材料仍然存在着各种各样的问题。
氮化碳是一种黄色石墨结构物质,氮化碳不含金属,没有毒性,廉价易得,且其原料在地球中储量丰富,易于合成,并且具有良好的化学与热稳定性。因此,其在光催化领域引起了广泛的关注。但是氮化碳也存在着一些问题,例如:其禁带宽度为2.7eV,禁带宽度过大,可见光区的光子能量不足以使价带上的电子发生跃迁,这使得其对太阳能的利用效率偏低;另一方面,其光生电子和空穴发生分离之后,在传输的过程中,极易重新发生复合,这就会导致大量光生电子与空穴没法与空气中的水与氧气发生反应生成超氧自由基以及羟基自由基,限制其降解污染物以及杀灭细菌的能力。
发明内容
针对现有制备氮化碳禁带宽度较大,光生电子与空穴分离效率不高的缺点,本发明目的在于提供一种快速制备碘钾共掺杂氮化碳的方法。
本发明的再一目的在于:提供一种上述方法制备的包裹IR780@硅质体产品。
本发明的又一目的在于:提供一种上述产品的应用。
本发明目的通过下述方案实现:一种快速制备碘钾共掺杂氮化碳的方法,包括如下步骤:
1)按三聚氰胺与碘化钾和去离子水的质量比为1:(0.01~1):(5~200)称取三聚氰胺、碘化钾以及去离子水,将三聚氰胺以及碘化钾加入去离子水中,在50~100℃下搅拌使其蒸干成固体;
2)将上述得到的固体研磨粉碎之后放入陶瓷坩埚中,然后于马弗炉中加热到400~650℃保温焙烧0.1~15h,升温速率为1~20℃/min,然后自然冷却,得到的棕色固体为钾以及少量碘掺杂的氮化碳;
3)将上述得到的钾以及少量碘掺杂的氮化碳加入球磨罐中,按钾以及少量碘掺杂氮化碳与碘单质和去离子水的质量比为1:(0.1~1):(5~200)加入单质碘以及去离子水,于球磨机中以50~500 r/min转速研磨1~72h,然后过滤、洗涤、干燥,即得碘钾共掺杂氮化碳。
本发明还提供了一种碘钾共掺杂氮化碳,根据上述所述方法制备得到。
本发明也提供了一种碘钾共掺杂氮化碳在降解亚甲基蓝中作为光催化剂的应用。
本发明提供的快速制备碘钾共掺杂氮化碳的方法为:准确称量三聚氰胺、碘化钾以及去离子水溶剂,将三聚氰胺以及碘化钾加入去离子水中,在一定温度下搅拌蒸干。将其研磨粉碎之后放入带盖坩埚中于马弗炉中进行焙烧,然后将焙烧产物与单质碘加入去离子水中之后于行星式球磨机中研磨一段时间,过滤、洗涤、干燥之后,即得碘钾共掺杂氮化碳。
本发明通过采用碘与钾共掺杂的方式来提高其光催化效率,一方面通过无机碘元素掺杂来降低氮化碳的能带间隙,另一方面通过金属元素钾掺杂来提高其光生电子与空穴的分离效率,通过两者的协同效应来提高氮化碳的光催化效率。采用本发明提出的制备方法得到的碘钾共掺杂氮化碳,禁带宽度适中,光生电子与空穴的分离效率高,光催化降解亚甲基蓝效果好,且操作简单,步骤少,原料易得,成本低,适合放大化生产。
本发明创造性的采用非金属元素碘以及金属元素钾对氮化碳进行共掺杂,一方面通过非金属元素碘掺杂来降低氮化碳的禁带宽度;另一方面,通过金属元素钾的掺杂来降低氮化碳的光生电子与空穴的复合率,从而来提高光生电子与空穴对产生超氧自由基以及羟基自由基的数量。通过两者的协同效应,达到大幅度提高光催化效率的效果。采用本发明所述方法制备的碘钾共掺杂氮化碳,禁带宽度适中,光生电子与空穴的分离效率高,光催化降解亚甲基蓝效果好,且操作简单,步骤少,原料易得,成本低,适合放大化生产。
附图说明
图1 采用本发明方法制备碘钾共掺杂氮化碳在可见光下降解亚甲基蓝的性能。
具体实施方式
下面通过实施例进一步说明本发明,而不是限制本发明的范围。
实施例1:
一种碘钾共掺杂氮化碳,按如下步骤快速制备:
1)按三聚氰胺与碘化钾和去离子水的质量比为1:1:100称取三聚氰胺、碘化钾以及去离子水,将三聚氰胺以及碘化钾加入去离子水中,在80℃下搅拌使其蒸干成固体;
2)将上述得到的固体研磨粉碎之后放入陶瓷坩埚中,然后于马弗炉中加热到550℃保温焙烧3h,升温速率为3℃/min,然后自然冷却,得到的棕色固体;
3)将上述得到的棕色固体加入球磨罐中,按棕色固体与碘单质和去离子水的质量比为1:0.2:50加入单质碘以及去离子水,于行星式球磨机中以200 r/min转速研磨36h,然后过滤、洗涤、干燥,即得碘钾共掺杂氮化碳。
本发明方法制备碘钾共掺杂氮化碳在可见光下降解亚甲基蓝的性能如图1所示,降解率达92.3%。
实施例2:
一种碘钾共掺杂氮化碳,与实施例1步骤相同,按如下步骤快速制备:
1)按三聚氰胺与碘化钾和去离子水的质量比为1:0.3:50称取三聚氰胺、碘化钾以及去离子水,将三聚氰胺以及碘化钾加入去离子水中,在90℃下搅拌使其蒸干成固体;
2)将上述得到的固体研磨粉碎之后放入陶瓷坩埚中,然后于马弗炉中加热到500℃保温焙烧5h,升温速率为5℃/min,然后自然冷却,得到的棕色固体为钾以及少量碘掺杂的氮化碳;
3)将上述得到的棕色固体加入球磨罐中,按棕色固体与碘单质和去离子水的质量比为1:0.5:100加入单质碘以及去离子水,于行星式球磨机中以300 r/min转速研磨48h,然后过滤、洗涤、干燥,即得碘钾共掺杂氮化碳。
本发明方法制备碘钾共掺杂氮化碳在可见光下降解亚甲基蓝的性能如图1所示,降解率达84.7%。
实施例3:
一种碘钾共掺杂氮化碳,与实施例1步骤相同,按如下步骤快速制备:
1)按三聚氰胺与碘化钾和去离子水的质量比为1:0.5:80称取三聚氰胺、碘化钾以及去离子水,将三聚氰胺以及碘化钾加入去离子水中,在100℃下搅拌使其蒸干成固体;
2)将上述得到的固体研磨粉碎之后放入陶瓷坩埚中,然后于马弗炉中加热到600℃保温焙烧5h,升温速率为10℃/min,然后自然冷却,得到的棕色固体为钾以及少量碘掺杂的氮化碳;
3)将上述得到的棕色固体加入球磨罐中,按棕色固体与碘单质和去离子水的质量比为1:0.3:80加入单质碘以及去离子水,于行星式球磨机中以100 r/min转速研磨24h,然后过滤、洗涤、干燥,即得碘钾共掺杂氮化碳。
本发明方法制备碘钾共掺杂氮化碳在可见光下降解亚甲基蓝的性能如图1所示,降解率达96.7%。
附表1 采用本发明方法制备碘钾共掺杂氮化碳在可见光下降解亚甲基蓝的性能:
Claims (6)
1.一种快速制备碘钾共掺杂氮化碳的方法,其特征在于包括如下步骤:
1)按三聚氰胺与碘化钾和去离子水的质量比为1:(0.01~1):(5~200)称取三聚氰胺、碘化钾以及去离子水,将三聚氰胺以及碘化钾加入去离子水中,在50~100℃下搅拌使其蒸干成固体;
2)将上述得到的固体研磨粉碎之后放入陶瓷坩埚中,然后于马弗炉中加热到400~650℃保温焙烧0.1~15h,升温速率为1~20℃/min,然后自然冷却,得到的棕色固体为钾以及少量碘掺杂的氮化碳;
3)将上述得到的钾以及少量碘掺杂的氮化碳加入球磨罐中,按钾以及少量碘掺杂氮化碳与碘单质和去离子水的质量比为1:(0.1~1):(5~200)加入单质碘以及去离子水,于球磨机中以50~500 r/min转速研磨1~72h,然后过滤、洗涤、干燥,即得碘钾共掺杂氮化碳。
2.根据权利要求1所述的快速制备碘钾共掺杂氮化碳的方法,其特征在于,
按如下步骤:
1)按三聚氰胺与碘化钾和去离子水的质量比为1:1:100称取三聚氰胺、碘化钾以及去离子水,将三聚氰胺以及碘化钾加入去离子水中,在80℃下搅拌使其蒸干成固体;
2)将上述得到的固体研磨粉碎之后放入陶瓷坩埚中,然后于马弗炉中加热到550℃保温焙烧3h,升温速率为3℃/min,然后自然冷却,得到的棕色固体;
3)将上述得到的棕色固体加入球磨罐中,按棕色固体与碘单质和去离子水的质量比为1:0.2:50加入单质碘以及去离子水,于行星式球磨机中以200 r/min转速研磨36h,然后过滤、洗涤、干燥,即得碘钾共掺杂氮化碳。
3.根据权利要求1所述的快速制备碘钾共掺杂氮化碳的方法,其特征在于,
按如下步骤:
1)按三聚氰胺与碘化钾和去离子水的质量比为1:0.3:50称取三聚氰胺、碘化钾以及去离子水,将三聚氰胺以及碘化钾加入去离子水中,在90℃下搅拌使其蒸干成固体;
2)将上述得到的固体研磨粉碎之后放入陶瓷坩埚中,然后于马弗炉中加热到500℃保温焙烧5h,升温速率为5℃/min,然后自然冷却,得到的棕色固体为钾以及少量碘掺杂的氮化碳;
3)将上述得到的棕色固体加入球磨罐中,按棕色固体与碘单质和去离子水的质量比为1:0.5:100加入单质碘以及去离子水,于行星式球磨机中以300 r/min转速研磨48h,然后过滤、洗涤、干燥,即得碘钾共掺杂氮化碳。
4.根据权利要求1所述的快速制备碘钾共掺杂氮化碳的方法,其特征在于,
按如下步骤:
1)按三聚氰胺与碘化钾和去离子水的质量比为1:0.5:80称取三聚氰胺、碘化钾以及去离子水,将三聚氰胺以及碘化钾加入去离子水中,在100℃下搅拌使其蒸干成固体;
2)将上述得到的固体研磨粉碎之后放入陶瓷坩埚中,然后于马弗炉中加热到600℃保温焙烧5h,升温速率为10℃/min,然后自然冷却,得到的棕色固体为钾以及少量碘掺杂的氮化碳;
3)将上述得到的棕色固体加入球磨罐中,按棕色固体与碘单质和去离子水的质量比为1:0.3:80加入单质碘以及去离子水,于行星式球磨机中以100 r/min转速研磨24h,然后过滤、洗涤、干燥,即得碘钾共掺杂氮化碳。
5.一种碘钾共掺杂氮化碳,其特征在于根据权利要求1至4任一项所述方法制备得到。
6.一种根据权利要求5所述碘钾共掺杂氮化碳在降解亚甲基蓝中作为光催化剂的应用。
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