CN112495420A - 一种富氮石墨相氮化碳/偏钒酸银复合光催化剂的制备方法 - Google Patents
一种富氮石墨相氮化碳/偏钒酸银复合光催化剂的制备方法 Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 16
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- 239000000725 suspension Substances 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 14
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Abstract
本发明涉及一种富氮石墨相氮化碳/偏钒酸银复合光催化剂的制备方法。首先,使用简单的水浴加热方法合成g‑C3N5;然后,将制备好的g‑C3N5加入到AgNO3溶液中,搅拌一段时间后,加入偏钒酸铵溶液,将其调节pH到7,将调节好pH值的悬浊液超声一段时间后,离心并分别使用去离子水和乙醇洗涤,最后将得到的产物转移到真空干燥箱低于80℃干燥即可得到目标产物。g‑C3N5和AgVO3复合形成二元异质结构,能够有效促进光生载流子的分离和转移,可有效提高光催化效率。
Description
技术领域
本发明属于复合材料制备的技术领域,特别涉及一种g-C3N5/AgVO3二元异质结构光催化剂的制备方法。
背景技术
随着科技的进步和大规模的工业化,在环境中已检测到大量有害和有毒污染物,包括重金属、抗生素和染料等物质。这些污染物可能对人类、动物和生态系统构成严重威胁。因此科研人员探索了多种方法来降解环境中的污染物。其中光催化活性高和结构稳定的半导体可见光催化剂近年来在太阳能转换和水污染物处理方面被视为大有应用前景的先进材料。
AgVO3由于其窄的带隙和良好的结晶作用,被证明是一种有效的可见光催化剂。但是,其光催化产率差和不良的可见光吸收效率仍然是影响AgVO3光催化性能以满足实际应用的最重要的问题。为了解决这个问题,人们致力于开发和制备新型光催化材料,以提高催化剂的光催化性能,包括染料敏化、元素掺杂、间隙半导体和半导体异质结的能带工程。在这些工作中,半导体异质结的构建因其改善光催化活性的完美功效而备受关注。
氮化碳材料由于其独特的特性(出色的导电性,良好的化学稳定性和可控制的带隙)而受到了越来越多的关注。但是由于其光生电子较高的重组率,因此希望将g-C3N4的光催化活性提高到更高的水平。根据最近的实验和理论研究,发现了低带隙以及富氮的石墨氮化碳g-C3N5在光催化领域引起了极大的关注。g-C3N5电子带隙低至1.76eV,可以使材料在可见光区域提供高吸收性能。
因此,我们将g-C3N5和AgVO3复合在一起,由于二元异质结构的形成有效抑制光生载流子的复合,因而提高光催化效率。
发明内容
本发明要解决的技术问题是公开一种g-C3N5/AgVO3二元异质结构光催化剂及制备方法和应用。该催化剂拓宽了光催化剂的光响应范围,提高了光催化效率。该发明制备过程简单易控,产品性质稳定。
本发明的技术方案是:
一种富氮石墨相氮化碳/偏钒酸银复合光催化剂制备方法,
首先,使用简单的水浴加热方法合成g-C3N5;
然后,将制备好的g-C3N5加入到AgNO3溶液中,搅拌一段时间后,加入偏钒酸铵溶液,将其调节pH到7,将调节好pH值的悬浊液超声一段时间后,离心并分别使用去离子水和乙醇洗涤,最后将得到的产物转移到真空干燥箱低于80℃干燥即可得到目标产物。
g-C3N5的制备:将溴化钾固体和去离子水以18.5:1的比例混合均匀,然后向其中加入1.5g的3-氨基-1,2,4-三唑固体继续混合均匀,将其转移至80℃水浴蒸干,最后将得到的产物转移到真空干燥箱低于60℃干燥8小时,即可得到g-C3N5固体粉末。
将硝酸银和去离子水以质量比为48:1的比例混合均匀,向其中加入合成好的g-C3N5固体继续搅拌均匀,再将偏钒酸铵和去离子水以质量比为34:1的比例混合均匀,然后将两种溶液混合之后在室温下搅拌一定时间至混合均匀,之后调节pH到7,超声60分钟后,用去离子水和乙醇洗涤数次,再将产物在低于80℃的条件下干燥24小时,即可得到g-C3N5/AgVO3晶体粉末。
本发明的有益效果是:
1、AgVO3材料的加入能够有效拓宽光催化剂的光响应范围,复合材料吸收边波长可达700nm。
2、g-C3N5和AgVO3复合形成二元异质结构,能够有效促进光生载流子的分离和转移,可有效提高光催化效率。
3、该发明制备过程简单易控,产品性质稳定。
附图说明
图1为g-C3N5和g-C3N4的EPR图。
图2a,b为g-C3N5和图2c,d为g-C3N4的SEM照片。
图3为g-C3N5和g-C3N4样品的照片
图4为g-C3N5、AgVO3、g-C3N5/AgVO3的XRD图
图5为g-C3N5、g-C3N5/AgVO3的FT-IR图
图6为g-C3N5、g-C3N5/AgVO3的UV-vis DRS图
图7为g-C3N5/AgVO3的SEM图及EDS元素拍照图
图8a为催化剂降解罗丹明行为图
图8b为g-C3N5/AgVO3催化剂对不同污染物降解效率图。
具体实施方式
实施例1
(一)g-C3N5的制备
(1)将10g的溴化钾溶解于30mL的去离子水中;
(2)将1.5g 3-氨基-1,2,4-三唑加入到溴化钾溶液中搅拌均匀;
(3)将上述溶液放置到80℃水浴中蒸干,然后冷却,将产物转移到60℃真空干燥箱中干燥8h,即可得到g-C3N5固体粉末。
产物g-C3N5的XRD、FT-IR和UV-vis DRS谱图等分别如图1-6所示。
(二)g-C3N5/AgVO3的制备
(1)将0.0085g的硝酸银溶解于10mL的去离子水中,向其中加入0.06g g-C3N5固体,搅拌30min;
(2)将0.0085g的偏钒酸铵溶解于10mL的去离子水中,将其逐滴滴加到(1)中的悬浊液中,继续搅拌30min;
(3)然后将搅拌好的悬浊液用氨水调节pH到7后,转移到超声机中超声60min;
(4)将超声好的悬浊液离心,并分别用水和乙醇洗涤三次,转移到80℃真空干燥箱中干燥24h。
产物g-C3N5/AgVO3的XRD、FT-IR和UV-vis DRS谱图等分别如图4-7
实施例2
在光化学反应仪中进行光催化实验,将20mg的光催化剂放入100mL浓度为10mgL-1的罗丹明B溶液中,在磁力搅拌的情况下,首先暗反应5min,罗丹明B在光催化剂表面达到吸附平衡状态。然后用300W的氙灯照射用来提供可见光,在氙灯和反应容器之间使用滤光片去除紫外光,每隔10分钟取出4mL的悬浊液,将其离心取上层清液用紫外-可见分光光度计测试罗丹明B溶液的浓度。
对照物AgVO3的制备
(1)将0.0085g的硝酸银溶解于10mL的去离子水中,搅拌30min;
(2)将0.0085g的偏钒酸铵溶解于10mL的去离子水中,将其逐滴滴加到(1)中的悬浊液中,继续搅拌30min;
(3)然后将搅拌好的悬浊液用氨水调节pH到7后,转移到超声机中超声60min;
(4)将超声好的悬浊液离心,并分别用水和乙醇洗涤三次,转移到80℃真空干燥箱中干燥24h。
附图详细说明
图1为g-C3N5和g-C3N4的EPR图。图中显示了一条单一的洛伦兹线,这是由庚嗪环的碳原子上不成对的电子诱导的。g-C3N4的EPR强度比g-C3N5要高很多,这表明g-C3N4产生的空位比g-C3N5多。
图2为g-C3N5(a,b)和g-C3N4(c,d)的SEM图,从图中可以看出g-C3N5样品的表面较为光滑,而g-C3N4样品的表面较为粗糙。
图3为g-C3N5和g-C3N4样品的照片,从照片中可以看出g-C3N5样品颜色更深,证明其可见光吸收范围更宽。
图4为所制备样品的XRD图。从g-C3N5/AgVO3的XRD图可以看出,基本符合g-C3N5的衍射峰。从中没有观察到AgVO3的衍射峰,是由于AgVO3的含量较低。
图5为所制备样品g-C3N5和g-C3N5/AgVO3的FT-IR图。从图中可以看出,在复合样品g-C3N5/AgVO3的红外谱图中都可以找到C3N5的衍射峰,说明g-C3N5/AgVO3二元异质结构光催化剂成功合成。
图6为所制备样品g-C3N5和g-C3N5/AgVO3的UV-vis DRS谱图。从图中可以看出复合光催化剂对可见光有较强的吸收,复合材料吸的收边波长为700nm。说明AgVO3材料的加入能够有效拓宽光催化剂的光响应范围。
图7为所制备样品g-C3N5/AgVO3的SEM图,从图中可以看出样品为块状。从EDS元素拍照表明C、N、O、V、Ag元素的存在,证明g-C3N5/AgVO3二元异质结构光催化剂成功合成。
图8a为催化剂降解罗丹明行为,从图中可以看出g-C3N5/AgVO3催化剂光催化效率较纯相g-C3N5及AgVO3高得多。图8b为g-C3N5/AgVO3催化剂对不同污染物降解效率。采用20mgg-C3N5/AgVO3催化剂,光照下罗丹明B、甲基橙染料及抗生素四环素降解率分别可达98%、93%及80%。
Claims (3)
1.一种富氮石墨相氮化碳/偏钒酸银复合光催化剂的制备方法,其特征在于:
首先,使用简单的水浴加热方法合成g-C3N5;
然后,将制备好的g-C3N5加入到AgNO3溶液中,搅拌一段时间后,加入偏钒酸铵溶液,将其调节pH到7,将调节好pH值的悬浊液超声一段时间后,离心并分别使用去离子水和乙醇洗涤,最后将得到的产物转移到真空干燥箱低于80℃干燥即可得到目标产物。
2.根据权利要求1所述的一种富氮石墨相氮化碳/偏钒酸银复合光催化剂的制备方法,其特征在于:g-C3N5的制备:将溴化钾固体和去离子水以18.5:1的比例混合均匀,然后向其中加入1.5g的3-氨基-1,2,4-三唑固体继续混合均匀,将其转移至80℃水浴蒸干,最后将得到的产物转移到真空干燥箱低于60℃干燥8小时,即可得到g-C3N5固体粉末。
3.根据权利要求1所述的一种富氮石墨相氮化碳/偏钒酸银复合光催化的剂制备方法,其特征在于:将硝酸银和去离子水以质量比为48:1的比例混合均匀,向其中加入合成好的g-C3N5固体继续搅拌均匀,再将偏钒酸铵和去离子水以质量比为34:1的比例混合均匀,然后将两种溶液混合之后在室温下搅拌一定时间至混合均匀,之后调节pH到7,超声60分钟后,用去离子水和乙醇洗涤数次,再将产物在低于80℃的条件下干燥24小时,即可得到g-C3N5/AgVO3晶体粉末。
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CN114904547A (zh) * | 2022-04-11 | 2022-08-16 | 塔里木大学 | 混合晶相WO3@g-C3N5复合光催化剂的制备方法 |
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