CN105664993A - 一种荧光掺杂碳纳米光催化剂及其制备方法与应用 - Google Patents
一种荧光掺杂碳纳米光催化剂及其制备方法与应用 Download PDFInfo
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Abstract
本发明提供一种荧光掺杂碳纳米N,B,S-CDs及其制备方法与应用，该方法以柠檬酸、硼酸、硫脲、乙二胺作为前聚体；柠檬酸提供碳源，乙二胺提供氮源，硼酸提供硼源，硫脲提供硫源制备得N？B？S-CDs。本发明不仅制备工艺简单，而且制备的荧光掺杂碳纳米材料具有很强的荧光，优秀的稳定性，良好的水溶性。在可见光照射下展现优秀的光催化降解罗丹明B（简称为RhB）能力，其降解率高达98.5？%，因此在环境修复、污水处理及分离科学等领域有着良好的应用前景。
Description
技术领域
本发明属于生化分析领域，具体是一种新型荧光掺杂碳纳米光催化剂及其制备方法与在光催化降解罗丹明B(简称为RhB)中的应用。
背景技术
碳点(CDs)，作为碳纳米材料家族的新成员，是直径小于10nm的碳纳米颗粒，通常由SP2杂化的碳原子、富含氧和氢的物质所组成。碳点作为一种新型荧光碳纳米材料，拥有特殊的荧光性能，如激发和发射波长可调、光稳定性好、无光闪烁现象等，CDs相比与传统的有机荧光染料和金属量子点，有许多优点，其独特的发光性质和生物相容性在光催化、发光设备、光电子学、生化分析、细胞成像及检测等领域具有较好的应用前景。为了提高荧光CDs的光电特性，硼、氮、氟、硫等作为掺杂化学元素引入到CDs里面(DongY,PangH,YangHB,GuoCX,ShaoJW,ChiYW,LiCM,YuT.AngewandteChemieInternationalEdition,2013,52(30):7800-7804.JahanS,MansoorF,NazS,LeiJ,KanwalS..Analyticalchemistry,2013,85(21):10232-10239.)，使CDs的量子产率大大提高，光学特性显著增强，应用更为广泛。
据统计，我国每生产1t染料就会排放废水744t，而在印染过程中，染料废水流失率约为10％～20％，其中约50％进入环境。染料(颜色)是废水中最早被确认的一类污染物，即使水体中存在少量染料(对一些染料而言，浓度低于1mg/L)也会出现颜色的变化，排入水体中，会影响水生物的光合作用，给人感官上也带来不悦，而且大多的有机染料都属于难降解“致畸、致癌、致突变”的三致物质(CGregorio,BioresourceTechnology,2006,97(9):1061-1085)。人工合成的染料RhB广泛用于印染行业，其形成的废水有机物含量高，色度高，水质变化大，毒性大，成为最难检测与处理的染料废水之一。使用半导体催化剂(如：氧化锌和二氧化钛)光催化降解废水中的有机染料已有发展(LamSM,SinJC,AbdullahAZ,MohamedAR.DesalinationandWaterTreatment,2012,41(1-3):131-169)，但现有技术中常见的光催化剂很多需要通过紫外线或近紫外辐照，严格限制了其大规模的实际应用，因为太阳光里大约有只有5％的紫外线，其它是43％可见光和52％红外线。因此，发展可以直接应用太阳光的新型高效光催化剂是非常有必要的。
发明内容
本发明的目的是提供一种新型荧光掺杂碳纳米N,B,S-CDs光催化剂及其制备方法与应用，该荧光掺杂碳纳米N,B,S-CDs光催化剂能有效降解有机染料，并且具有简便、便宜、环保、快速的特点。该方法通过柠檬酸、硼酸、硫脲、乙二胺作为前聚体，柠檬酸提供碳源、乙二胺提供氮源、硼酸提供硼源、硫脲提供硫源，制备得NBS-CDs。本发明不仅制备工艺简单，而且制备的荧光掺杂碳纳米材料具有很强的荧光，优秀的稳定性，良好的水溶性。在可见光照射下展现优秀的光催化降解RhB能力，因此在环境修复、污水处理及分离科学等领域有着良好的应用前景。
实现本发明目的的技术方案是：
一种荧光掺杂碳纳米N,B,S-CDs光催化剂的制备方法，包括如下步骤：
(1)称取2.1g柠檬酸、1.4g硫脲、1.4g硼酸、5mL乙二胺溶解在5mL水中，然后转移到聚四氟乙烯内衬的高压反应釜里，以每分钟10℃的速率加热至220℃，并保持3h，得到的红棕色溶液；
(2)用1molL-1NaOH溶液调节pH至7.0，然后离心8000rpm，20min，将所得水溶解进行，透析，分离未反应的物质得到棕色的N,B,S-CDs水溶液；
(3)旋转蒸发除去水，然后溶解在去离子水中于4℃避光保存。
用上述荧光掺杂碳纳米N,B,S-CDs光催化剂在自然光催化下降解RhB，其应用步骤如下：
(1)将30mg浓度为10.0mg/mL的RhB、2700μL浓度为0.1mg/mL的N,B,S-CDs和300μL浓度为3％H2O2溶液置于容器中；
(2)在黑暗条件下持续搅拌2h，使RhB和催化剂达到吸附-解析平衡；
(3)然后在300W氙灯模拟的自然光下持续照射并搅拌反应进行光催化降解实验，直到溶液无色。
步骤(3)中所述的自然光持续照射，光源距液面的髙度约为20cm。
步骤(3)中所述的自然光持续照射时间为90min。
步骤(3)中所述自然光光降解过程中反应液的温度维持在25℃左右。
本发明具有以下优点：
1.该荧光掺杂碳纳米N,B,S-CDs光催化剂的制备方法是一种低成本的制备方法。该方法具有合成原料成本低廉的优点。
2.该荧光掺杂碳纳米N,B,S-CDs光催化剂采用水热合成方法。该方法具有设备仪器简单、制备时间短、成本低等优点。
3.该荧光掺杂碳纳米N,B,S-CDs光催化剂制备方法简单、快速、无毒。具有环境友好的优点。
4.该荧光掺杂碳纳米N,B,S-CDs光催化剂在光催化降解RhB时，可以直接使用太阳光。具有适用范围广泛，使用方便的优点。
5.该荧光掺杂碳纳米N,B,S-CDs光催化剂在光催化降解RhB时快速、效率高。其降解率高达98.5％。
因此，本发明方法制备所得该荧光掺杂碳纳米N,B,S-CDs可以作为光催化降解RhB的催化剂。由于其该制备方法具有简单、低成本、快速、效率高等特征，具有很好的应用前景。
附图说明
图1.N,B,S-CDs的透射电镜图及粒径分布图；
图2.N,B,S-CDs的X射线光电子能谱图；
图3.N,B,S-CDs的荧光谱图和紫外吸收光谱图；
图4.N,B,S-CDs催化降解RhB的UV-Vis三维图；
图5.N,B,S-CDs在不同条件、不同时间催化降解RhB情况。
具体实施方式
实施例1
荧光掺杂碳纳米材料N,B,S-CDs的制备方法，具体步骤是：
称取2.1g柠檬酸、1.4g硫脲、1.4g硼酸、5mL乙二胺溶解在5mL水中，然后转移到聚四氟乙烯内衬的高压反应釜里，以每分钟10℃的速率加热至220℃，并保持3h，得到的红棕色溶液；用1molL-1NaOH溶液调节pH至7.0，然后离心8000rpm，20min，将所得水溶解进行，透析，分离未反应的物质得到棕色的N,B,S-CDs水溶液；旋转蒸发除去水，然后溶解在去离子水中于4℃避光保存。
实施例2
利用荧光掺杂碳纳米材料N,B,S-CDs光催化降解RhB的实验，具体步骤是：
向2700μLN,B,S-CDs(0.1mg/mL)和300μLH2O2(3％)的溶液中加入30mg的RhB(即浓度为10.0mg/mL)，所得混合溶液置于小烧杯里，先在黑暗条件下持续搅拌2h以使RhB和催化剂达到吸附-解析平衡，然后再在300W氙灯模拟的自然光下持续照射并搅拌反应进行光催化降解实验，光源距液面的髙度约为20cm，光降解过程中反应液的温度维持在25℃左右，持续光照90min，得到无色溶液。
分别取0、10、20、30、40、50、60、70、80和90min的溶液100μL测其UV-Vis光谱，记录RhB的最大吸收波长554nm对应的吸光度(见图4、图5)。实验结果表明，本发明荧光掺杂碳纳米材料N,B,S-CDs光催化剂能有效降解RhB，90min时降解率达到98.5％。
Claims (6)
1.一种荧光掺杂碳纳米N,B,S-CDs光催化剂的制备方法，其特征是：包括如下步骤：
(1)称取2.1g柠檬酸、1.4g硫脲、1.4g硼酸、5mL乙二胺溶解在5mL水中，然后转移到聚四氟乙烯内衬的高压反应釜里，以每分钟10℃的速率加热至220℃，并保持3h，得到的红棕色溶液；
(2)用1molL-1NaOH溶液调节pH至7.0，然后离心8000rpm，20min，将所得水溶解进行，透析，分离未反应的物质得到棕色的N,B,S-CDs水溶液；
(3)旋转蒸发除去水，得到荧光掺杂碳纳米N,B,S-CDs光催化剂，然后溶解在去离子水中于4℃避光保存。
2.用权利要求1所述的制备方法制备的荧光掺杂碳纳米N,B,S-CDs光催化剂。
3.权利要求2所述的荧光掺杂碳纳米N,B,S-CDs光催化剂在光催化降解RhB中的应用，其特征是：应用方法包括如下步骤：
(1)将30mg浓度为10.0mg/mL的RhB、2700μL浓度为0.1mg/mL的N,B,S-CDs和300μL浓度为3％H2O2溶液置于容器中；
(2)在黑暗条件下持续搅拌2h，使RhB和催化剂达到吸附-解析平衡；
(3)然后在300W氙灯模拟的自然光下持续照射并搅拌反应进行光催化降解实验，直到溶液无色。
4.根据权利要求3所述的应用，其特征是：所述的自然光持续照射，光源距液面的髙度约为20cm。
5.根据权利要求3所述的应用，其特征是：所述的自然光持续照射时间为90min。
6.根据权利要求3所述的应用，其特征是：所述自然光光降解过程中反应液的温度维持在25℃左右。
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