CN113088284A - 有机染料制备荧光石墨烯量子点的方法及应用 - Google Patents
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Abstract
本发明提供了一种从有机染料直接制备荧光石墨烯量子点的方法及应用，为水中有机染料的无污染降解及重新利用提供了全新的解决方案。本发明涉及的有机染料包括：橙黄II (AO7)，亚甲基蓝(MB)，活性蓝19 (RB19)和甲基橙(MO)。发现有机染料橙黄II (AO7)可经水热法直接生成具有强绿色荧光的石墨烯量子点。该石墨烯量子点溶液作为检测金属离子的荧光探针有显著的效果，能够在30 s内对水中的金属离子Fe3+做到快速响应。
Description
技术领域
本发明涉及本发明提供了一种从有机染料直接制备石墨烯量子点的方法及应用，为水中有机染料的无污染降解及重新利用提供了全新的解决方案。属于环境保护及纳米材料领域。
背景技术
在过去的几十年里，由于全球淡水危机和工业废水污染问题的异常增长，水处理引起了人们的广泛关注。有机化合物染料，如橙黄II (AO7)，亚甲基蓝(MB)，活性蓝19(RB19)和甲基橙(MO)等来自各种来源，包括工业废水和染料废水，是严重的水体污染物。除此之外，重金属离子对水资源的污染也无法忽视。这些有机有害物质及重金属离子毒性很高，即使浓度很低，也会对人类健康和生态系统造成相当大的损害和威胁，应通过科学的技术方法从水及时检测并将其清除。
发明内容
为了解决这些问题，本发明提供了一种从有机染料直接水热法制备石墨烯量子点及利用石墨烯量子点选择性检测水中金属离子的方法。与传统的采用高级氧化技术降解有机染料相比，直接水热法无需额外添加催化剂及氧化剂，更重要的是其产物为附加值更高的石墨烯量子点。
石墨烯量子点由于其量子限域和边缘效应，呈现出独特的光学和电子性质，具有更小的尺寸和更强的光致发光活性，越来越受到人们的关注。可以应用于许多领域，如光伏设备、细胞成像、药物递送、传感、荧光探针等应用。
现有技术中用有机染料直接水热法制备石墨烯量子点的方法尚未见报道；利用有机染料直接水热法得到的石墨烯量子点作为检测金属离子的荧光探针也尚未报道。所制备的石墨烯量子点荧光强度高、发光明显、对金属离子Fe3+的检测能够在30 s内显著响应，在荧光探针方面有广阔的应用前景。
针对上述技术问题，本发明提供了一种从有机染料直接制备石墨烯量子点的方法，所制备的石墨烯量子点可以发出强绿色荧光，具有优异的水溶性、荧光稳定性；同时发现该石墨烯量子点对金属离子Fe3+的检测能够在30s内显著响应，在荧光探针方面有广阔的应用前景。
所述其从有机染料制备石墨烯量子点的方法，具体步骤如下：
将有机染料橙黄II置于水热反应釜中，在温度为190-240℃下，水热反应时间为8-16 h，反应后的溶液离心过滤后即得到石墨烯量子点溶液。
有机染料橙黄II的质量浓度为1-5 mg/mL。
本发明的技术应用是采用从有机染料制备的石墨烯量子点用作荧光探针检测水中金属离子，具体是选择性检测水溶液中金属离子Fe3+，步骤如下：
步骤1：取制备的石墨烯量子点溶液，补加去离子水至浓度为0.05-4 mg/mL；
步骤2：吸取金属离子水溶液（所述的金属离子水溶液包括Fe3+、Fe2+、Co2+、Ni2+、Cr3 +、Ca2+、Al3+、Na+、Cu2+、K+、Zn2+，浓度为8 mmol/L）直接加入到步骤1溶液中，摇晃10-30s；
步骤3：取步骤2中溶液于石英比色皿中，在荧光分光光度计上检测溶液荧光强度值，并与不加金属离子的量子点溶液（Blank）的荧光强度做对比。
结果显示本发明的石墨烯量子点对Fe3+具有优异的选择性，Fe3+在30s内具有显著的量子点荧光淬灭效果，同时测得Fe3+检测范围为40 μM-1800 μM。
附图说明
图1为实施例1所制备的石墨烯量子点在365 nm紫外灯下的荧光照片，图1a为200℃，经不同水热反应时间制备的石墨烯量子点在365 nm紫外灯下的照片；图1b为不同温度下，经14h水热反应制备的石墨烯量子点在365 nm紫外灯下的照片。
图2为实施例1所制备石墨烯量子点的UV-vis光谱图。
图3为实施例1所制备的石墨烯量子点的透射电子显微镜图片及粒径分布图，其中3a为透射电子显微镜图片，图3b为粒径分布图片。
图4为实施例1所制备的石墨烯量子点的X-射线衍射图。
图5为实施例1所制备的石墨烯量子点的拉曼光谱图。
图6为实施例2亚甲基蓝(MB)，活性蓝19 (RB19)和甲基橙(MO)）产物溶液与橙黄II制备的石墨烯量子点的荧光强度对比图。
图7为实施例3 所制备的石墨烯量子点分别于与不同种金属离子混合后的荧光发射光谱图。
图8为实施例3所制备的石墨烯量子点对Fe3+的检测范围图。
具体实施方式
实施例1
从有机染料橙黄II (AO7)制备石墨烯量子点的方法具体步骤如下：
步骤1：取橙黄II染料150 mg，加入34 mL水后剧烈搅拌溶解，得到橙黄II水溶液；
步骤2：将步骤1中溶液倒入反应釜，将其置于干燥箱中，调节反应温度为190-240℃，反应时间为8-16h；
步骤3：将步骤2中反应后的溶液离心过滤后即得到石墨烯量子点溶液。
图1为实施例1所制备的石墨烯量子点在365 nm紫外灯下的荧光照片，图1a为200℃，经不同水热反应时间制备的石墨烯量子点在365 nm紫外灯下的照片；图1b为不同温度下，经14h水热反应制备的石墨烯量子点在365 nm紫外灯下的照片。
图2为实施例1所制备石墨烯量子点的UV-vis光谱图，反应温度为200℃，不同反应时间的产物溶液UV-vis谱图，图中反应6 h的UV-vis图显示500 nm左右范围的鼓包峰为原料AO7的紫外吸收特征峰，可以观察到在14 h反应时间下，AO7的特征峰降低完全，说明最佳反应时间及温度为14 h、200℃。
图3为图3为实施例1所制备的石墨烯量子点的透射电子显微镜图片及粒径分布图，其中3a为透射电子显微镜图片，图3b为粒径分布图片。图片说明石墨烯量子点的粒径分布主要集中在3-4 nm，平均粒径为3.54 nm。
图4为实施例1所制备的石墨烯量子点的X-射线衍射图，图片说明在24°有石墨的（002）晶面衍射峰，说明制备的材料中有石墨结构，进一步说明反应产物为石墨烯量子点。
图5为实施例1所制备的石墨烯量子点的拉曼光谱图，图中D峰代表石墨烯的无序振动峰、G峰是石墨烯的主要特征峰，说明石墨烯量子点存在石墨烯结构。
实施例2
200℃，14h反应条件下，从其它染料制备产物溶液的方法。
步骤1：取其它染料（甲基橙、亚甲基蓝或活性蓝19）150 mg，加入34 mL水后剧烈搅拌溶解，得到染料水溶液；
步骤2：将步骤1中溶液倒入反应釜，将其置于干燥箱中，调节反应温度为200℃，反应时间为14h；
步骤3：将步骤2中反应后的溶液离心过滤后即得到相对应染料产物溶液。
图6为实施例2 所制备的其它染料（包括亚甲基蓝(MB)，活性蓝19 (RB19)和甲基橙(MO)）产物溶液与橙黄II制备的石墨烯量子点的荧光强度对比图（测试条件为激发光带宽与发射光带宽为5 nm，改变激发波长为380 nm，检测发射波长从400 nm-700 nm的荧光发射峰），图中发现与橙黄II制备的石墨烯量子点溶液比较，其它染料（包括亚甲基蓝(MB)，活性蓝19 (RB19)和甲基橙(MO)）制得的产物荧光强度极低，无法进行金属离子检测应用。
实施例3
本发明采用实施例1制备得到的石墨烯量子点作为荧光探针检测水中金属离子，具体步骤如下：
步骤1：取制备的石墨烯量子点溶液（4mg/mL）0.1mL 补加去离子水3.6mL；
步骤2：吸取金属离子水溶液0.3mL直接加入到步骤1溶液中（所述的金属离子水溶液包括Fe3+、Fe2+、Co2+、Ni2+、Cr3+、Pd2+、Ca2+、Al3+、Cu2+、K+、Zn2+,浓度为8 mmol/L），摇晃30s；
步骤3：取步骤2中溶液于石英比色皿中，在荧光光度计上检测溶液荧光强度。
图7为实施例3 所制备的石墨烯量子点分别于与不同种金属离子混合后的荧光发射光谱图，图片说明在加入不同金属离子后，与Blank对照，混合Fe3+后能够引起荧光强度显著降低，而加入其它金属离子（曲线从上到下依次为Blank、Na+、K+、Ni2+、Al3+、Ca2+、Zn2+、Co2 +、Fe2+、Cu2+、Cr3+）后，溶液的荧光强都没有发生明显下降。从而达到选择性检测金属离子的目的。
图8为实施例3所制备的石墨烯量子点对Fe3+的检测范围图，曲线从上至下依次为添加了不同量的Fe3+后的荧光发射图，说明测得Fe3+检测范围为40 μM-1800 μM。
Claims (5)
1.一种有机染料制备荧光石墨烯量子点的制备方法，其特征在于，将有机染料橙黄II置于水热反应釜中，在温度为190-240℃下水热反应时间为8-16 h，即可制备得到荧光石墨烯量子点。
2.根据权利要求1所述的有机染料制备荧光石墨烯量子点的制备方法，其特征在于，有机染料橙黄II溶液的质量浓度为1-5 mg/mL。
3.根据权利要求1或2所述制备得到的荧光石墨烯量子点在选择性检测水溶液中金属离子Fe3+上的应用。
4.根据权利要求3所述的应用，其特征在于，荧光石墨烯量子点的浓度为0.05-4 mg/mL。
5.根据权利要求3所述的应用，其特征在于，Fe3+的检测范围为40 μM-1800 μM。
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