CN107601467B - 一种油溶性石墨烯量子点的制备方法 - Google Patents

一种油溶性石墨烯量子点的制备方法 Download PDF

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CN107601467B
CN107601467B CN201710946525.8A CN201710946525A CN107601467B CN 107601467 B CN107601467 B CN 107601467B CN 201710946525 A CN201710946525 A CN 201710946525A CN 107601467 B CN107601467 B CN 107601467B
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graphene quantum
quantum dots
citric acid
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CN107601467A (zh
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李忠平
朱瑞琦
杨振华
张月霞
李红荣
双少敏
董川
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Shanxi University
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Abstract

本发明提供了一种油溶性石墨烯量子点的制备方法，属于纳米材料制备技术领域。该方法包括如下步骤：(1)取柠檬酸置于容器中于180‑250℃加热熔化，直到柠檬酸变为橙色；(2)在橙色的柠檬酸热解液中加入适量油胺，于180‑250℃反应3‑8min；(3)停止加热，将上述反应物逐滴加入甲苯中，剧烈震荡，直到完全混匀；(4)在上述混匀的甲苯溶液中加入水，缓慢摇匀，静置，直到溶液分层；(5)取上层甲苯层，经冷冻干燥，得到的固体粉末即为油溶性石墨烯量子点。本发明制备的油溶性石墨烯量子点纯度较高；本发明所用试剂常见、易得，方法简单，易于大规模制备。

Description

一种油溶性石墨烯量子点的制备方法
技术领域
本发明涉及纳米材料的制备，具体属于一种油溶性石墨烯量子点的制备方法。
背景技术
石墨烯量子点是尺寸小于10nm的石墨烯薄片。石墨烯量子点具有许多优异的性能，比如说较大的表面积，较高的机械性能，较高的电子迁移率，而且具有较好的生物相容性，因此在生物医学，电子材料，光学材料，磁性材料及环境检测等领域具有重要的应用前景。
石墨烯量子点的制备方法主要分为两类，自上而下法和自下而上法。自上而下法是指将石墨烯片经过化学或物理处理，从而得到石墨烯量子点，具体包括电化学法，水热法，化学剥离碳纤维法等；自下而上法是指把一些小分子当做反应前体，经过一系列化学反应步骤而得到石墨烯量子点，具体包括化学气相沉积法，热解法，微波法等。
目前油溶性石墨烯量子点一般为先合成量子点，然后再对其进行功能化修饰。但实现过程步骤繁琐，难以推广。CN201710381811公开了一种氮掺杂石墨烯量子点的熔融制备方法，在熔融条件下可以获得氮掺杂石墨烯量子点。但该方法制备的石墨烯量子点为水溶性，不是油溶性。而且该方法制备的量子点纯度难以得到保证。
发明内容
本发明的目的在于提供一种简单有效的油溶性石墨烯量子点的制备方法。
本发明提供的一种油溶性石墨烯量子点的制备方法，包括如下步骤：
(1)取柠檬酸置于容器中于180-250℃加热熔化，直到柠檬酸变为橙色；
(2)在橙色的柠檬酸热解液中加入适量油胺，于180-250℃反应3-8min；
(3)停止加热，将上述反应物逐滴加入甲苯中，剧烈震荡，直到完全混匀；
(4)在上述混匀的甲苯溶液中加入水，缓慢摇匀，静置，直到溶液分层；
(5)取上层甲苯层，经冷冻干燥，得到的固体粉末即为油溶性石墨烯量子点。
所述步骤(1)中的柠檬酸为纯度99.5％的分析纯柠檬酸；步骤(2)中的油胺为分析纯油胺；步骤(3)中的甲苯为分析纯甲苯；步骤(4)中的水为去离子水。
与现有技术相比本发明具有如下有益效果：
1、本发明制备的油溶性石墨烯量子点通过冷冻干燥后可以去除甲苯及其未反应完全的油胺，因此纯度较高。
2、本发明所用试剂常见、易得，方法简单，易于大规模制备。
附图说明
附图1本发明制备的油溶性石墨烯量子点投射电镜图。
附图2本发明制备的油溶性石墨烯量子点的甲苯溶液的紫外-可见光谱。
附图3本发明制备的油溶性石墨烯量子点的甲苯溶液的荧光发射光谱(激发光波长为420纳米)。
具体实施方式：
实施例1
(1)称取柠檬酸4g置于25ml烧杯中在200℃加热，直到柠檬酸熔化、热解液变为橙色(55min)；
(2)在橙色柠檬酸热解液中加入0.5ml油胺，200℃反应6min；
(3)停止加热，将上述柠檬酸与油胺反应物加入100ml甲苯中，剧烈震荡，直到完全混匀；
(4)在上述溶液中加入100ml水，摇匀，静置，直到溶液出现清晰分层；
(5)取上层甲苯层，将甲苯层经冷冻干燥36h得到固体粉末0.08g，即为油溶性石墨烯量子点。
实施例2
(1)称取柠檬酸4g置于25ml烧杯中在220℃加热，直到柠檬酸熔化、热解液变为橙色(43min)；
(2)在橙色柠檬酸热解液中加入1ml油胺，220℃反应8min；
(3)停止加热，将上述柠檬酸与油胺反应物加入100ml甲苯中，剧烈震荡，直到完全混匀；
(4)在上述溶液中加入100ml水，摇匀，静置，直到溶液出现清晰分层；
(5)取上层甲苯层，将甲苯层经冷冻干燥36h得到固体粉末0.11g，即为油溶性石墨烯量子点。

Claims (2)

1.一种油溶性石墨烯量子点的制备方法，其特征在于包括如下步骤：
(1)取柠檬酸置于容器中于180-250℃加热熔化，直到柠檬酸变为橙色；
(2)在橙色的柠檬酸热解液中加入适量油胺，于180-250℃反应3-8min；
(3)停止加热，将上述反应物逐滴加入甲苯中，剧烈震荡，直到完全混匀；
(4)在上述混匀的甲苯溶液中加入水，缓慢摇匀，静置，直到溶液分层；
(5)取上层甲苯层，经冷冻干燥，得到的固体粉末即为油溶性石墨烯量子点。
2.如权利要求1所述的油溶性石墨烯量子点的制备方法，其特征在于所述步骤(4)中的水为去离子水。
CN201710946525.8A 2017-10-12 2017-10-12 一种油溶性石墨烯量子点的制备方法 Active CN107601467B (zh)

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