CN111977634A - 一种用于比色识别pH的量子点的制备方法 - Google Patents
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Abstract
本发明公开了一种用于比色识别pH的量子点的制备方法,属于纳米材料技术领域。本发明以常见的小分子为原料,包括如下步骤:1)称取一定量的尿素溶于去离子水中,加入一定量的对苯二胺,超声得到澄清溶液;2)将上述澄清溶液转移至PTFE内衬的水热反应釜,并将反应釜置于马弗炉中反应;3)反应结束后,待反应液体冷却至室温后,对其进行过滤、透析等处理,得到澄清的量子点水溶液;4)将上述量子点水溶液进行冷冻干燥得到量子点粉末。本发明制备的量子点在不同pH环境下,显示出不同的颜色,并且通过肉眼可直接清晰观察,可应用在pH的检测与传感、食品、生物检测等领域。
Description
技术领域
本发明属于纳米功能材料领域,具体地说,涉及一种用于肉眼比色识别的具有pH响应性的量子点的制备方法。
背景技术
近些年来,关于量子点的研究成为材料领域科研工作者们的研究热点。量子点是一类零维材料,其各个维度上的尺寸都为纳米级别,尺寸上的优势赋予其独特的性质,例如:光致发光,化学稳定性,优异的生物相容性和无毒性。常见的量子点一般是由半导体材料组成,又称为半导体纳米晶体,是介于分子与晶体之间的一种过渡态,具有独特的光学性质和电学性质,如荧光强度高、耐光漂白、激发波长范围比较宽、发射峰形比较窄、发射波长可调控等特点,但是半导体量子点的毒性和潜在的危害性限制了它的应用。近年来,硅量子点、碳量子点以及贵金属纳米簇的出现,进一步拓宽了量子点的范畴。新型量子点的开发,为寻找适合于生物标记、疾病探测以及药物输送等生物化学领域中所需的优异纳米材料带来了可能,具有重要的研究意义。
碳量子点作为其中重要的一员,具有良好的生物相容性、化学稳定性。近来,基于碳量子点的刺激响应的光学传感器因其快速的响应时间以及简单的操作而备受关注。尤其是关于pH和温度的传感***,因为pH和温度是一类重要的基本参数,在环境、食品以及生物医学领域都有重要的意义。但是,通常它们的感应范围较窄,且测试结果不容易捕捉。
发明内容
发明目的:为了解决上述问题,本发明提供一种用于比色识别pH的量子点的制备方法,并用于直接肉眼比色的方式判断pH值,此制备方法操作简便,且其比色结果具有可靠性。
为了实现上述发明目的,是以尿素和对苯二胺为原料,本发明采用的技术方案如下:
1)称取一定量的尿素溶于去离子水中,加入一定量的对苯二胺,超声得到澄清溶液;
2)将上述澄清溶液转移至PTFE内衬的水热反应釜,并将反应釜置于马弗炉中反应一定时间;
3)反应结束后,待反应液体冷却至室温后,对其进行过滤、透析等处理,得到澄清的量子点水溶液;
4)将上述量子点水溶液进行冷冻干燥得到量子点粉末。
所述的用于比色识别pH的量子点的制备方法,尿素和对苯二胺的质量比为1∶1-1∶5;
所述的用于比色识别pH的量子点的制备方法,反应温度为180-260℃;
所述的用于比色识别pH的量子点的制备方法,反应时间为8-36h;
所述的用于比色识别pH的量子点的制备方法,所使用的过滤孔径为0.22-0.45μm;
所述的用于比色识别pH的量子点的制备方法,透析袋的截留分子量为7000-14000Da,透析时间为3-15天。
有益效果:与现有技术相比,本发明具有以下优势:
1)本发明所使用的方法简单,原料易得,对环境友好且成本低;
2)本发明制备的量子点具有良好的粒径分布,尺寸均一;
3)本发明制备的量子点具有良好的分散性和稳定性,可分散于不同pH值的水溶液中;
4)本发明制备的量子点对环境的pH值具有响应性,在不同的pH值下显示出不同的颜色,肉眼可清晰辨别。
附图说明
图1为本发明实施例1制备的量子点的粒径分布图。
图2为本发明实施例1制备的量子点对不同pH响应的颜色照片(pH=2,4,6,8,11)。
具体实施方式
实施例1
(1)称取100mg尿素溶于去离子水中,加入100mg对苯二胺,超声得到均匀的澄清溶液;
(2)将上述澄清溶液转移至PTFE内衬的水热反应釜,并将反应釜置于马弗炉中250℃反应12h;
(3)反应结束后,待反应液体冷却至室温,使用0.22μm的针筒过滤器进行过滤,再使用截留分子量为14000Da的透析袋透析10天,期间每小时换一次水,得到澄清的量子点水溶液;
(4)将上述量子点水溶液进行冷冻干燥得到量子点粉末。
实施例2
(1)称取60mg尿素溶于去离子水中,加入300mg对苯二胺,超声得到均匀的澄清溶液;
(2)将上述澄清溶液转移至PTFE内衬的水热反应釜,并将反应釜置于马弗炉中200℃反应26h;
(3)反应结束后,待反应液体冷却至室温,使用0.45μm的针筒过滤器进行过滤,再使用截留分子量为3500Da的透析袋透析7天,期间每小时换一次水,得到澄清的量子点水溶液;
(4)将上述量子点水溶液进行冷冻干燥得到量子点粉末。
实施例3
(1)称取80mg尿素溶于去离子水中,加入160mg对苯二胺,超声得到均匀的澄清溶液;
(2)将上述澄清溶液转移至PTFE内衬的水热反应釜,并将反应釜置于马弗炉中220℃反应20h;
(3)反应结束后,待反应液体冷却至室温,使用0.22μm的针筒过滤器进行过滤,再使用截留分子量为7000Da的透析袋透析14天,期间每小时换一次水,得到澄清的量子点水溶液;
(4)将上述量子点水溶液进行冷冻干燥得到量子点粉末。
实施例4
(1)称取50mg尿素溶于去离子水中,加入200mg对苯二胺,超声得到均匀的澄清溶液;
(2)将上述澄清溶液转移至PTFE内衬的水热反应釜,并将反应釜置于马弗炉中180℃反应15h;
(3)反应结束后,待反应液体冷却至室温,使用0.22μm的针筒过滤器进行过滤,再使用截留分子量为14000Da的透析袋透析8天,期间每小时换一次水,得到澄清的量子点水溶液;
(4)将上述量子点水溶液进行冷冻干燥得到量子点粉末。
实施例5
(1)称取70mg尿素溶于去离子水中,加入210mg对苯二胺,超声得到均匀的澄清溶液;
(2)将上述澄清溶液转移至PTFE内衬的水热反应釜,并将反应釜置于马弗炉中240℃反应36h;
(3)反应结束后,待反应液体冷却至室温,使用0.45μm的针筒过滤器进行过滤,再使用截留分子量为3500Da的透析袋透析15天,期间每小时换一次水,得到澄清的量子点水溶液;
(4)将上述量子点水溶液进行冷冻干燥得到量子点粉末。
以上对本发明的几项具体实施例进行了描述。但是需要注意的是,本发明不局限于上述几种实施方式,可以做出多种改变,而不脱离本发明的实质内容。
Claims (8)
1.一种用于比色识别pH的量子点的制备方法,其特征在于:碳量子点具备pH的响应性,可以直接用肉眼比色识别pH。
2.根据权利要求1所述的用于比色识别pH的量子点的制备方法,其特征在于:量子点的尺寸范围为1-6nm。
3.一种制备权利要求1-2任一项所述的用于比色识别pH的量子点的制备方法,包括以下步骤:
称取一定量的尿素溶解在去离子水中,加入一定量的对苯二胺,超声得到澄清溶液,将其置于水热反应釜中反应,所得溶液经过滤、透析、冷冻干燥,得到量子点粉末。
4.根据权利要求3所述的方法,其特征在于:尿素和对苯二胺的质量比为1∶1-1∶5。
5.根据权利要求3所述的方法,其特征在于:反应温度为180-260℃。
6.根据权利要求3所述的方法,其特征在于:反应时间为8-36h。
7.根据权利要求3所述的方法,其特征在于:所使用的过滤孔径为0.22-0.45μm。
8.根据权利要求3所述的方法,其特征在于:所使用的透析袋截留分子量为7000-14000Da,透析时间为3-15天。
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