CN114045171B - 一种手性碳量子点的制备方法 - Google Patents

一种手性碳量子点的制备方法 Download PDF

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CN114045171B
CN114045171B CN202111487063.0A CN202111487063A CN114045171B CN 114045171 B CN114045171 B CN 114045171B CN 202111487063 A CN202111487063 A CN 202111487063A CN 114045171 B CN114045171 B CN 114045171B
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carbon quantum
chiral carbon
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覃爱苗
凡新刚
蒋丽
廖雷
覃迎喜
孙伟
杨莉花
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Guilin University of Technology
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Abstract

本发明公开了一种手性碳量子点的制备方法。(1)将2~3g甘蔗糖蜜和0.1g~0.2g的L‑半胱氨酸依次加入到20~30mL的超纯水中搅拌混合均匀;(2)将混合溶液进行超声和离心,加入到聚四氟乙烯内衬中,加至体积为聚四氟乙烯内衬体积的75%~80%,并装入反应釜的不锈钢的钢套中;(3)将反应釜置于真空干燥箱中,升温至120℃~165℃下水热反应20~24小时,冷却至室温,过滤和离心,得手性碳量子点。本发明成本低廉,工艺简单,条件易控,制得的手性碳量子点不仅继承了手性性质且具备优异的荧光性能,能作为纳米发光材料应用在荧光传感器或手性识别方面。

Description

一种手性碳量子点的制备方法
技术领域
本发明涉及一种以甘蔗糖蜜为碳源,L-半胱氨酸为手性源来制备手性碳量子点的方法。
背景技术
手性碳量子点不仅具备手性性质,而且也继承了碳量子点的光致发光强度高、毒性低、生物相容性好等优异的性能,在传感器、手性识别等领域展现出了巨大的应用前景。现有合成碳量子点的原料多采用柠檬酸,合成方法多数是化学氧化法或高温热解法,其原料成本昂贵,工艺复杂,工艺条件可控性不强,限制了其进一步应用。
因此,需要开发一种成本低廉,制备工艺简单的合成手性碳量子点的方法,用来推进进一步的应用。
发明内容
本发明的目的在于克服现有技术中手性碳量子点成本昂贵,制备工艺复杂,工艺条件可控性不强等缺陷,提供一种手性碳量子点的制备方法。
具体步骤为:
(1)将2~3g甘蔗糖蜜和0.1g~0.2g的L-半胱氨酸依次加入到20~30mL的超纯水中搅拌混合均匀,形成混合溶液。
(2)将步骤(1)所得混合溶液进行超声和离心,最后将离心好的溶液,加入到聚四氟乙烯内衬中,加至体积为聚四氟乙烯内衬体积的75%~80%,并装入反应釜的不锈钢的钢套中,旋紧。
(3)将步骤(2)反应釜置于真空干燥箱中,升温至120℃~165℃下水热反应20~24小时,待冷却至室温,将产物进行过滤和离心,所得上清液即为手性碳量子点。
控制反应温度、时间和L-半胱氨酸加入量的合成手性碳量子点的关键步骤。本发明的发明人通过研究发现,当选用L-半胱氨酸在0.2g,温度在160℃,时间在24小时,其合成的手性碳量子点的手性能够很好的继承在碳量子点中,且具备优异的荧光性能,相比碳量子点具有更高的荧光强度。
本发明成本低廉,制备工艺简单,工艺条件容易控制,制备得到的手性碳量子点不仅继承了手性性质而且具备优异的荧光性能,能作为纳米发光材料应用在荧光传感器或手性识别方面。
附图说明
图1为实施实例1制得的手性碳量子点的CD图。
图2为实施实例1制得的手性碳量子点的荧光发射光谱对比图。
图3为实施实例2制得的手性碳量子点的CD图。
具体实施方式
实施例1:
(1)将2.874g甘蔗糖蜜和0.2g的L-半胱氨酸依次加入到28.2mL的超纯水中搅拌混合均匀,形成混合溶液。
(2)将步骤(1)所得混合溶液进行超声10分钟,在7500r/min的离心机上离心10分钟,最后将离心好的溶液放入到50mL的聚四氟乙烯内衬中并装入水热反应釜的不锈钢的钢套中,旋紧。
(3)将步骤(2)反应釜置于真空干燥箱中,升温至160℃下水热反应24小时,待冷却至室温,将产物进行过滤和离心,所得上清液即为手性碳量子点。
(4)取步骤(3)中少量上清液并稀释1000倍,在200nm~400nm范围内测试其圆二色性光谱(CD),在205nm附近会出现一个向上的手性信号,从而说明合成了手性碳量子点。
(5)取步骤(3)中少量上清液并用超纯水稀释100倍,在电压为600v,激发狭缝和发射狭缝为5nm的荧光分光光度计上检测,当激发波长在348nm时,手性碳量子点在400nm~450nm荧光强度最大,与碳量子点相比其荧光强度有较高的提高。
实施例2:
(1)称取2.874g甘蔗糖蜜溶解在28.2mL的超纯水中,随后添加0.2g L-半胱氨酸。
(2)将步骤(1)所得混合溶液进行超声10分钟,在7500r/min的离心机上离心10分钟,最后将离心好的溶液放入到50mL的聚四氟乙烯内衬中并装入水热反应釜的不锈钢的钢套中,旋紧。
(3)将步骤(2)反应釜置于真空干燥箱中,升温至140℃下水热反应24小时,待冷却至室温,将产物进行过滤和离心,所得上清液即为手性碳量子点。
(4)取步骤(3)中少量上清液并稀释1000倍,在200nm~400nm范围内测试其圆二色性光谱(CD),在205nm附近会出现一个向上的手性信号,从而说明合成了手性碳量子点。
(5)取步骤(3)中少量上清液并用超纯水稀释100倍,在电压为600v,激发狭缝和发射狭缝为5nm的荧光分光光度计上检测,当激发波长在348nm时,手性碳量子点在400nm~450nm荧光强度最大,与碳量子点相比其荧光强度有较高的提高。

Claims (1)

1.一种手性碳量子点的制备方法,其特征在于具体步骤为:
(1)将2~3g甘蔗糖蜜和0.1g~0.2g的L-半胱氨酸依次加入到20~30mL的超纯水中搅拌混合均匀,形成混合溶液;
(2)将步骤(1)所得混合溶液进行超声和离心,最后将离心好的溶液,加入在聚四氟乙烯内衬中,加至体积为聚四氟乙烯内衬体积的75%~80%,并装入反应釜的不锈钢的钢套中,旋紧;
(3)将步骤(2)反应釜置于真空干燥箱中,升温至120℃~165℃下水热反应20~24小时,待冷却至室温,将产物进行过滤和离心,所得上清液即为手性碳量子点。
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