碱木质素/聚乙烯亚胺碳点的制备及其对pH敏感性

doi:10.16085/j.issn.1000-6613.2018-2348

化工进展 ›› 2019, Vol. 38 ›› Issue (04): 1970-1977.DOI: 10.16085/j.issn.1000-6613.2018-2348

碱木质素/聚乙烯亚胺碳点的制备及其对pH敏感性

洪碧云¹(),唐丽荣^1,²(),陈伟香¹,黄彪¹

1. 福建农林大学材料工程学院，福建福州 350002
2. 福建农林大学金山学院，福建福州 350002

收稿日期:2018-12-03 修回日期:2019-01-02 出版日期:2019-04-05 发布日期:2019-04-05
通讯作者: 唐丽荣
作者简介:<named-content content-type="corresp-name">洪碧云</named-content>（1995-），女，硕士研究生，研究方向为林产化工与纳米材料。E-mail: <email>hongbiyun0625@163.com</email>。|唐丽荣，讲师，研究方向为生物质功能材料。E-mail: <email>tanglr0201@126.com</email>。
基金资助:
国家自然科学基金(31870561);福建省科技厅自然科学基金(2016J01088);福建省高校杰出青年科研人才培育计划(2017年度);福建农林大学"校杰出青年科研人才"培养专项基金(xjq201422)

Preparation of alkali lignin/polyethyleneimine carbon dots and their pH sensitivity

Biyun HONG¹(),Lirong TANG^1,²(),Weixiang CHEN¹,Biao HUANG¹

1. College of Material Engineering, Fujian Agriculture and Forestry University, Fuzhou 350002, Fujian, China
2. Jinshan College of Fujian Agriculture and Forestry University, Fuzhou 350002, Fujian, China

Received:2018-12-03 Revised:2019-01-02 Online:2019-04-05 Published:2019-04-05
Contact: Lirong TANG

摘要/Abstract

摘要：

以碱木质素（alkali lignin，AL）、聚乙烯亚胺（polyethylenimine，PEI）为碳源，其中PEI不仅作为碳源还作为表面钝化剂，在H₂O₂氧化下通过一步水热法绿色、高效制备高荧光、寿命长和多氨基化功能碳点（alkali lignin/polyethylenimine carbon dots，AL/PEI-CDs）。探究了碱木质素/PEI质量比、水热温度和水热时间等因素对碳点荧光强度的影响，确定了最佳的反应条件，同时考察了AL/PEI-CDs对pH的敏感性及稳定性。采用紫外分光光度计（ultraviolet spectrophotometer，UV-vis）、荧光分光光度计、原子力显微镜（atomic force microscope，AFM）、高分辨透射显微镜（high resolution transmission electon microscopy，HRTEM）、傅里叶红外光谱仪（Fourier transform infrared spectroscopy，FTIR）和X射线衍射仪（X-ray diffractometer，XRD），对AL/PEI-CDs的光学性质、形貌结构、化学结构和晶体结构等进行了表征分析。结果表明，在碱木质素/PEI质量比为1∶12、水热温度190℃、水热时间12h的条件下，合成的AL/PEI-CDs荧光量子产率为25.53％，荧光寿命为5.06ns，表面含有丰富的氨基和羟基，且粒径均一、水溶性好，有良好的稳定性，在最佳激发波长为ex=313nm下对应的发射峰位为405nm，稀释液在紫外灯下发出明亮的蓝光。本研究制备的碳点在离子监测和细胞代谢过程监测质子传感器中可能具有良好的应用前景。

关键词: 碳点, 碱木质素, 聚乙烯亚胺, 水热法

Abstract:

Alkali lignin (AL) and polyethylenimine (PEI) were used as carbon sources. PEI was used not only as a carbon source but to efficiently prepare the also as a surface passivator. Under the oxidation of H₂O₂, it was one step hydrothermal green method to efficiently prepare the high fluorescence, long life and polyethylenimine carbon dots (AL/PEI-CDs). The effects of alkali lignin/PEI mass ratio, hydrothermal temperature and hydrothermal time on the fluorescence intensity of carbon dots were studied. The optimal reaction conditions were determined. The sensitivity and stability of AL/PEI-CDs to pH were also investigated. Ultraviolet spectrophotometer (UV-vis), fluorescence spectrophotometer, atomic force microscope (AFM), high resolution transmission electron microscopy (HRTEM), Fourier infrared spectrometer (Fourier), the optical properties, morphology, chemical structure and crystal structure of AL/PEI-CDs were characterized by transform infrared spectroscopy (FTIR) and X-ray diffractometer (XRD). The results showed that the fluorescence quantum yield (QY) of the synthesized AL/PEI-CDs was 25.53%, fluorescence under the condition of alkali lignin/PEI mass ratio of 1∶12, hydrothermal temperature of 190℃ and hydrothermal time of 12h. The life was 5.06ns, the surface was rich in amino and hydroxyl groups, and the particle size was uniform, water-soluble and good stability. The corresponding emission peak was 405 nm at the optimal excitation wavelength of ex=313nm. Bright blue light was emitted under the UV lamp. The carbon dots prepared in this study may have good application prospects in ion monitoring and cell metabolic process monitoring proton sensors.

Key words: carbon dots, alkali lignin, polyethylenimine, hydrothermal method

中图分类号:

O613.71

洪碧云, 唐丽荣, 陈伟香, 黄彪. 碱木质素/聚乙烯亚胺碳点的制备及其对pH敏感性[J]. 化工进展, 2019, 38(04): 1970-1977.

Biyun HONG, Lirong TANG, Weixiang CHEN, Biao HUANG. Preparation of alkali lignin/polyethyleneimine carbon dots and their pH sensitivity[J]. Chemical Industry and Engineering Progress, 2019, 38(04): 1970-1977.

图/表 10

图1 AL/PEI-CDs合成与纯化示意图

图2 AL/PEI-CDs水溶液的紫外-可见吸收光谱、荧光光谱不同波长激发下的发射光谱

图3 碱木质素/PEI的质量比对荧光强度的影响

图4 反应温度对荧光强度的影响

图5 反应时间对荧光强度的影响

图6 AL/PEI-CDs的荧光寿命

图7 碳点的形貌

图8 碱木质素、PEI和AL/PEI-CDs的红外光谱图

图9 碱木质素、PEI和AL/PEI-CDs的XRD谱图

图10 AL/PEI-CDs的pH依赖性荧光发射光谱和zeta电位随pH的变化

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碱木质素/聚乙烯亚胺碳点的制备及其对pH敏感性

Preparation of alkali lignin/polyethyleneimine carbon dots and their pH sensitivity

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