现代化工

现代化工 ›› 2025, Vol. 45 ›› Issue (4) : 25-29. DOI: 10.16606/j.cnki.issn0253-4320.2025.04.005

技术进展

碳点基水凝胶的合成、特性与环境应用

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Synthesis,characterization and environmental applications of carbon dots-based hydrogel

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文章历史 +

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摘要

综述了碳点基水凝胶(CDH)的制备方法、特性及其在水污染治理中的应用。介绍了CDH的合成方法,包括碳点的合成技术路线(自上而下和自下而上方法)以及碳点与水凝胶的结合方式(独立合成与原位合成)。研究总结了CDH在检测和吸附水体污染物方面的性能,探讨了荧光猝灭和增强机制,以及静电相互作用、离子交换和表面络合等吸附机理。CDH凭借荧光稳定性和高吸附能力,在重金属离子、有机化合物和抗生素的检测与去除中展现出显著优势,具有广泛的应用前景。尽管如此,CDH在动态条件下的稳定性以及传感功能的集成仍需进一步优化,最后提出了未来研究方向,包括优化碳点设计、简化生产工艺、提高材料稳定性和开发配套分析技术,以推动CDH在环境保护和可持续发展中的应用。

Abstract

The preparation methods and characteristics of carbon dot-based hydrogel (CDH),as well as its application in treatment of water pollution are reviewed.The synthetic methods of CDH are introduced,including the synthesis technology route of carbon dots (top-down and bottom-up methods) and the combination mode of carbon dots and hydrogel (independent synthesis and in-situ synthesis).The performance of CDH in detecting and adsorbing pollutants in water is researched and summarized.The detection mechanism of CDH,involving fluorescence quenching and fluorescence enhancing,is explored,and the corresponding adsorption mechanism such as electrostatic interaction,ion exchange,and surface complexation is also expounded.Given the fluorescence stability and high adsorption ability,CDH displays significant superiority in detecting and removing heavy metal ions,organic compounds and antibiotics,showing a promising application prospect.However,the stability of CDH under dynamic conditions and the integration of its sensing functions still need further optimization.The research directions for CDH in the future is also proposed,such as optimizing the design of carbon dots,simplifying the production process,improving the stability of materials,and developing the matched analysis technology,aiming to promote the application of CDH in environmental protection and sustainable development.

Graphical abstract

关键词

碳点 / 检测与吸附 / 污染物 / 荧光性 / 水凝胶

Key words

carbon dots / detection and adsorption / pollutants / fluorescence / hydrogel

Author summay

刘旭亮(1996-),男,硕士生。

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由于全球人口激增、工业化步伐加快和城市化水平不断提升,水污染已成为国际社会亟需解决的重大问题。碳点(CDs)作为一种新兴的纳米材料,以生物相容性、荧光稳定性和原料易得等特性,在水污染治理研究中受到广泛关注。CDs能对废水中的重金属离子和有机污染物产生特异性荧光变化,为水体污染物的快速检测提供了创新途径,通过精细调控合成策略,CDs在污染物检测中实现了极低的检测限。然而,碳点以粉末或溶液形式存在,在使用过程中存在灵活性和便携性不足,限制了在环境监测中的广泛应用。此外,复杂的样品分离过程加剧了环境污染和经济成本。

水凝胶作为多功能载体,凭借3D聚合物网络为小分子提供丰富的结合位点。但其本身性能较差,需要通过改性来满足不同应用的需要,水凝胶的改性主要通过2种方法实现:化学改性和物理改性。化学改性涉及使用各种引发剂、交联剂或功能单体,通过共价键合或非共价相互作用,增强水凝胶的化学稳定性和反应活性^[1];物理改性则通过改变水凝胶的微观结构,如通过冷冻干燥、热处理或机械加工等方法提高机械强度和耐久性。经过化学改性或物理改性后,水凝胶在吸附效率、溶胀平衡、孔隙构造等性能^[2]均获得了显著提升,特别是对水体中污染物的吸附性能。

碳点基水凝胶(CDH)由碳点和水凝胶单元协同构建,实现了两者特性的互补优势,物理缔合作用使碳点与水凝胶聚合物单体结合,增强了水凝胶的机械强度,同时碳点表面的官能团对水体污染物具有显著的诱导吸附作用,显著提升了吸附效率^[3];此外,水凝胶的三维网络为碳点提供了稳定的支撑,提高了碳点的荧光稳定性和传感效果,避免产生聚集诱导的荧光淬灭现象^[4]。与传统的水溶液体系相比,CDH的固态基质特性提升了量子点在保存、运输和回收过程的便携性^[5],从而在实际应用中展现出显著的优势。

本研究综述了CDH的制备方法,并探讨了其在污染物检测与吸附中的应用。总结了CDH在水污染治理中的技术进展,并讨论了在环保和可持续发展中的潜在贡献。重点强调了CDH作为新型环保材料的重要性,以及在推动绿色高效环保技术中的关键作用。

1 CDH的合成方法

1.1 CDH合成

在CDH体系中,碳点作为关键组分,是调节水凝胶荧光特性的关键因素之一。碳点的合成可通过2种主要技术路线实现:自上而下和自下而上方法(见图1)。自上而下方法利用高温热解、溶剂热解等方式将大分子前体分解,从而获得碳点;自下而上方法则通过有机小分子等简单前体逐步聚合形成碳点。在CDH的应用中,自下而上方法合成的碳点溶液更易与水凝胶相结合,形成复合体系。此外,根据碳点是否直接参与水凝胶部分的合成,CDH的制备方法又分为2种。一种涉及水凝胶和碳点悬浮液的独立合成,之后通过混合工艺进一步合成CDH。此法便于对CDH的物理化学性质进行定向调控,为材料的工业化生产提供了理论基础。另一种则采用原位合成策略,在碳点悬浮液中直接形成水凝胶网络,此方法的优势在于简化了合成步骤、提高了合成效率。

1.2 CDH锚定

在CDH体系中,水凝胶网络通过酰胺键和酯键实现对碳点的有效整合,这种化学键不仅增强了碳点与水凝胶的相互作用,而且有助于构建稳定的互穿网络结构,提升材料的综合性能。Cui等^[6]通过聚乙烯亚胺衍生的碳点和二醛淀粉水凝胶之间的席夫碱反应[图2(a)]成功制备了具有增强微孔均匀性的CDH。Sheng等^[7]利用大蒜汁和果胶、丙烯酸制备的水凝胶与碳点之间通过酯键形成了互穿网络结构[图2(b)],获得了具有良好生物相容性的 CDs-PAA水凝胶。Hu等^[8]使用邻苯二胺碳点和聚丙烯酰胺水凝胶通过酰胺键连接[图2(c)],使其对Ag⁺的吸附性能超过251.4 mg/g。Wang等^[9]使用嗜盐柳和乙二胺制备碳点后和纤维素水凝胶之间通过酰胺键连接[图2(d)],合成的CDH对Fe³⁺最低检测限达到3.9 mg/L。Luo等^[10]使用乙二胺和柠檬酸制备碳点通过酰胺键和纳米原纤维水凝胶连接[图2(e)],通过掺杂α-FeOOH对Cr⁶⁺同时进行吸附和光降解,在80 min内对Cr⁶⁺的去除率达到100%。Du等^[11]采用柠檬酸制备的碳点与聚丙烯酸水凝胶发生酰胺基团的交联[图2(f)],获得了拉伸强度、断裂强度、抗压强度更高的水凝胶结构。碳点在水凝胶中均匀分布,提升了CDH的稳定性。

2 CDH对水体中污染物的检测和吸附

CDH凭借荧光性质和三维多孔结构,对水体中污染物实现了高效的检测与吸附。尤其在针对重金属离子、有机化合物和抗生素等污染物的处理上展现了广泛的应用潜力。

2.1 CDH对污染物的检测机理

CDH对污染物的检测依靠荧光性变化来进行,荧光猝灭机理主要由内滤效应、光致电子转移、静态猝灭、动态猝灭、Förster共振能量转移、聚集引起猝灭和荧光增强等来解释。Zhang等^[12]制备的CDH对四环素具有高灵敏荧光响应,当CDH与四环素相互作用后,由于CDH的荧光吸收峰与四环素的吸收峰之间的重叠效应,即内滤效应,使得CDH在 365 nm紫外光激发下的蓝色荧光发生猝灭。Dong等^[13]发现碳点在与锰离子混合后发生猝灭,锰离子氧化态由Mn⁷⁺降低为Mn⁴⁺。电子顺磁共振分析确认了CDs在该反应中作为电子供体。此外,氧化离子的添加导致CDs的ζ电位减少,这一现象为电子从CDs向锰离子转移提供了证据。据此,研究者分析,猝灭机理主要是由于在激发态下进行的氧化还原反应,即光诱导能量转移。Ma等^[14]发现加入Hg²⁺后的碳点发射峰高显著降低,这是因为荧光基团与Hg²⁺之间形成非荧光基态配合物,发生静态猝灭。Zhou等^[15]发现同一荧光基团与Cr⁶⁺发生内滤效应,而与Fe³⁺则形成非辐射配合物。动态猝灭是由于激发的荧光基团和污染物之间的碰撞而导致的电子转移,使荧光分子以无辐射形式跃迁回基态发生猝灭。黄金荣^[16]通过加入Cu²⁺前后荧光寿命变化,认为是激发态的电子转移到Cu²⁺的d轨道上,抑制了电子辐射的跃迁,发生动态猝灭。Förster共振能量转移发生在荧光基团和污染物相互靠得很近(1~10 nm)时,光子转移导致猝灭。Liao等^[17]通过荧光寿命的变化、荧光基团和污染物之间的距离提出,加入对硝基苯酚后碳点荧光猝灭的原因是FRET。聚集引起猝灭多发生在碳点荧光性检测上,而CDH由于其三维网络结构可以抑制荧光基团的聚集性猝灭。

尽管大多数CDH的检测是基于荧光猝灭现象,但是也有研究通过加入污染物后荧光增强的现象来进行检测。荧光性增强的机制是多方面的。Tang等^[18]在对Cd²⁺检测中检测到荧光强度增强,提出CDH的孤对电子与Cd²⁺的空轨道形成配合物。Li等^[19]观察到荧光强度增强且紫外吸收峰变宽发生红移,推测荧光增强的原因是发色团(C=O)和辅助色素(—OH,—NH₂)共存,即四环素分子中存在的C=O、—OH和—NH₂基团可以与氮掺杂碳点表面的—NH₂和—OH基团通过氢键相互作用,从而影响碳点的表面缺陷,最终导致荧光强度的增强。Niu等^[20]推测有2种可能,一是吸附物和CDH之间的静电排斥增加了两者之间的距离,减少非辐射跃迁从而导致荧光强度增强。二是吸附物作为配体消除了碳点的表面缺陷,增强荧光性。Liu等^[21]提出,CDH聚集导致芳香环和酚羟基旋转受限,增强了π共轭,减少了非辐射衰变。Ruiz-Palomero等^[22]提出由于π-π堆积相互作用,芳香族污染物与碳点之间的非共价相互作用得到加强导致CDH的荧光强度增强。荧光强度增强的原因较为复杂,具体机制仍需进一步深入研究。

2.2 CDH对污染物的吸附机理

CDH对污染物的吸附主要通过静电相互作用、离子交换和表面络合(包括配位/螯合)。前2种吸附机制通常是可逆的,再生后的吸附剂可重复使用。而表面络合涉及到吸附剂表面与吸附物之间的化学反应和化学键合,通常不可逆。CDH的吸附速率和适用性取决于目标污染物的种类、背景浓度以及水凝胶的表面性质(见表1),离子交换多发生在对重金属离子的吸附中,Zhang等^[23]合成了一种新型荧光淀粉基水凝胶(FSH),在检测Pb²⁺过程中发现Pb²⁺首先通过静电相互作用吸附在FSH表面,随后通过FSH三维结构中的离子传输通道与Na⁺之间发生离子交换。Hu等^[8]在对Ag⁺吸附后发现吸光度出现2个新的吸收峰,并根据XPS中C—O、C=O和Ag⁺峰面积变化分析原因是Ag⁺将C—O氧化为C=O后与Ag⁺形成非荧光配合物。Luo等^[24]在研究四环素的吸附过程中发现,四环素吸附前后CDH的FT-IR谱图中O—H和N—H的拉伸振动发生了显著变化。XPS O 1s光谱中—C、C=O、—COO和—OH结合能增加,提出四环素与—OH、—COOH之间出现非共价键结合,发生静电相互作用吸附。尽管已经开发了多种水凝胶基吸附剂用于水的高效净化,但CDH在动态条件下的稳定性和对污染物检测线性范围方面,仍存在进一步改进的空间。

此外,在对污染物的检测吸附完成后,未经处理的CDH可能成为环境二次污染的源头。为了解决这一问题,研究人员(Meetam等^[29]和Ali等^[30])通过向吸附了Cu²⁺的水凝胶中引入硼氢化钠,将Cu²⁺还原为铜纳米颗粒。这一过程不仅去除了水凝胶中的重金属,还合成了可用于催化还原4-硝基苯酚、刚果红和甲基橙的金属纳米颗粒。

3 结论和展望

CDH的原料来源广泛、成本低,是构建绿色、高效环保技术体系的核心材料。本项研究探讨了CDH在水污染治理中的应用,特别是在污染物检测与吸附机制中的关键作用。CDH结合了碳点的荧光特性和水凝胶的高吸附能力,通过物理缔合和化学锚定提高了材料的综合性能,尤其在检测和吸附水体中的重金属离子、有机化合物和抗生素等方面展现出了应用潜力。重点分析了对污染物的检测和吸附机理,主要包括荧光猝灭和增强机制,以及静电相互作用、离子交换和表面络合等吸附机制。

未来的研究应聚焦于以下几个方面:优化碳点的设计与合成,利用机器学习等方式进行材料设计;开发适用于大规模生产的简单工艺和纯化系统;提高CDH在实际应用中的便捷性和准确性,如开发配套软件分析荧光变化;解决水凝胶在动态条件下的稳定性问题和集成传感功能的需求;克服在现实水样中特定波长发射和收集的困难。通过这些研究,CDH有望在环境保护和可持续发展中发挥更大的作用,为全球水污染治理提供创新解决方案。

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