CN110452692B - 一种离子液体修饰的荧光碳点的制备和应用 - Google Patents

一种离子液体修饰的荧光碳点的制备和应用 Download PDF

Info

Publication number
CN110452692B
CN110452692B CN201910649556.6A CN201910649556A CN110452692B CN 110452692 B CN110452692 B CN 110452692B CN 201910649556 A CN201910649556 A CN 201910649556A CN 110452692 B CN110452692 B CN 110452692B
Authority
CN
China
Prior art keywords
fluorescent carbon
cds
ionic liquid
liquid modified
carbon dot
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201910649556.6A
Other languages
English (en)
Other versions
CN110452692A (zh
Inventor
吴大同
潘菲
高丽
孔泳
陶永新
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changzhou University
Original Assignee
Changzhou University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Changzhou University filed Critical Changzhou University
Priority to CN201910649556.6A priority Critical patent/CN110452692B/zh
Publication of CN110452692A publication Critical patent/CN110452692A/zh
Application granted granted Critical
Publication of CN110452692B publication Critical patent/CN110452692B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N2021/6432—Quenching

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Molecular Biology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

本发明属于纳米材料制备和光学传感检测领域，具体为一种离子液体修饰的荧光碳点的制备和应用。主要包括以下步骤：（1）4‑甲氨基吡啶与柠檬酸混合后，在一定温度下，经脱水缩合得到吡啶修饰的荧光碳点材料；（2）1,6‑二溴己烷与步骤1中制备的荧光碳点反应得到离子液体修饰的功能性荧光碳点材料；（3）1‑溴十二烷与步骤1中制备的荧光碳点反应得到两亲性荧光碳点材料；（4）步骤2，3中所得功能性碳点实现对亚铁离子选择性检测。本发明的有益效果是：制备方法简单，成本低廉，所得功能性荧光碳点材料具有良好的稳定性，对Fe2+检测有良好的选择性和较高的灵敏度。

Description

一种离子液体修饰的荧光碳点的制备和应用
技术领域
本发明属于纳米材料制备和光学传感检测领域，具体为一种离子液体修饰的荧光碳点的制备和应用。
背景技术
近年来，碳量子点(CDs)、石墨烯量子点、多环芳烃等发光材料受到了广泛的关注，且已广泛应用于传感器和生物成像领域。其中，荧光碳点材料不再仅限于由共轭基团或凝聚基团组成的发射源，它表现出特殊的物理化学和光学特性。在CDs的合成中，常用柠檬酸作为碳源，通过聚合或热裂解与胺类低聚物反应，得到目标荧光材料。前期研究表明，选择不同化学结构的胺前驱体，可以获得可调控的光学性能。然而，现有的制备方法和相关应用也存在着一定的缺陷，主要是选择的胺前驱体结构单一和所得荧光材料应用范围有限。
此外，大多数制备的荧光碳点材料对不同pH值溶液敏感，稳定性较差，容易产生荧光猝灭，极大地限制其在某些领域的进一步应用。鉴于此，对现有的合成方法进行改进具有重要的实际价值和研究意义。
本发明的目的是在于提供一种离子液体修饰的荧光碳点的制备方法和应用研究。本发明的技术任务之一：提供一种制备方法简单，成本低廉的合成方法。
本发明的技术任务之二：所得功能性荧光碳点材料应具有良好的稳定性，对Fe2+检测有良好的选择性和较高的灵敏度。
为实现上述目的，本发明采用的技术方案如下：
1. 一种离子液体修饰的荧光碳点的制备，步骤如下：
（1）在耐压试管中依次称取加入2.10-4.20g柠檬酸，3.24-6.48 g 4-甲氨基吡啶和20-40 mL乙醇，在一定温度下搅拌，反应完全后即可获得荧光碳点材料CDs-1；
（2）将步骤1中制备的CDs-1与3.66-7.32 g 1,6-二溴己烷混合，在一定温度下搅拌，减压除去溶剂，20-30 mL正己烷洗涤产物，真空干燥，即可获得离子液体修饰的功能性荧光碳点材料CDs-2；
（3）将步骤1中制备的CDs-1与7.47-1.494 g 1-溴十二烷混合，在一定温度下搅拌，减压除去溶剂，用20-30 mL正己烷洗涤产物，真空干燥，即可获得离子液体修饰的功能性荧光碳点材料CDs-3。
进一步地，步骤（1）中反应温度为155 ℃，磁力搅拌转速为300-500 r/min，反应完全时间为8 h。
进一步地，步骤（2）中反应温度为85 ℃，磁力搅拌转速为300-500 r/min，反应完全时间为24 h。
进一步地，步骤（3）中反应温度为85 ℃，磁力搅拌转速为300-500 r/min，反应完全时间为24 h。
2. 如上1所述的制备方法制备的碳点复合材料CDs-2和CDs-3用于荧光信号检测Fe2+的应用，步骤如下：
（4）分别称取100-200 mg CDs-2和100-200 mg CDs-3溶于50-100 mL去离子水，配制成相应溶液，取1 mL上述溶液对不同浓度的 Fe2+水溶液进行荧光强度检测，记录相应荧光强度的变化。
进一步地，步骤（4）中Fe2+检测所用激发波长为350 nm，波长范围为360-675 nm，Fe2+浓度范围为 0.08-1.5 μM。
本发明的有益效果是：制备方法简单，成本低廉，所得功能性荧光碳点材料具有良好的稳定性，对Fe2+检测有良好的选择性和较高的灵敏度等优势。
具体实施方式
现在结合具体实施例对本发明做进一步说明，以下实施例旨在说明本发明而不是对本发明的进一步限定。
实施例一：一种离子液体修饰的荧光碳点的制备
（1）在耐压试管中依次称取加入2.10柠檬酸，3.24g 4-甲氨基吡啶和20 mL乙醇，升温至155 ℃，300 r/min磁力搅拌，反应8 h后即可获得荧光碳点材料4.88 g CDs-1。
（2）将步骤1中制备的CDs-1与3.66 g 1,6-二溴己烷混合，升温至85 ℃，300 r/min磁力搅拌，反应24 h后，减压除去溶剂，20 mL正己烷洗涤产物，真空干燥，即可获得离子液体修饰的功能性荧光碳点材料CDs-2，产率为82%。
（3）将步骤1中制备的CDs-1与7.47 g 1-溴十二烷混合，升温至85 ℃，300 r/min磁力搅拌，反应24 h后，减压除去溶剂，20 mL正己烷洗涤产物，真空干燥，即可获得离子液体修饰的功能性荧光碳点材料CDs-3，产率为86%。
实施例二：Fe2+检测
分别称取100 mg实施例一中步骤（2）和（3）制备的 CDs-2和CDs-3，溶于溶于50 mL去离子水，配制成相应溶液，取1 mL上述溶液对1 μM Fe2+水溶液进行荧光强度检测，检测过程中所用激发波长为350 nm，检测波长范围为360-675 nm，记录相应荧光强度的变化。实验结果表明，CDs-2作为荧光探针时，Fe2+对其荧光强度影响较小；CDs-3作为荧光探针时，Fe2+对其荧光强度影响较大，发生明显的荧光猝灭现象。通过两者信号差异的比较，可以有效排除其他金属离子的干扰，确定了对Fe2+的专一性检测。同时在0.08-1.5 μM范围内保持良好的线性关系，相关系数在0.994以上，检测限为0.01 μM。

Claims (3)

1.一种离子液体修饰的荧光碳点检测水中亚铁离子的应用，其特征在于包括以下步骤：
（1）在耐压试管中依次称取加入2.10-4.20g柠檬酸，3.24-6.48 g 4-甲氨基吡啶和20-40 mL乙醇，在155 ℃下搅拌，反应8小时后，即可获得荧光碳点CDs-1；
（2）将步骤1中制备的CDs-1与3.66-7.32 g 1,6-二溴己烷混合，在85 ℃下搅拌，反应24小时后，减压除去溶剂，20-30 mL正己烷洗涤产物，真空干燥，即可获得离子液体修饰的功能性荧光碳点CDs-2；
（3）将步骤1中制备的CDs-1与7.47-1.494 g 1-溴十二烷混合，在85 ℃下搅拌，反应24小时后，减压除去溶剂，用20-30 mL正己烷洗涤产物，真空干燥，即可获得离子液体修饰的功能性荧光碳点CDs-3；
（4）分别称取100-200 mg CDs-2和100-200 mg CDs-3溶于50-100 mL去离子水，配制成相应溶液，取1 mL上述溶液对不同浓度 Fe2+水溶液进行荧光强度检测，记录相应荧光强度的变化。
2.根据权利要求1所述的一种离子液体修饰的荧光碳点检测水中亚铁离子的应用，其特征是：所述步骤（4）中亚铁离子水溶液浓度范围为0.08-1.5 μM。
3.根据权利要求1所述的一种离子液体修饰的荧光碳点检测水中亚铁离子的应用，其特征是：所述步骤（4）中亚铁离子检测限为0.01 μM。
CN201910649556.6A 2019-07-18 2019-07-18 一种离子液体修饰的荧光碳点的制备和应用 Active CN110452692B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910649556.6A CN110452692B (zh) 2019-07-18 2019-07-18 一种离子液体修饰的荧光碳点的制备和应用

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910649556.6A CN110452692B (zh) 2019-07-18 2019-07-18 一种离子液体修饰的荧光碳点的制备和应用

Publications (2)

Publication Number Publication Date
CN110452692A CN110452692A (zh) 2019-11-15
CN110452692B true CN110452692B (zh) 2022-06-24

Family

ID=68482880

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910649556.6A Active CN110452692B (zh) 2019-07-18 2019-07-18 一种离子液体修饰的荧光碳点的制备和应用

Country Status (1)

Country Link
CN (1) CN110452692B (zh)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111272717B (zh) * 2020-02-10 2024-02-27 河南师范大学 基于离子液体新型荧光碳点的一步水热合成及其对磺胺噻唑的检测应用

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104327851A (zh) * 2014-09-18 2015-02-04 中国科学院长春光学精密机械与物理研究所 两亲性碳纳米点及其制备方法与应用
CN105176528A (zh) * 2015-08-24 2015-12-23 中物院成都科学技术发展中心 一种氮掺杂碳基量子点的制备方法
CN108384539A (zh) * 2018-02-08 2018-08-10 中国科学院苏州生物医学工程技术研究所 一种绿色荧光碳量子点、制备方法及其应用

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104327851A (zh) * 2014-09-18 2015-02-04 中国科学院长春光学精密机械与物理研究所 两亲性碳纳米点及其制备方法与应用
CN105176528A (zh) * 2015-08-24 2015-12-23 中物院成都科学技术发展中心 一种氮掺杂碳基量子点的制备方法
CN108384539A (zh) * 2018-02-08 2018-08-10 中国科学院苏州生物医学工程技术研究所 一种绿色荧光碳量子点、制备方法及其应用

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"One-step sonochemical synthesis of versatile nitrogen-doped carbon quantum dots for sensitive detection of Fe2+ ions and temperature in vitro";Meice Lu et al.,;《Materials Science & Engineering C》;20190329;第101卷;第325-359页 *

Also Published As

Publication number Publication date
CN110452692A (zh) 2019-11-15

Similar Documents

Publication Publication Date Title
Liu et al. Recent advances in sensors for tetracycline antibiotics and their applications
Zhou et al. A sensing approach for dopamine determination by boronic acid-functionalized molecularly imprinted graphene quantum dots composite
Chen et al. Covalent organic frameworks as a sensing platform for water in organic solvent over a broad concentration range
Ye et al. Constructing a fluorescent probe for specific detection of catechol based on 4-carboxyphenylboronic acid-functionalized carbon dots
Liu et al. Turn-on fluorescence sensor for the detection of heparin based on rhodamine B-modified polyethyleneimine–graphene oxide complex
Liu et al. Electrochemiluminescence sensing platform for ultrasensitive DNA analysis based on resonance energy transfer between graphitic carbon nitride quantum dots and gold nanoparticles
Shi et al. An off-on fluorescent probe based on graphene quantum dots intercalated hydrotalcite for determination of ascorbic acid and phytase
WO2020228640A1 (zh) 一种锌离子荧光探针化合物及其制备方法与应用
Lei et al. A turn-on fluorescent sensor for the detection of melamine based on the anti-quenching ability of Hg 2+ to carbon nanodots
CN109762558A (zh) 一种用于定量检测尿液中PPi含量的比率型荧光探针的制备方法
Song et al. “On-off-on” fluorescent system for detection of Zn2+ in biological samples using quantum dots-carbon dots ratiometric nanosensor
Wang et al. A highly sensitive and selective turn-on fluorescent sensor for dihydrogen phosphate in living cells
Li et al. Discrimination and detection of benzaldehyde derivatives using sensor array based on fluorescent carbon nanodots
CN109705111B (zh) 一种汞离子检测探针及其制备方法和应用
Jiang et al. Dimethoxy triarylamine-derived terpyridine–zinc complex: A fluorescence light-up sensor for citrate detection based on aggregation-induced emission
CN107245334A (zh) 一种检测汞离子的水溶性高分子荧光素类荧光探针及其制备方法
CN110618178B (zh) 一种用于检测细菌的电化学阻抗电极的制备方法
CN108469428A (zh) 基于氮掺杂石墨烯量子点荧光淬灭机制检测多巴胺的方法
Miao et al. Self-assembly of phosphorescent quantum dots/boronic-acid-substituted viologen nanohybrids based on photoinduced electron transfer for glucose detection in aqueous solution
Yin et al. Sensing of perfluorinated compounds using a functionalized tricolor upconversion nanoparticle based fluorescence sensor array
CN110452692B (zh) 一种离子液体修饰的荧光碳点的制备和应用
Tang et al. Luminescent lanthanide coordination polymer as a platform for DNA colorimetric detection
CN112251216A (zh) 一种基于磁性共价有机框架的双酚a碳点分子印迹荧光复合探针的制备方法及应用
Song et al. Natural deep eutectic solvent-assisted preparation of nitrogen-doped carbon dots for ratiometric determination of pirimicarb and pH
Eftekhari-Sis et al. Graphene oxide-terpyridine conjugate: a highly selective colorimetric and sensitive fluorescence Nano-chemosensor for Fe2+ in aqueous media

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant