CN106757138A - The electrochemical preparation method of nitrogenous carbon quantum dot - Google Patents
The electrochemical preparation method of nitrogenous carbon quantum dot Download PDFInfo
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- CN106757138A CN106757138A CN201611053884.2A CN201611053884A CN106757138A CN 106757138 A CN106757138 A CN 106757138A CN 201611053884 A CN201611053884 A CN 201611053884A CN 106757138 A CN106757138 A CN 106757138A
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- quantum dot
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- nitrogenous carbon
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/20—Processes
- C25B3/23—Oxidation
Abstract
The present invention relates to chemical sensor field, and in particular to a kind of electrochemical preparation method of nitrogenous carbon quantum dot.The electrochemical preparation method of nitrogenous carbon quantum dot, the mL of anhydrous ethylenediamine 100 is measured with graduated cylinder, and the g of lithium perchlorate 1.6 is added in beaker, stirring and dissolving, then lead to nitrogen 30 min, then make of the graphite rod of a diameter of 0.5cm the anode and cathode reacted respectively, be passed through dc source；Seeing during reaction around negative electrode has bubble to produce, and with the carrying out of reaction, the color of solution is gradually changed, and by colourless to light yellow, finally to celadon, reaction continues 4 hours；After reaction terminates, sand core funnel suction filtration is used, the solution colour obtained after suction filtration is glassy yellow, is spin-dried for, then with water dissolves, extracted with dichloromethane, obtain the homogeneous nitrogenous carbon quantum dot of particle size.The nitrogenous carbon quantum dot of the present invention has the fluorescence response of stabilization in the solution of pH=3 ~ 9, its interference very little, thus can be used for the quantitative fluorescence analysis of micro copper ion concentration in solution.
Description
Technical field
The present invention relates to chemical sensor field, and in particular to a kind of electrochemistry preparation side of nitrogenous carbon quantum dot
Method.
Background technology
Carbon quantum dot is size less than the scattered spherical fluorescence carbon nano-particles of 10 nm, in being fluorescence carbon nanomaterial
Topmost one kind.Compared with traditional dye molecule and semiconductor-quantum-point, it not only fluorescence it is strong and stablize, resistance to photobleaching,
Unglazed scintillation, and exciting light spectrum width and it is continuous, achievable unitary excites polynary transmitting.Its low toxicity characteristic, good life
Thing compatibility and environmental safety and water solubility ensure that carbon quantum dot can relievedly be applied to the detection of active somatic cell, no
Cause mistaken diagnosis to the influence of active somatic cell with worry fluorescent material, it is also possible to for a long time in research cell between biomolecule
Interact.Similar to inorganic-quantum-dot, the emission spectrum span of carbon quantum dot is very big, is extended to closely from visible range
Infrared spectral region, this advantage compensate for deficiency of the common fluorescent reagent near infrared spectrum less varieties.Additionally, carbon quantum dot
Can be not only used for single photon image, two photon imaging can be used for again, be expected to substitute inorganic-quantum-dot turn into biomedical sector in most
Has the environmentally friendly fluorescent nano material of application prospect.At present, existing many document report carbon quantum dots are used as fluorescence spy
Pin is applied to the fluorescence observation of cell and live body.
The carbon quantum dot synthetic method reported has a lot, electrochemical method synthesize carbon quantum dot due to it is simple to operate, set
It is standby to require low, repeatable strong, product stabilization, it is not necessary to carry out further moditied processing, it is only necessary to which centrifugation can just be obtained
To luminous carbon nano-particle, and used by many researchers.During electrochemical process prepares carbon nano-particle, working electrode
Generally conductive carbon materials, under certain electric current or potential, by electrolyte anodic oxidation, shells from working electrode
The tiny carbon nano-particle under.Common carbon quantum dot is generally using oxygenatedchemicals such as ethanol, glucose as carbon source.
Technical program of the present invention lies in：
The electrochemical preparation method of nitrogenous carbon quantum dot, comprises the following steps：
The mL of anhydrous ethylenediamine 100 is measured with graduated cylinder first, the g of lithium perchlorate 1.6, stirring and dissolving, Ran Houtong are added in beaker
The min of nitrogen 30, then the anode and cathode reacted is made of graphite rod, it is passed through dc source；See during reaction has around negative electrode
Bubble is produced, and with the carrying out of reaction, the color of solution gradually changes, and by colourless to light yellow, finally to celadon, reaction is held
Continue 4 hours；After reaction terminates, suction filtration, the solution colour obtained after suction filtration is glassy yellow, is spin-dried for, and then with water dissolves, is used
Dichloromethane is extracted, and obtains the homogeneous nitrogenous carbon quantum dot of particle size.
The control range of described dc source current density is in 20 ~ 100 mA/cm2Between.
The whole experimental procedure of electrochemical preparation method of described nitrogenous carbon quantum dot is carried out under nitrogen protection.
Described to be spin-dried for using Rotary Evaporators, temperature is 65 DEG C.
A diameter of 0.5cm of described graphite rod.
Described suction filtration is realized by sand core funnel.
The technical effects of the invention are that：
With ethylenediamine as raw material, Applied Electrochemistry method successfully synthesizes nitrogenous carbon quantum dot to the present invention.The nitrogenous carbon quantum dot
There is the fluorescence response of stabilization in the solution of pH=3 ~ 9, other metal ions disturb it very little, thus can be used in solution
The quantitative fluorescence analysis of micro copper ion concentration.
Specific embodiment
The electrochemical preparation method of nitrogenous carbon quantum dot, comprises the following steps：
Embodiment 1
The mL of anhydrous ethylenediamine 100 is measured with graduated cylinder first, the g of lithium perchlorate 1.6, stirring and dissolving, Ran Houtong are added in beaker
The min of nitrogen 30, then the anode and cathode reacted is made of graphite rod, it is passed through dc source；See during reaction has around negative electrode
Bubble is produced, and with the carrying out of reaction, the color of solution gradually changes, and by colourless to light yellow, finally to celadon, reaction is held
Continue 4 hours；After reaction terminates, suction filtration, the solution colour obtained after suction filtration is glassy yellow, is spin-dried for, and then with water dissolves, is used
Dichloromethane is extracted, and obtains the homogeneous nitrogenous carbon quantum dot of particle size.
Wherein, the control range of described dc source current density is in 20 mA/cm2Between.Described nitrogenous carbon quantum
The whole experimental procedure of electrochemical preparation method of point is carried out under nitrogen protection.It is described to be spin-dried for using Rotary Evaporators, temperature
It is 65 DEG C.
Embodiment 2
The mL of anhydrous ethylenediamine 100 is measured with graduated cylinder first, the g of lithium perchlorate 1.6, stirring and dissolving, Ran Houtong are added in beaker
The min of nitrogen 30, then the anode and cathode reacted is made of graphite rod, it is passed through dc source；See during reaction has around negative electrode
Bubble is produced, and with the carrying out of reaction, the color of solution gradually changes, and by colourless to light yellow, finally to celadon, reaction is held
Continue 4 hours；After reaction terminates, suction filtration, the solution colour obtained after suction filtration is glassy yellow, is spin-dried for, and then with water dissolves, is used
Dichloromethane is extracted, and obtains the homogeneous nitrogenous carbon quantum dot of particle size.
Wherein, the control range of described dc source current density is in 80 mA/cm2Between.Described nitrogenous carbon quantum
The whole experimental procedure of electrochemical preparation method of point is carried out under nitrogen protection.It is described to be spin-dried for using Rotary Evaporators, temperature
It is 65 DEG C.
Embodiment 3
Anhydrous ethylenediamine 90mL is measured with graduated cylinder first, the g of lithium perchlorate 1.5 is added in beaker, then stirring and dissolving leads to nitrogen
Gas 45min, then the anode and cathode reacted is made of graphite rod, it is passed through dc source；See there is gas around negative electrode during reaction
Bubble is produced, and with the carrying out of reaction, the color of solution is gradually changed, and by colourless to light yellow, finally to celadon, reaction continues
4 hours；After reaction terminates, suction filtration, the solution colour obtained after suction filtration is glassy yellow, is spin-dried for, then with water dissolves, with two
Chloromethanes is extracted, and obtains the homogeneous nitrogenous carbon quantum dot of particle size.
Wherein, the control range of described dc source current density is in 100 mA/cm2Between.Described nitrogenous carbon amounts
The whole experimental procedure of electrochemical preparation method of son point is carried out under nitrogen protection.It is described to be spin-dried for using Rotary Evaporators, temperature
Spend is 70 DEG C.
Claims (6)
1. the electrochemical preparation method of nitrogenous carbon quantum dot, it is characterised in that：Comprise the following steps：
The mL of anhydrous ethylenediamine 100 is measured with graduated cylinder first, the g of lithium perchlorate 1.6, stirring and dissolving, Ran Houtong are added in beaker
The min of nitrogen 30, then the anode and cathode reacted is made of graphite rod, it is passed through dc source；See during reaction has around negative electrode
Bubble is produced, and with the carrying out of reaction, the color of solution gradually changes, and by colourless to light yellow, finally to celadon, reaction is held
Continue 4 hours；After reaction terminates, suction filtration, the solution colour obtained after suction filtration is glassy yellow, is spin-dried for, and then with water dissolves, is used
Dichloromethane is extracted, and obtains the homogeneous nitrogenous carbon quantum dot of particle size.
2. the electrochemical preparation method of nitrogenous carbon quantum dot according to claim 1, it is characterised in that：Described direct current
The control range of ource electric current density is in 20 ~ 100 mA/cm2Between.
3. the electrochemical preparation method of nitrogenous carbon quantum dot according to claim 1, it is characterised in that：Described nitrogenous carbon
The whole experimental procedure of electrochemical preparation method of quantum dot is carried out under nitrogen protection.
4. the electrochemical preparation method of nitrogenous carbon quantum dot according to claim 1, it is characterised in that：It is described to be spin-dried for making
With Rotary Evaporators, temperature is 65 DEG C.
5. the electrochemical preparation method of nitrogenous carbon quantum dot according to claim 1, it is characterised in that：Described graphite rod
A diameter of 0.5cm.
6. the electrochemical preparation method of nitrogenous carbon quantum dot according to claim 1, it is characterised in that：Described suction filtration leads to
Cross sand core funnel realization.
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| CN201611053884.2A CN106757138A (en) | 2016-11-25 | 2016-11-25 | The electrochemical preparation method of nitrogenous carbon quantum dot |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108468071A (en) * | 2017-02-23 | 2018-08-31 | 中国科学院苏州纳米技术与纳米仿生研究所 | Electrochemical ion impact prepares the method and its application of inorganic non-metallic material quantum dot |
| CN112095113A (en) * | 2020-09-07 | 2020-12-18 | 太原理工大学 | Method for preparing carbon quantum dots by taking coal as raw material |
-
2016
- 2016-11-25 CN CN201611053884.2A patent/CN106757138A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108468071A (en) * | 2017-02-23 | 2018-08-31 | 中国科学院苏州纳米技术与纳米仿生研究所 | Electrochemical ion impact prepares the method and its application of inorganic non-metallic material quantum dot |
| CN112095113A (en) * | 2020-09-07 | 2020-12-18 | 太原理工大学 | Method for preparing carbon quantum dots by taking coal as raw material |
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Application publication date: 20170531 |