CN106629657A - Fluorescent carbon dots and preparation method and application thereof - Google Patents
Fluorescent carbon dots and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to fluorescent carbon dots and a preparation method and application thereof. The invention adopts the technical scheme as follows: the fluorescent carbon dots are prepared by putting malic acid and a passivator into a reaction kettle lined by polytetrafluoroethylene at room temperature, heating for 2-6 hours at 170-220 DEG C, naturally cooling to room temperature, adding ultrapure water, centrifuging, and dialyzing a supernatant. According to the invention, by a high-temperature solid phase reaction method, the fluorescent carbon dots are prepared by taking the DL-malic acid as a carbon source and an amino acid as the passivator through one-step synthesis. When the preparation method is used for preparing the carbon dots, raw materials are easy to obtain, the preparation method is simple, the yield is high, the synthesis conditions are mild and controllable, and the prepared carbon dots are good in water solubility, good in stability and high in fluorescence quantum yield.
Description
Technical field
The present invention relates to carbon nanomaterial technical field, and in particular to a kind of fluorescent carbon with compared with high-fluorescence quantum yield
Point.
Background technology
Carbon point (carbon dots, CDs) is a kind of New Type of Carbon nanoparticle of the diameter for occurring in recent years less than 10nm
Son.Fluorescence property is carbon point performance the most prominent.Carbon point has excitation wavelength tunable with launch wavelength, and fluorescence property is steady
It is fixed, the excellent fluorescence property such as resistance to photobleaching and unglazed scintillation.Additionally, fluorescent carbon point has good biocompatibility, toxicity
Low, excitation spectrum is wider and continuous, is a kind of extraordinary fluorescent labeling and image forming material, and successfully applied cell with
In living imaging.Although about the existing many document reports of preparation method and application research of fluorescent carbon point, existing preparation
It is complicated also to there is preparation process in method, the low problem of quantum yield, therefore, find simple, it is convenient, quickly prepare luminescent properties
The method of excellent carbon point is very important.
The content of the invention
It is an object of the invention to provide a kind of preparation method is simple, the high fluorescent carbon point of quantum yield.
The present invention seeks to be achieved through the following technical solutions：A kind of fluorescent carbon point, comprises the steps：Under room temperature,
Malic acid and passivator are put in the reactor of inner liner polytetrafluoroethylene, at 170-220 DEG C, 2-6 hours is heated, it is naturally cold
But to room temperature, add ultra-pure water, centrifugation to dialyse supernatant, obtain fluorescent carbon point.
Preferably, above-mentioned fluorescent carbon point, described passivator is aminoacid.It is furthermore preferred that described aminoacid is color
Propylhomoserin, glutamic acid or glycine.
Preferably, above-mentioned fluorescent carbon point, by weight, malic acid:Passivator=1:0.1-1.
Application of the above-mentioned fluorescent carbon point in photocatalysis degradation organic contaminant and bio-imaging.
Application of the above-mentioned fluorescent carbon point in photocatalysis degradation organic contaminant, method is as follows：In containing organic contamination
In the solution of thing, above-mentioned fluorescent carbon point, the stirring and adsorbing under dark surrounds are added so as to reach adsorption and desorption balance, subsequently
Add H2O2, irradiate under the high mercury lamps of 250W.
Application of the above-mentioned fluorescent carbon point in bio-imaging, method is as follows：Above-mentioned fluorescent carbon point and cell are trained altogether
Support, with fluorescence microscope cell imaging effect.
The invention has the beneficial effects as follows：The present invention, using a step high-temperature solid phase reaction method carbon dots solution is obtained,
Under 365nm ultraviolet lights, synthesized carbon point presents excellent fluorescence property.The carbon dots solution of preparation is ultraviolet in 365nm
Bright blue-fluorescence is sent under light irradiation.Synthetic method of the present invention is simply effective, and raw material is easy to get, and reaction condition is gently controllable,
Can complete in general laboratory.Using the carbon point fluorescence quantum yield of the inventive method preparation up to more than 15%.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of fluorescent carbon point prepared by embodiment 1.
Fig. 2 is the X-ray diffractogram of fluorescent carbon point prepared by embodiment 1.
Fig. 3 is the infrared spectrum of fluorescent carbon point prepared by embodiment 1.
Fig. 4 is the uv-visible absorption spectra of fluorescent carbon point solution prepared by embodiment 1.
Fig. 5 is the fluorescence excitation and emission spectrum of fluorescent carbon point solution prepared by embodiment 1.
Fig. 6 is fluorescent carbon point solution fluorescence emission spectrum (excitation wavelength prepared by the embodiment 1 under different wavelengths of light is excited
By 348nm to 418nm, step-length is 10nm).
Fig. 7 is the photocatalytic degradation figure of fluorescent carbon point solution prepared by embodiment 1.
Fig. 8 is intake situation of the fluorescence microscope cell to carbon point.
Specific implementation method
With reference to specific embodiment, the invention will be further described.
Embodiment 1
(1) preparation method
Under room temperature, 0.50 gram of DL-malic acid and 0.50 gram of glycine are placed on into the reactor of inner liner polytetrafluoroethylene
In, 180 DEG C of heated at constant temperature naturally cool to room temperature after 6 hours, are subsequently adding 10ml ultra-pure waters, are centrifuged under 10000rmp
After 10min, supernatant is dialysed, that is, obtain dark-brown carbon dots solution, be designated as fluorescent carbon point -1.In 365nm uviol lamps
Under irradiation, the blue-fluorescence of the carbon dots solution emitting bright.
Fluorescent carbon point solution quinine sulfate manufactured in the present embodiment is cooked reference material, is measured fluorescence quantum yield and is
20.5%.
(2) result
1. Fig. 1 is the transmission electron microscope photo of carbon point manufactured in the present embodiment.By photo it is found that the shape of the carbon point for preparing
Looks are homogeneous, and particle diameter is about 5nm, and favorable dispersibility has a good application prospect in bioanalysiss, catalytic field.
2. Fig. 2 is the X-ray diffractogram of carbon point manufactured in the present embodiment.It is observed that in 2 θ=27 ° or so in figure
There is a typical wide spike, this is relevant with the structure of graphite, further demonstrate that their crystallographic properties.
3. Fig. 3 is the infrared spectrogram of carbon point manufactured in the present embodiment.As seen from the figure ,～3366cm-1Flexible for-OH shakes
It is dynamic to absorb ,～1659cm-1For the characteristic absorption peak of C=O ,～1400cm-1It is the bending vibration of C-H.
4. Fig. 4 is the uv-visible absorption spectra after carbon dots solution ultra-pure water dilution manufactured in the present embodiment.The figure shows
Show, carbon dots solution has an obvious characteristic absorption peak at 368nm or so places.
5. Fig. 5 is the fluorescence excitation and launching light spectrogram of carbon dots solution manufactured in the present embodiment.As seen from the figure, carbon dots solution
The a length of 368nm of optimum excitation wave, optimal launch wavelength is 452nm.In this embodiment, when carrying out spectrofluorimetry,
Excitation wavelength adopts 368nm.It is 84nm by the Stokes shift that prepared carbon point is can be found that in Fig. 5, it is larger
Stokes shift are more beneficial for being analyzed and detection using its fluorescence property.
6. Fig. 6 is glimmering under being excited with different wavelengths of light again after the carbon dots solution ultra-pure water dilution of the preparation of the present embodiment
Optical emission spectroscopy.As seen from the figure, carbon dots solution has fluorescence exciting wavelength dependency.With the increase of excitation wavelength, carbon point
Fluorescent emission peak intensity first increases and declines afterwards, and red shift occurs in peak position.
(3) contrast test
Under room temperature, 0.50 gram of DL-malic acid is placed in the reactor of inner liner polytetrafluoroethylene, 180 DEG C of heated at constant temperature 6
After hour, room temperature is naturally cooled to, be subsequently adding 10ml ultra-pure waters, be centrifuged after 10min under 10000rmp, supernatant is carried out
Dialysis, obtains fluorescent carbon point, is designated as fluorescent carbon point -2.
Prepared fluorescent carbon point solution quinine sulfate is cooked into reference material, its fluorescence quantum yield is measured and is shown in Table 1.
Table 1
| Fluorescent carbon point -1 | Fluorescent carbon point -2 | |
| Quantum yield | 20.5% | <2.3% |
From table 1, add glycine to cause the surface texture of carbon point and functional group to there occurs change, make the photic of carbon point
Luminescent properties are significantly increased.So adding glycine in this experiment as passivator.
Embodiment 2
Under room temperature, 0.50 gram of DL-malic acid and 0.1 gram of L-Tryptophan are put into into the reactor of inner liner polytetrafluoroethylene
In, after 170 DEG C of constant temperature are processed 2 hours, room temperature is naturally cooled to, 10ml ultra-pure waters are subsequently adding, it is centrifuged under 10000rmp
After 10min, supernatant is dialysed, that is, obtain the carbon dots solution of purification.
Fluorescent carbon point solution quinine sulfate manufactured in the present embodiment is cooked reference material, is measured fluorescence quantum yield and is
17.4%.
Embodiment 3
Under room temperature, 0.5 gram of DL-malic acid and 0.20 gram of L-Glutamic Acid are put into into the reactor of inner liner polytetrafluoroethylene
In, 210 DEG C of heated at constant temperature naturally cool to room temperature after 5 hours, are subsequently adding 10ml ultra-pure waters, are centrifuged under 10000rmp
After 10min, supernatant is dialysed, that is, obtain the carbon dots solution of purification.
Fluorescent carbon point solution quinine sulfate manufactured in the present embodiment is cooked reference material, is measured fluorescence quantum yield and is
15.2%.
Application of the fluorescent carbon point of embodiment 4 in photocatalysis degradation organic contaminant
Method：50ml methylene blue solutions (concentration is 10mg/L) are measured in beaker, the fluorescence of the preparation of embodiment 1 is added
The solution 2ml of carbon point -1, stirring and adsorbing 1h under dark surrounds so as to reach adsorption and desorption balance, be subsequently added 0.1ml H2O2
(30%), then sampled every 20 minutes with the high Hg lamp irradiations of 250W, Asia is determined at wavelength 664nm by spectrophotometer
The absorbance of methyl blue solution, by below equation the percent of decolourization of methylene blue is calculated, as a result such as Fig. 1.
Wherein, A0:Methylene blue solution initial absorbance
A:Methylene blue solution absorbance after reaction
As seen from Figure 7, carbon point has certain photocatalysis performance, can be used for dyestuff etc. in photocatalytic degradation sewage organic
Thing.
Application of the fluorescent carbon point of embodiment 5 in bio-imaging
Method：The solution of fluorescent carbon point -1 prepared by the embodiment 1 that concentration is 200 μ g/L exists with stomach cancer cell BGC-823
Co-culture at 37 DEG C, respectively in 6h and 24h, with intake situation of the fluorescence microscope cell to carbon point, as a result such as Fig. 8 institutes
Show.As seen from Figure 8, increase over time, cell is better to CDs intakes effect, shows good cell imaging effect.
Claims (7)
1. a kind of fluorescent carbon point, it is characterised in that comprise the steps：Under room temperature, malic acid and passivator are put into into liner and are gathered
In the reactor of tetrafluoroethene, at 170-220 DEG C, 2-6 hours are heated, naturally cool to room temperature, add ultra-pure water, be centrifuged,
Supernatant is dialysed, fluorescent carbon point is obtained.
2. fluorescent carbon point according to claim 1, it is characterised in that described passivator is aminoacid.
3. fluorescent carbon point according to claim 2, it is characterised in that described aminoacid is tryptophan, glutamic acid or sweet
Propylhomoserin.
4. fluorescent carbon point according to claim 1, it is characterised in that by weight, malic acid:Passivator=1:0.1-1.
5. application of the fluorescent carbon point described in claim 1 in photocatalysis degradation organic contaminant and bio-imaging.
6. application of the fluorescent carbon point according to claim 5 in photocatalysis degradation organic contaminant, it is characterised in that side
Method is as follows：In the solution containing organic pollution, the fluorescent carbon point described in claim 1 is added, stirred under dark surrounds
Absorption so as to reach adsorption and desorption balance, be subsequently added H2O2, irradiate under the high mercury lamps of 250W.
7. application of the fluorescent carbon point according to claim 5 in bio-imaging, it is characterised in that method is as follows：Will power
Profit requires the fluorescent carbon point and co-culture of cells described in 1, with the imaging effect of fluorescence microscope cell.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325815A (en) * | 2017-07-20 | 2017-11-07 | 辽宁大学 | High quantum production rate fluorescent carbon point of N doping and its preparation method and application |
| CN107555416A (en) * | 2017-08-07 | 2018-01-09 | 河南师范大学 | The method of hydro-thermal method synthetic nitrogen doping fluorescent carbon point |
| CN108483423A (en) * | 2018-04-08 | 2018-09-04 | 太原理工大学 | A kind of fast preparation method of right-handed chirality carbon dots |
| CN108659836A (en) * | 2018-07-23 | 2018-10-16 | 辽宁大学 | A kind of high quantum production rate nitrogen sulphur codope fluorescent carbon point and its preparation method and application |
| CN110044861A (en) * | 2019-05-09 | 2019-07-23 | 南宁师范大学 | The detection method of concentration of hydrogen peroxide |
| CN110187124A (en) * | 2019-05-20 | 2019-08-30 | 上海凯创生物技术有限公司 | A kind of preparation method and its usage of carbon quantum dot |
| CN111088043A (en) * | 2019-12-18 | 2020-05-01 | 辽宁大学 | Visible light excited and long-wavelength emitted fluorescent carbon dot and preparation method and application thereof |
| CN111573653A (en) * | 2020-05-19 | 2020-08-25 | 山西大学 | Nitrogen-sulfur self-doped fluorescent carbon quantum dot and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104927849A (en) * | 2015-07-08 | 2015-09-23 | 安徽工业大学 | Green synthetic method for blue fluorescence carbon quantum dots with high fluorescence quantum yield |
| CN105647529A (en) * | 2016-03-09 | 2016-06-08 | 沈阳大学 | Method for preparing carbon-dot solid-state fluorescent powder |
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2016
- 2016-11-21 CN CN201611025684.6A patent/CN106629657A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104927849A (en) * | 2015-07-08 | 2015-09-23 | 安徽工业大学 | Green synthetic method for blue fluorescence carbon quantum dots with high fluorescence quantum yield |
| CN105647529A (en) * | 2016-03-09 | 2016-06-08 | 沈阳大学 | Method for preparing carbon-dot solid-state fluorescent powder |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325815A (en) * | 2017-07-20 | 2017-11-07 | 辽宁大学 | High quantum production rate fluorescent carbon point of N doping and its preparation method and application |
| CN107555416A (en) * | 2017-08-07 | 2018-01-09 | 河南师范大学 | The method of hydro-thermal method synthetic nitrogen doping fluorescent carbon point |
| CN108483423A (en) * | 2018-04-08 | 2018-09-04 | 太原理工大学 | A kind of fast preparation method of right-handed chirality carbon dots |
| CN108659836A (en) * | 2018-07-23 | 2018-10-16 | 辽宁大学 | A kind of high quantum production rate nitrogen sulphur codope fluorescent carbon point and its preparation method and application |
| CN108659836B (en) * | 2018-07-23 | 2021-06-01 | 辽宁大学 | High-quantum-yield nitrogen-sulfur co-doped fluorescent carbon dot and preparation method and application thereof |
| CN110044861A (en) * | 2019-05-09 | 2019-07-23 | 南宁师范大学 | The detection method of concentration of hydrogen peroxide |
| CN110187124A (en) * | 2019-05-20 | 2019-08-30 | 上海凯创生物技术有限公司 | A kind of preparation method and its usage of carbon quantum dot |
| CN110187124B (en) * | 2019-05-20 | 2022-10-04 | 上海凯创生物技术有限公司 | Preparation method and application of carbon quantum dots |
| CN111088043A (en) * | 2019-12-18 | 2020-05-01 | 辽宁大学 | Visible light excited and long-wavelength emitted fluorescent carbon dot and preparation method and application thereof |
| CN111573653A (en) * | 2020-05-19 | 2020-08-25 | 山西大学 | Nitrogen-sulfur self-doped fluorescent carbon quantum dot and preparation method and application thereof |
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Application publication date: 20170510 |