CN104388083B - A kind of method synthesizing glassy yellow fluorescent carbon point - Google Patents
A kind of method synthesizing glassy yellow fluorescent carbon point Download PDFInfo
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- CN104388083B CN104388083B CN201410656110.3A CN201410656110A CN104388083B CN 104388083 B CN104388083 B CN 104388083B CN 201410656110 A CN201410656110 A CN 201410656110A CN 104388083 B CN104388083 B CN 104388083B
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Abstract
The invention belongs to the preparation field of carbon nanomaterial, it is intended to provide a kind of method synthesizing glassy yellow fluorescent carbon point. The method is that carbon source and passivator and phosphoric acid are put into solvent in the lump, reacts 1 ~ 5 hour to synthesize glassy yellow fluorescent carbon point at 80 ~ 110 DEG C; The mass ratio of described passivator and carbon source is 0.1 ~ 0.7, and the mass ratio of phosphoric acid and carbon source is 5 ~ 30, and the mass ratio of solvent and carbon source is 20 ~ 100. The present invention is simply efficient, adopts solvent-thermal method to take xitix as carbon source, and amino acid is passivator, and phosphoric acid is that reaction medium one-step synthesis goes out the carbon point presenting glassy yellow fluorescence under 365 nano-ultraviolet lights irradiate. The method prepares carbon point cheaper starting materials, and step is simple, and mild condition is controlled, prepares the carbon point luminous intensity height, good stability.
Description
Technical field
The present invention relates to the preparation method of carbon nanomaterial, be specifically related to a kind of method synthesizing glassy yellow fluorescent carbon point, the method is the method that xitix and amino acid prepare glassy yellow fluorescent carbon point.
Background technology
Carbon point (CarbonDots, CDs) is the novel carbon nano-particles that a kind of diameter occurred in recent years is less than 10 nanometers. Fluorescence property is the most outstanding performance of carbon point. The fluorescence property that carbon point has excitation wavelength and emission wavelength is tunable, the resistance to photobleaching of fluorescent stabilization and unglazed scintillation etc. are excellent. Meanwhile, particle diameter and the molecular weight of carbon point are all very little, good biocompatibility. Carbon point can enter cell interior by cell endocytic and not affect nucleus, it is also possible to DNA interaction of biomacromolecules, thus carries out identification and the detection of DNA. Therefore, carbon point can be applied to the field such as biomarker and bio-imaging as the surrogate of semiconductor-quantum-point (such as CdS, CdSe, CdTe etc.) and organic dye. At present, the carbon point of synthesis is the photoluminescence property with blue light mostly, and there is stronger autologous blue-fluorescence due to the cell or tissue of organism, and it being unfavorable for the differentiation of target signal and background signal when these carbon points are used for cell imaging, background interference is bigger. Therefore, it is necessary very much that searching is a kind of simply, by carbon source of the raw material of cheapness to synthesize the method for the carbon point of other glow colors, can reduce background interference like this when biomarker and imaging.
Summary of the invention
It is an object of the invention to provide a kind of method synthesizing glassy yellow fluorescent carbon point, the method one step solvent-thermal method obtains carbon point solution, under portable 365 nanometers of ultra violet lamps, the carbon point solution synthesized presents bright yellow fluorescence, synthetic method of the present invention is simply effective, and cheaper starting materials is easy to get, reaction conditions gentleness and environmental friendliness, all can complete in common laboratory, be easy to promote.
It is an object of the invention to be achieved through the following technical solutions:
Synthesizing a method for glassy yellow fluorescent carbon point, described method comprises the following steps:
Carbon source and passivator and phosphoric acid are put into solvent in the lump, 1 ~ 5 hour is reacted to synthesize glassy yellow fluorescent carbon point at 80 ~ 110 DEG C, under room temperature, by the glycine of the xitix of 0.50 gram and 0.10 gram, the phosphoric acid of 8.5 grams is dissolved in 30 grams of ethylene glycol, is transferred in hydrothermal reaction kettle by solution, and 90 DEG C process 3 hours, naturally cool to room temperature, obtain the carbon point solution of yellow; Or under room temperature, by the tyrosine of the xitix of 0.50 gram and 0.20 gram, the phosphoric acid of 2.5 grams is dissolved in 10 grams of ethylene glycol, is transferred in hydrothermal reaction kettle by solution, 110 DEG C process 1 hour, naturally cool to room temperature, obtain the carbon point solution of yellow; Or under room temperature, by the phenylalanine of the xitix of 0.50 gram and 0.05 gram, the phosphoric acid of 15 grams is dissolved in 50 grams of ethylene glycol, is transferred in hydrothermal reaction kettle by solution, 90 DEG C process 4 hours, naturally cool to room temperature, obtain the carbon point solution of yellow; Or under room temperature, by the L-glutamic acid of the xitix of 0.50 gram and 0.35 gram, the phosphoric acid of 10 grams is dissolved in 30 grams of ethylene glycol, is transferred in hydrothermal reaction kettle by solution, 80 DEG C process 5 hours, naturally cool to room temperature, obtain the carbon point solution of yellow; Obtained carbon point, sends bright yellow fluorescence under 365nm ultra violet lamp.
A kind of described method synthesizing glassy yellow fluorescent carbon point, the mass ratio of described passivator and carbon source is 0.1 ~ 0.7.
A kind of described method synthesizing glassy yellow fluorescent carbon point, the mass ratio of described phosphoric acid and carbon source is 5 ~ 30, and the mass ratio of solvent and carbon source is 20 ~ 100.
A kind of described method synthesizing glassy yellow fluorescent carbon point, described carbon source is xitix; Passivator is any one in glycine, tyrosine, phenylalanine, L-glutamic acid.
A kind of described method synthesizing glassy yellow fluorescent carbon point, described solvent is any one in ethylene glycol, glycol ether, ethanol.
Advantage and the effect of the present invention be:
The present invention can obtain carbon point solution by a step solvent-thermal method, and under portable 365 nanometers of ultra violet lamps, the carbon point solution synthesized presents bright yellow fluorescence. The method of synthesis glassy yellow fluorescent carbon point of the present invention is simply effective, and cheaper starting materials is easy to get, and reaction conditions gentleness and environmental friendliness, all can complete in common laboratory, is easy to promote.
Accompanying drawing explanation
Fig. 1: X-ray diffraction (XRD) figure (corresponding embodiment 1 product) of carbon point;
Fig. 2: the photo (corresponding embodiment 1 product) of carbon point under transmission electron microscope (TEM);
Fig. 3: the infrared spectrogram (corresponding embodiment 1 product) of carbon point;
Fig. 4: the fluorescence spectrum figure (excitation wavelength by 320nm to 540nm, step-length be 20nm) of the carbon point aqueous solution under different wave length optical excitation.
Embodiment
Below in conjunction with accompanying drawing illustrated embodiment, the invention will be further described.
First the method utilizes xitix and glycine to be initial reactant, in phosphoric acid medium, take ethylene glycol as solvent, prepares carbon point solution by solvent thermal reaction.In addition have also been attempted other amino acid except glycine (such as tyrosine, phenylalanine, L-glutamic acid etc.), they and ascorbic acid solution heat altogether, all can obtain glassy yellow fluorescent carbon point.
Concrete steps are: carbon source and passivator and phosphoric acid are put into solvent in the lump, react 1 ~ 5 hour to synthesize glassy yellow fluorescent carbon point at 80 ~ 110 DEG C; The mass ratio of passivator and carbon source is 0.1 ~ 0.7, and the mass ratio of phosphoric acid and carbon source is 5 ~ 30, and the mass ratio of solvent and carbon source is 20 ~ 100. Carbon source is xitix; Passivator is any one in glycine, tyrosine, phenylalanine, L-glutamic acid; Solvent is any one in ethylene glycol, glycol ether, ethanol.
Embodiment 1:
By the glycine of the xitix of 0.50 gram and 0.10 gram, the phosphoric acid of 8.5 grams is dissolved in 30 grams of ethylene glycol, is transferred in hydrothermal reaction kettle by solution, and 90 DEG C process 3 hours, naturally cool to room temperature, obtain the carbon point solution of yellow. Under 365nm ultra violet lamp, the yellow fluorescence of this carbon point aqueous solution emitting bright.
As optional alternative, ethylene glycol can also use glycol ether, ethanol to replace, and can realize the carbon point being obtained by reacting equally.
Fig. 1 is the X-ray diffractogram of carbon point prepared by the present embodiment, has a very wide peak about 2 θ=22 °, and this peak is the characteristic peak of the amorphous state of carbon.
Fig. 2 is the transmission electron microscope photo of carbon point prepared by the present embodiment, can find out the carbon point shape looks equal of preparation by photo, and particle diameter about 5 nanometers, favorable dispersity, has good application prospect in the field such as bioanalysis, catalysis.
Fig. 3 is the infrared spectrogram of carbon point prepared by embodiment 1, and ~ 3420cm-1 is the absorption of vibrations of-OH, and～1640cm-1 is the characteristic peak of C=O, and～1150cm-1 is the stretching vibration of P=O in P=O (OH) 2 group. Infrared spectra shows that phosphoric acid has participated in reaction and made carbon point surface-functionalized.
Fig. 4 is the fluorescence spectrum figure after the carbon point solution with water that the present embodiment obtains is diluted. As seen from the figure, carbon point solution has fluorescence excitation wavelength dependency, and along with the increase of excitation wavelength, fluorescent emission peak intensity first strengthens and declines afterwards, and the trend of red shift occurs in peak position.
Embodiment 2:
Under room temperature, by the tyrosine of the xitix of 0.50 gram and 0.20 gram, the phosphoric acid of 2.5 grams is dissolved in 10 grams of ethylene glycol, is transferred in hydrothermal reaction kettle by solution, and 110 DEG C process 1 hour, naturally cool to room temperature, obtain the carbon point solution of yellow.
Embodiment 3:
Under room temperature, by the tyrosine of the xitix of 0.50 gram and 0.20 gram, the phosphoric acid of 2.5 grams is dissolved in 10 grams of ethylene glycol, is transferred in hydrothermal reaction kettle by solution, and 110 DEG C process 1 hour, naturally cool to room temperature, obtain the carbon point solution of yellow.
Embodiment 4:
Under room temperature, by the L-glutamic acid of the xitix of 0.50 gram and 0.35 gram, the phosphoric acid of 10 grams is dissolved in 30 grams of ethylene glycol, is transferred in hydrothermal reaction kettle by solution, and 80 DEG C process 5 hours, naturally cool to room temperature, obtain the carbon point solution of yellow.
Claims (3)
1. one kind is synthesized the method for glassy yellow fluorescent carbon point, it is characterised in that, described method comprises the following steps:
By the glycine of the xitix of 0.50 gram and 0.10 gram, the phosphoric acid of 8.5 grams is dissolved in 30 grams of ethylene glycol, is transferred in hydrothermal reaction kettle by solution, and 90 DEG C process 3 hours, naturally cool to room temperature, obtain the carbon point solution of yellow.
2. one kind is synthesized the method for glassy yellow fluorescent carbon point, it is characterised in that, described method comprises the following steps:
Under room temperature, by the tyrosine of the xitix of 0.50 gram and 0.20 gram, the phosphoric acid of 2.5 grams is dissolved in 10 grams of ethylene glycol, is transferred in hydrothermal reaction kettle by solution, and 110 DEG C process 1 hour, naturally cool to room temperature, obtain the carbon point solution of yellow.
3. one kind is synthesized the method for glassy yellow fluorescent carbon point, it is characterized in that, described method comprises the following steps: under room temperature, by the L-glutamic acid of the xitix of 0.50 gram and 0.35 gram, the phosphoric acid of 10 grams is dissolved in 30 grams of ethylene glycol, is transferred in hydrothermal reaction kettle by solution, and 80 DEG C process 5 hours, naturally cool to room temperature, obtain the carbon point solution of yellow.
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| CN105219386A (en) * | 2015-11-06 | 2016-01-06 | 东华大学 | A kind of preparation method of carbon quantum dot of no cytotoxicity of unprotect gas |
| US11066599B2 (en) | 2016-01-26 | 2021-07-20 | Nissan Chemical Industries, Ltd. | Production method for carbon-based light-emitting material |
| CN105688898B (en) * | 2016-03-08 | 2017-11-28 | 沈阳大学 | Method and the application of Nano Silver photochemical catalyst are prepared under light radiation using fluorescent carbon point |
| CN106381143B (en) * | 2016-08-30 | 2020-09-15 | 上海交通大学 | Method for batch green synthesis of nitrogen and phosphorus doped fluorescent carbon dots |
| CN106974659A (en) * | 2017-05-20 | 2017-07-25 | 复旦大学 | A kind of latent fingerprint detection method based on red fluorescence carbon point material |
| CN106995699B (en) * | 2017-05-31 | 2018-06-01 | 中国矿业大学 | Carbon quantum dot prepared by the method and this method of the adjustable fluorescent carbon point of a large amount of synthetic wavelengths |
| CN107384384B (en) * | 2017-07-17 | 2021-01-15 | 太原理工大学 | Preparation method of blue-green light carbon quantum dots with pH response |
| CN108455564B (en) * | 2018-02-05 | 2020-04-10 | 中南民族大学 | Method for preparing yellow or green carbon dots |
| CN109097036A (en) * | 2018-09-06 | 2018-12-28 | 中国药科大学 | A kind of longer emission wavelength fluorescent carbon quantum dot and preparation method thereof |
| CN112409602A (en) * | 2019-08-21 | 2021-02-26 | Tcl集团股份有限公司 | Nano material, preparation method thereof and printing display material |
| CN110482527A (en) * | 2019-08-29 | 2019-11-22 | 临沂大学 | A kind of fast preparation method for converting double fluorescent carbon points up and down |
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| CN103086355A (en) * | 2013-02-01 | 2013-05-08 | 浙江大学 | Synthetic method of carbon quantum dot material |
| CN103602332A (en) * | 2013-11-15 | 2014-02-26 | 沈阳药科大学 | Preparation method of carbon nanoparticle with high luminous intensity |
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| CN103086355A (en) * | 2013-02-01 | 2013-05-08 | 浙江大学 | Synthetic method of carbon quantum dot material |
| CN103602332A (en) * | 2013-11-15 | 2014-02-26 | 沈阳药科大学 | Preparation method of carbon nanoparticle with high luminous intensity |
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| Low temperature synthesis of highly stable phosphate functionalized two color carbon nanodots and their application in cell imaging;Zi-Qiang Xu等;《CARBON》;20130910;第66卷;第351-360页 * |
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