CN112266786A - Preparation method of dual-emission fluorescent carbon quantum dots with adjustable light emitting colors - Google Patents
Preparation method of dual-emission fluorescent carbon quantum dots with adjustable light emitting colors Download PDFInfo
- Publication number
- CN112266786A CN112266786A CN202011260126.4A CN202011260126A CN112266786A CN 112266786 A CN112266786 A CN 112266786A CN 202011260126 A CN202011260126 A CN 202011260126A CN 112266786 A CN112266786 A CN 112266786A
- Authority
- CN
- China
- Prior art keywords
- carbon quantum
- quantum dot
- dual
- emission
- fluorescent carbon
- 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.)
- Pending
Links
Images
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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biophysics (AREA)
- Optics & Photonics (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention relates to the field of nano material luminescence, in particular to a preparation method of a dual-emission fluorescent carbon quantum dot with adjustable luminescence color. The invention provides a preparation method of dual-emission fluorescent carbon quantum dots with adjustable light emission colors, which comprises the following steps: 1) mixing: dissolving p-phenylenediamine in a solvent to obtain a solution of the p-phenylenediamine, adding auxiliary acid into the solution under stirring, and uniformly mixing to obtain a mixed solution; wherein the solvent is ethyl acetate or glycerol; 2) reaction: carrying out solvothermal reaction on the mixed solution in the step 1) in a container, and naturally cooling to room temperature after the reaction is finished to obtain a reaction stock solution; 3) and (3) purification: centrifuging, filtering and dialyzing the reaction stock solution in the step 2). The technical scheme of the invention can solve the technical problem of single emission of the carbon quantum dots in the prior art.
Description
Technical Field
The invention relates to the field of nano material luminescence, in particular to a preparation method of a dual-emission fluorescent carbon quantum dot with adjustable luminescence color.
Background
The carbon quantum dot is a novel quasi-spherical carbon nano particle, and has the characteristics of adjustable excitation and emission wavelength range, good light stability, high fluorescence intensity and the like due to the unique structure, so that the carbon quantum dot has potential application values in the aspects of biochemical sensing, drug delivery, biomedicine, photoelectric equipment, ion detection and the like. Since the accidental discovery of carbon quantum dots in 2004, synthetic methods such as arc discharge, laser ablation, electrochemical oxidation, chemical oxidation, pyrolysis, microwave synthesis, etc. have been proposed, however, these methods require a large number of complicated instruments and extreme operating conditions, and may cause safety problems and energy waste. Moreover, most of the synthesized carbon quantum dots only show single emission, which limits the luminescent color thereof. It is therefore of particular importance to develop a carbon quantum dot with multiple, at least dual and controllable emission.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a dual-emission fluorescent carbon quantum dot with adjustable light-emitting color, so as to solve the technical problem of single emission of the carbon quantum dot in the prior art.
The inventor prepares a carbon quantum dot showing double emission in order to solve the problem of single fluorescence emission of the carbon quantum dot, and finds that different reaction solvents can regulate and control the luminescence of the carbon quantum dot so as to move the emission wavelength of the carbon quantum dot to a long wave direction.
The invention provides a preparation method of dual-emission fluorescent carbon quantum dots with adjustable light emission colors, which comprises the following steps:
1) mixing: dissolving p-phenylenediamine in a solvent to obtain a solution of the p-phenylenediamine, adding auxiliary acid into the solution under stirring, and uniformly mixing to obtain a mixed solution; wherein the solvent is ethyl acetate or glycerol;
2) reaction: carrying out solvothermal reaction on the mixed solution in the step 1) in a container, and naturally cooling to room temperature after the reaction is finished to obtain a reaction stock solution;
3) and (3) purification: centrifuging, filtering and dialyzing the reaction stock solution in the step 2).
Further, the auxiliary acid in the step 1) is phosphoric acid with the mass fraction of 85%.
Further, the mass-volume ratio of the p-phenylenediamine to the ethyl acetate or the glycerol in the step 1) is 0.1: 40; the mass-volume ratio of the p-phenylenediamine to the auxiliary acid is 0.1: 1. In the technical scheme of the application, the mass-to-volume ratio is g: and (3) ml.
Further, the temperature of the solvothermal reaction in the step 2) is 180 ℃, and the solvothermal time is 24 hours.
Further, the centrifugation rate of the step 3) is 10000 r/min; the aperture of the filtered organic filter membrane is 0.22 mu m.
Further, the centrifugation in step 3) comprises the following specific steps: centrifuging the reaction stock solution obtained in the step 2) at a centrifugal rate of 10000r/min for 10 minutes to remove insoluble large-particle impurities, and repeating the operation for three times; the centrifuged solution is filtered by a 0.22 mu m organic filter membrane to remove small particle impurities.
Further, the specific dialysis steps in step 3) are: dialyzing the filtered filtrate by using a dialysis bag with the molecular weight cutoff of 500Da for 24h to remove inorganic salt impurities.
Further, the obtained carbon quantum dots show bright green and yellow fluorescence under ultraviolet lamp irradiation.
Further, the emission peak of the carbon quantum dot has 449 nm and 503nm when the excitation wavelength is 360 nm.
Further, the carbon quantum dots have emission peaks at 465 and 513nm when the excitation wavelength is 360nm, respectively.
Compared with the prior art, the invention has the beneficial effects that: the invention discloses a preparation method of a dual-emission fluorescent carbon quantum dot with adjustable light-emitting color, which is characterized in that phosphoric acid is used as an auxiliary acid, the emission of the carbon quantum dot is regulated and controlled by changing a reaction solvent, the carbon quantum dot shows dual-emission behavior which is different from most reports, and the fluorescence emission wavelength of the carbon quantum dot is changed. The carbon quantum dots prepared by taking p-phenylenediamine as a carbon source and ethyl acetate and glycerol as solvents respectively emit bright green and yellow fluorescence, have good luminescence characteristics, and have the advantages of simple preparation method, economy and greenness.
Drawings
FIG. 1 is a graph showing fluorescence emission of carbon quantum dots obtained in example 1 of the present invention.
FIG. 2 is a graph showing fluorescence emission of carbon quantum dots obtained in example 2 of the present invention.
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Example 1:
(1) synthesis of carbon quantum dots
Weighing 0.1g of p-phenylenediamine in a beaker, adding 40mL of ethyl acetate solution, mixing, adding 1mL of phosphoric acid under the stirring condition, uniformly stirring, putting the mixed solution into a reaction kettle, carrying out solvothermal reaction at 180 ℃ for 24h, and naturally cooling to room temperature to obtain a primary product.
(2) Purification of carbon quantum dots
Centrifuging the obtained primary product at a centrifugal rate of 10000r/min for 10 minutes to remove insoluble large-particle impurities, and repeating the operation for three times; filtering the centrifuged solution by using a 0.22 mu m organic filter membrane to remove small particle impurities; then dialyzing the carbon quantum dot solution obtained after filtration for 24 hours by using a dialysis bag with the molecular weight cutoff of 500Da to remove some inorganic salt impurities; finally, the dialyzed solution is collected for standby.
To further illustrate the beneficial effects of the present invention, fluorescence spectroscopy was performed on carbon quantum dots prepared according to the method of example 1:
and (2) sucking a certain amount of the collected carbon quantum dot solution into a cuvette by using a rubber head dropper, adding deionized water for dilution and shaking up, and testing a fluorescence emission spectrogram of the carbon quantum dot by using an F-4600 fluorescence spectrometer, wherein the result is shown in figure 1, the carbon quantum dot shows dual emission behaviors, and when the excitation wavelength is 360nm, the emission peaks of the carbon quantum dot respectively have the wavelengths of 449 (blue fluorescence) and 503nm (cyan fluorescence), and bright green fluorescence is shown under the irradiation of an ultraviolet lamp.
Example 2:
(1) synthesis of carbon quantum dots
Weighing 0.1g of p-phenylenediamine in a beaker, adding 40mL of glycerol, mixing, adding 1mL of phosphoric acid under the stirring condition, uniformly stirring, putting the mixed solution into a reaction kettle, carrying out solvothermal reaction at 180 ℃ for 24h, and naturally cooling to room temperature to obtain a primary product.
(2) Purification of carbon quantum dots
Centrifuging the obtained primary product at a centrifugal rate of 10000r/min for 10 minutes to remove insoluble large-particle impurities, and repeating the operation for three times; filtering the centrifuged solution by using a 0.22 mu m organic filter membrane to remove small particle impurities; then dialyzing the carbon quantum dot solution obtained after filtration for 24 hours by using a dialysis bag with the molecular weight cutoff of 500Da to remove some inorganic salt impurities; finally, the dialyzed solution is collected for standby.
To further illustrate the beneficial effects of the present invention, fluorescence spectroscopy was performed on carbon quantum dots prepared according to the method of example 2:
and (3) sucking a certain amount of the collected carbon quantum dot solution into a cuvette by using a rubber head dropper, adding deionized water for dilution and shaking up, and testing a fluorescence emission spectrogram of the carbon quantum dot by using an F-4600 fluorescence spectrometer, wherein the result is shown in figure 2, the carbon quantum dot shows dual emission behaviors, when the excitation wavelength is 360nm, the emission peaks of the carbon quantum dot respectively have the wavelengths of 465 (blue fluorescence) and 513nm (green fluorescence), and bright yellow fluorescence is shown under the irradiation of an ultraviolet lamp.
Claims (10)
1. A preparation method of double-emission fluorescent carbon quantum dots with adjustable light emission colors is characterized by comprising the following steps:
1) mixing: dissolving p-phenylenediamine in a solvent to obtain a solution of the p-phenylenediamine, adding auxiliary acid into the solution under stirring, and uniformly mixing to obtain a mixed solution; wherein the solvent is ethyl acetate or glycerol;
2) reaction: carrying out solvothermal reaction on the mixed solution in the step 1) in a container, and naturally cooling to room temperature after the reaction is finished to obtain a reaction stock solution;
3) and (3) purification: centrifuging, filtering and dialyzing the reaction stock solution in the step 2).
2. The method for preparing the dual-emission fluorescent carbon quantum dot with adjustable luminescent color according to claim 1, wherein the auxiliary acid in step 1) is phosphoric acid.
3. The method for preparing the dual-emission fluorescent carbon quantum dot with adjustable luminescent color according to claim 1 or 2, wherein the mass-to-volume ratio of the p-phenylenediamine to the ethyl acetate or the glycerol in the step 1) is 0.1: 40; the mass-volume ratio of the p-phenylenediamine to the auxiliary acid is 0.1: 1.
4. The method for preparing the dual-emission fluorescent carbon quantum dot with adjustable luminescent color according to claim 1, wherein the temperature of the solvothermal reaction in the step 2) is 180 ℃, and the solvothermal time is 24 h.
5. The method for preparing the dual-emission fluorescent carbon quantum dot with adjustable light emission color according to claim 1, wherein the centrifugation rate in the step 3) is 10000 r/min; the aperture of the filtered organic filter membrane is 0.22 mu m.
6. The method for preparing the dual-emission fluorescent carbon quantum dot with adjustable light emission color according to claim 5, wherein the centrifugation in the step 3) comprises the following specific steps: centrifuging the reaction stock solution obtained in the step 2) at a centrifugal rate of 10000r/min for 10 minutes to remove insoluble large-particle impurities, and repeating the operation for three times; the centrifuged solution is filtered by a 0.22 mu m organic filter membrane to remove small particle impurities.
7. The method for preparing the dual-emission fluorescent carbon quantum dot with adjustable light emission color according to claim 1, wherein the dialysis in the step 3) comprises the following specific steps: dialyzing the filtered filtrate by using a dialysis bag with the molecular weight cutoff of 500Da for 24h to remove inorganic salt impurities.
8. The method for preparing the dual-emission fluorescent carbon quantum dot with adjustable luminescent colors according to claim 1, 6 or 7, wherein the obtained carbon quantum dot shows bright green and yellow fluorescence under the irradiation of an ultraviolet lamp.
9. The method for preparing a dual emission fluorescent carbon quantum dot with tunable emission color according to claim 7, wherein the emission peak of the carbon quantum dot has 449 nm and 503nm wavelengths when the excitation wavelength is 360 nm.
10. The method for preparing a dual-emission fluorescent carbon quantum dot with tunable emission color as claimed in claim 6, wherein the emission peak of the carbon quantum dot has a wavelength of 465 nm and 513nm when the excitation wavelength is 360 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011260126.4A CN112266786A (en) | 2020-11-12 | 2020-11-12 | Preparation method of dual-emission fluorescent carbon quantum dots with adjustable light emitting colors |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011260126.4A CN112266786A (en) | 2020-11-12 | 2020-11-12 | Preparation method of dual-emission fluorescent carbon quantum dots with adjustable light emitting colors |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112266786A true CN112266786A (en) | 2021-01-26 |
Family
ID=74339957
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011260126.4A Pending CN112266786A (en) | 2020-11-12 | 2020-11-12 | Preparation method of dual-emission fluorescent carbon quantum dots with adjustable light emitting colors |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112266786A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115924887A (en) * | 2022-12-29 | 2023-04-07 | 北京建工环境修复股份有限公司 | Preparation method of novel carbon dot material and application of novel carbon dot material in detection of perfluorinated compounds |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104591124A (en) * | 2014-12-10 | 2015-05-06 | 西南交通大学 | Preparation method for fluorescent carbon quantum dot with vitamin as carbon source |
| CN106147760A (en) * | 2015-04-07 | 2016-11-23 | 中国科学院大连化学物理研究所 | A kind of preparation method of transient metal doped carbon fluorescence quantum |
| CN106995699A (en) * | 2017-05-31 | 2017-08-01 | 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 |
| CN108545715A (en) * | 2018-04-04 | 2018-09-18 | 桂林理工大学 | A kind of preparation method for the red fluorescence carbon dots that transmitting does not change with excitation wavelength |
-
2020
- 2020-11-12 CN CN202011260126.4A patent/CN112266786A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104591124A (en) * | 2014-12-10 | 2015-05-06 | 西南交通大学 | Preparation method for fluorescent carbon quantum dot with vitamin as carbon source |
| CN106147760A (en) * | 2015-04-07 | 2016-11-23 | 中国科学院大连化学物理研究所 | A kind of preparation method of transient metal doped carbon fluorescence quantum |
| CN106995699A (en) * | 2017-05-31 | 2017-08-01 | 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 |
| CN108545715A (en) * | 2018-04-04 | 2018-09-18 | 桂林理工大学 | A kind of preparation method for the red fluorescence carbon dots that transmitting does not change with excitation wavelength |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115924887A (en) * | 2022-12-29 | 2023-04-07 | 北京建工环境修复股份有限公司 | Preparation method of novel carbon dot material and application of novel carbon dot material in detection of perfluorinated compounds |
| CN115924887B (en) * | 2022-12-29 | 2024-02-06 | 北京建工环境修复股份有限公司 | Preparation method of carbon dot material and application of carbon dot material in detection of perfluorinated compounds |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Mu et al. | Carbogenic nanodots derived from organo-templated zeolites with modulated full-color luminescence | |
| EP0498689B1 (en) | Mixed lanthanum terbium and cerium phosphate, process for its preparation | |
| CN106398693A (en) | Preparation method and application of nitrogen doped yellow fluorescent carbon dots | |
| Baldovi et al. | Highly fluorescent C-dots obtained by pyrolysis of quaternary ammonium ions trapped in all-silica ITQ-29 zeolite | |
| CN110451483B (en) | Preparation method for synthesizing fluorescent carbon quantum dots by taking kiwi fruits as raw materials | |
| CN108545715A (en) | A kind of preparation method for the red fluorescence carbon dots that transmitting does not change with excitation wavelength | |
| CN102504815A (en) | Fluorescent carbon quantum dot and its preparation method and application | |
| CN112266786A (en) | Preparation method of dual-emission fluorescent carbon quantum dots with adjustable light emitting colors | |
| CN106497561B (en) | Method for preparing graphene quantum dot yellow fluorescent powder or mixture thereof and method for preparing white light LED device | |
| EP0524034B1 (en) | Mixed lanthanum terbium and cerium phosphate, process for its preparation from insoluble rare earth salts | |
| CN106219513A (en) | A kind of method utilizing solid-phase pyrolysis to prepare nitrogen-doped carbon quantum dot and application thereof | |
| CN107603610A (en) | Preparation method from mature vinegar carbon nano-particles | |
| CN114426845A (en) | Fluorescent carbon quantum dot-based probe and application thereof in detecting water content in organic solvent | |
| CN111286321B (en) | Preparation method and application of flavonoid fluorescent nano material | |
| CN111286322B (en) | Carbon dots capable of detecting hypochlorous acid in real time and visually, and preparation method and application thereof | |
| CN110272738A (en) | A kind of preparation method of secondary color fluorescent carbon quantum dot | |
| CN110987883B (en) | Correction method for reducing influence of soil organic matters on polycyclic aromatic hydrocarbon fluorescence working curve | |
| CN104910904B (en) | A kind of with sulfonated coal for carbon source by the simple and quick method preparing fluorescent carbon quantum dot of ozone oxidation photo-reduction technology | |
| CN110171806B (en) | Preparation method of water-soluble red light sulfur quantum dots | |
| CN109762560A (en) | A kind of preparation method of two kinds of fluorescence property graphene quantum dots of disposable synthesis | |
| Sadighian et al. | Rapid sampling during synthesis of lead halide perovskite nanocrystals for spectroscopic measurement | |
| CN110724528A (en) | Rosin-based carbon dot material and preparation method and application thereof | |
| CN115043393B (en) | Super-long phosphorescent keratin derived carbon quantum dot and preparation method thereof | |
| CN112852412A (en) | Method for rapidly synthesizing high-fluorescence sulfur quantum dots | |
| CN113088284A (en) | Method for preparing fluorescent graphene quantum dots by using organic dye and application of fluorescent graphene quantum dots |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210126 |