CN115820250B - Method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots - Google Patents
Method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots Download PDFInfo
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Abstract
The invention discloses a method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots. The prepared hydrophilic or hydrophobic carbon quantum dots are spherical particles with the particle size of 1-20nm and are uniformly distributed, and have an amorphous carbon structure. The two carbon quantum dots have excellent and stable fluorescence characteristics, the fluorescence quantum yield is 50% -80%, and the hydrophilic and hydrophobic properties of the two carbon quantum dots are easy to adjust.
Description
Technical Field
The invention relates to the technical field of fluorescent nano materials, in particular to a method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots.
Background
As an emerging fluorescent material, carbon quantum dots have shown unique properties in the fields of sensing, bioimaging, drug delivery, photocatalysis, and electrocatalysis. The carbon quantum dots show adjustable fluorescence emission property and chemical stability, besides good biocompatibility and low toxicity, the carbon quantum dots can be used as a new generation fluorescent probe in the fields of biological imaging and biological marking.
Currently, most of the carbon quantum dots contain oxygen or nitrogen groups such as carboxyl, hydroxyl, amino and the like on the surface, so that the carbon quantum dots are mostly hydrophilic. However, hydrophobic carbon quantum dots are of little interest because of synthesis difficulties and limited practical application due to incompatible aqueous environments.
Therefore, a one-step method is developed to synthesize the carbon quantum dots with two performances (hydrophilic and hydrophobic) at the same time, and the hydrophilicity or the hydrophobicity of the carbon quantum dots is regulated by controlling the proportion of raw materials and the reaction time, so that the method has important significance for practical application in different scenes.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots, and the two carbon quantum dots prepared by the method have excellent fluorescence performance, and the hydrophilicity or the hydrophobicity of the carbon quantum dots is regulated by controlling the proportion of raw materials and the reaction time.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the method for simultaneously synthesizing the hydrophilic carbon quantum dots and the hydrophobic carbon quantum dots provided by the invention comprises the following steps:
s1, taking organic acid as a carbon source, taking organic amine as a passivating agent, and dissolving the organic acid in a solvent;
s2, placing the mixed solution into a microwave oven for heating;
s3, after the reaction is finished, naturally cooling, adding ultrapure water, wherein the dissolved part is hydrophilic carbon quantum dots, and the insoluble part is hydrophobic carbon quantum dots.
Preferably, the organic acid is one or more of tartaric acid, oxalic acid, malic acid, citric acid, ascorbic acid, benzoic acid, salicylic acid and caffeic acid.
Preferably, the mass of one or more of tartaric acid, oxalic acid, malic acid, citric acid, ascorbic acid, benzoic acid, salicylic acid and caffeic acid is 0.01g-20.0g.
Preferably, the organic amine is one or more of ethylamine, ethylenediamine, diethylamine, diethylenetriamine, mercaptoethylamine, p-phenylenediamine and aniline.
Preferably, the mass of one or more of ethylamine, ethylenediamine, diethylamine, diethylenetriamine, mercaptoethylamine, p-phenylenediamine and aniline is 0.01g-20.0g.
Preferably, the solvent is any one of ethanol, benzene, carbon disulfide, carbon tetrachloride, water and sulfuric acid, and the volume is 5-30mL.
Preferably, the heating power of the microwave oven is 600-750W, and the heating time is 1-10min.
Preferably, the method also comprises S4, a method for regulating and controlling the hydrophilic/hydrophobic properties of the two carbon quantum dots, specifically, respectively dissolving organic acid with the same mass and organic amine with different mass in a certain solvent, and then placing the mixed solution in a microwave oven for heating for the same time; or respectively dissolving the organic acid with the same mass and the organic amine with the same mass in a certain solvent, and then placing the mixed solution in a microwave oven for heating for different times.
Preferably, the mass of the organic acid is 0.01g-20.0g; the mass of the organic amine with different mass is 0.01-4.0 g, 0.01-8.0 g, 0.01-12.0 g, 0.01-16.0 g and 0.01-20.0 g respectively.
Preferably, the heating time in the microwave oven is 1-5 min, 1-8 min, 1-11 min and 1-14 min respectively.
Compared with the prior art, the two carbon quantum dots prepared by the method have excellent chemical stability, good biocompatibility, low toxicity and excellent optical performance; the two carbon quantum dots have extremely high fluorescence quantum yield, strong repeatability and low cost; the hydrophilic carbon quantum dots and the hydrophobic carbon quantum dots are directly synthesized at the same time through a one-step method, and the preparation process is simple and easy to popularize.
Drawings
FIG. 1 is a transmission electron micrograph of hydrophilic carbon quantum dots;
FIG. 2 is a transmission electron micrograph of hydrophobic carbon quantum dots;
FIG. 3 is a photograph of a hydrophilic/hydrophobic carbon quantum dot prepared by a one-step process;
FIG. 4 is a fluorescence spectrum A) of hydrophilic carbon quantum dots at different excitation wavelengths; b) Hydrophobic carbon quantum dots.
Detailed Description
The invention is further illustrated below in connection with specific embodiments.
In this example, 0.01g-20.0g of one or more of organic acid-tartaric acid, oxalic acid, malic acid, citric acid, ascorbic acid, benzoic acid, salicylic acid and caffeic acid are taken as carbon sources, 0.01g-20.0g of one or more of organic amine-ethylamine, ethylenediamine, diethylamine, diethylenetriamine, mercaptoethylamine, p-phenylenediamine and aniline are taken as passivating agents, one of 5-30mL of solvents of ethanol, benzene, carbon disulfide, carbon tetrachloride, water and sulfuric acid is added for dissolution, the mixture is placed into a microwave oven with heating power of 600-750W for heating for 1-10min, after the sample is cooled to room temperature, 1-30mL of ultrapure water is added, the portion dissolved in the ultrapure water is the hydrophilic carbon quantum dots, and the portion insoluble in the ultrapure water is the hydrophobic carbon quantum dots, as shown in fig. 1-3.
Organic acid: the mass ratio of the organic amine is 1:0.01 to 1:0.5, the yield of the hydrophilic carbon quantum dots is greater than that of the hydrophobic carbon dots;
organic acid: the mass ratio of the organic amine is 1:0.5 to 1:10, the yield of the hydrophobic carbon quantum dots is greater than that of the hydrophilic carbon dots;
the reaction time is 1-15 min, and the proportion of hydrophobic carbon points increases with the increase of temperature.
And detecting the optimal excitation wavelength of the hydrophilic/hydrophobic carbon quantum dots by using the prepared two carbon quantum dot samples, and respectively detecting the fluorescence intensity by using a fluorescence spectrophotometer at the wavelength of 300-400 nm as shown in figure 4, so as to determine the optimal excitation wavelength of the hydrophilic carbon quantum dots and the optimal excitation wavelength of the hydrophobic carbon quantum dots, wherein the optimal excitation wavelength of the hydrophilic carbon quantum dots is 360-380nm, and the excitation wavelength of the hydrophobic carbon dots is 380-400nm.
The method of the embodiment utilizes a carbon source to prepare two carbon quantum dots with opposite performances simultaneously by a one-step method. One of the carbon quantum dots is a hydrophilic carbon dot, and the other carbon quantum dot is a hydrophobic carbon dot. The prepared hydrophilic or hydrophobic carbon quantum dots are spherical particles with the particle size of 1-20nm and are uniformly distributed, and have an amorphous carbon structure. The two carbon quantum dots have excellent and stable fluorescence characteristics, and the fluorescence quantum yield is 50% -80%. The hydrophilic and hydrophobic properties of the two carbon quantum dots are easy to adjust.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (9)
1. The method for simultaneously synthesizing the hydrophilic carbon quantum dots and the hydrophobic carbon quantum dots is characterized by comprising the following steps of:
s1, taking organic acid as a carbon source, taking organic amine as a passivating agent, and dissolving the organic acid in a solvent;
s2, heating the mixed solution obtained in the step S1 in a microwave oven;
s3, after the reaction is finished, naturally cooling, adding ultrapure water, wherein the dissolved part is hydrophilic carbon quantum dots, and the insoluble part is hydrophobic carbon quantum dots;
s4, regulating and controlling the hydrophilic/hydrophobic properties of the two carbon quantum dots, namely respectively dissolving the organic acid with the same mass and the organic amine with different mass in a certain solvent, and then heating the mixed solution of the organic acid and the organic amine in a microwave oven for the same time; or respectively dissolving the organic acid with the same mass and the organic amine with the same mass in a certain solvent, and then placing the mixed solution in a microwave oven for heating for different times.
2. The method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots according to claim 1, wherein the organic acid is one or more of tartaric acid, oxalic acid, malic acid, citric acid, ascorbic acid, benzoic acid, salicylic acid, and caffeic acid.
3. The method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots according to claim 2, wherein the mass of one or more of tartaric acid, oxalic acid, malic acid, citric acid, ascorbic acid, benzoic acid, salicylic acid and caffeic acid is 0.01g-20.0g.
4. The method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots according to claim 1, wherein the organic amine is one or more of ethylamine, ethylenediamine, diethylamine, diethylenetriamine, mercaptoethylamine, p-phenylenediamine, and aniline.
5. The method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots according to claim 4, wherein the mass of one or more of ethylamine, ethylenediamine, diethylamine, diethylenetriamine, mercaptoethylamine, p-phenylenediamine and aniline is 0.01g-20.0g.
6. The method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots according to claim 1, wherein the solvent is any one of ethanol, benzene, carbon disulfide, carbon tetrachloride, water and sulfuric acid, and the volume is 5-30mL.
7. The method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots according to claim 1, wherein the heating power of the microwave oven is 600-750W, and the heating time is 1-10min.
8. The method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots according to claim 1, wherein the organic acid has a mass of 20.0g; the mass of the organic amine with different mass is respectively 4.0g, 8.0g, 12.0g, 16.0g and 20.0g.
9. The method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots according to claim 1, wherein the heating time in the microwave oven is 5min, 8min, 11min, 14min, respectively.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104789217A (en) * | 2015-04-28 | 2015-07-22 | 安徽大学 | Amphipathy carbon quantum dot and preparation method thereof |
| CN104845619A (en) * | 2015-05-25 | 2015-08-19 | 广西师范学院 | Rapid synthesis method for high-quantum-yield fluorescent carbon dots |
| CN108410455A (en) * | 2018-03-07 | 2018-08-17 | 河南大学 | A kind of method of simultaneously synthesizing hydrophilic, hydrophobic carbon dots and its in detection Au3+With the application prepared in white light emitting diode |
| 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 |
| CN109399607A (en) * | 2018-11-01 | 2019-03-01 | 新乡医学院 | A kind of preparation method by the amphipathic carbon quantum dot of microwave method rapid synthesis |
| CN111718713A (en) * | 2020-07-21 | 2020-09-29 | 中南民族大学 | Carbon dot, preparation method and application thereof, and solid luminescent forming material |
| CN115128047A (en) * | 2021-03-24 | 2022-09-30 | 湖州恺文微纳科技股份有限公司 | Method for preparing hydrophilic-hydrophobic strength-adjustable fluorescent carbon dots at oil-water interface in one step |
| CN115124996A (en) * | 2021-03-24 | 2022-09-30 | 湖州恺文微纳科技股份有限公司 | Preparation method of hydrophilic-hydrophobic adjustable fluorescent carbon dots |
| CN115216294A (en) * | 2022-06-22 | 2022-10-21 | 成都理工大学 | Method for preparing peroxyoxalate-carbon dot chemiluminescent gel by light sensation |
-
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- 2022-12-20 CN CN202211642820.1A patent/CN115820250B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104789217A (en) * | 2015-04-28 | 2015-07-22 | 安徽大学 | Amphipathy carbon quantum dot and preparation method thereof |
| CN104845619A (en) * | 2015-05-25 | 2015-08-19 | 广西师范学院 | Rapid synthesis method for high-quantum-yield fluorescent carbon dots |
| CN108410455A (en) * | 2018-03-07 | 2018-08-17 | 河南大学 | A kind of method of simultaneously synthesizing hydrophilic, hydrophobic carbon dots and its in detection Au3+With the application prepared in white light emitting diode |
| 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 |
| CN109399607A (en) * | 2018-11-01 | 2019-03-01 | 新乡医学院 | A kind of preparation method by the amphipathic carbon quantum dot of microwave method rapid synthesis |
| CN111718713A (en) * | 2020-07-21 | 2020-09-29 | 中南民族大学 | Carbon dot, preparation method and application thereof, and solid luminescent forming material |
| CN115128047A (en) * | 2021-03-24 | 2022-09-30 | 湖州恺文微纳科技股份有限公司 | Method for preparing hydrophilic-hydrophobic strength-adjustable fluorescent carbon dots at oil-water interface in one step |
| CN115124996A (en) * | 2021-03-24 | 2022-09-30 | 湖州恺文微纳科技股份有限公司 | Preparation method of hydrophilic-hydrophobic adjustable fluorescent carbon dots |
| CN115216294A (en) * | 2022-06-22 | 2022-10-21 | 成都理工大学 | Method for preparing peroxyoxalate-carbon dot chemiluminescent gel by light sensation |
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