CN115125001A - Preparation method of green luminescent carbon dots - Google Patents
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Abstract
The invention discloses a preparation method of green luminescent carbon dots, which takes coffee grounds as raw materials, and comprises the steps of firstly carbonizing the raw materials at high temperature, then carrying out hydrothermal treatment on the raw materials after high-temperature carbonization under an acidic condition, and then carrying out hydrothermal treatment under an alkaline condition to obtain the green luminescent carbon dots. The carbon dots can be directly shot under the common illumination condition of a laboratory to observe bright and single green, the carbon dots do not need to be shot under the irradiation of ultraviolet light, the carbon dots have high luminous efficiency and high luminous brightness, and the problems of poor monochromaticity, low luminous efficiency and low luminous brightness of the common carbon dots are solved. The preparation method is simple and easy to implement, the carbon dots have high brightness, good monochromaticity and excellent luminescence property, and the carbon dots can be assisted to obtain better luminescence property, thereby showing strong application potential in the fields of image probes, fluorescent tracing, luminescence and the like.
Description
Technical Field
The invention relates to a preparation method of a carbon dot, in particular to a preparation method of an N-P co-doped green luminescent carbon dot with high luminescent efficiency, and belongs to the technical field of luminescent materials and application.
Background
The carbon dots are also called carbon nano particles, carbon nano dots and nano-scale graphite phase carbon particles, and refer to a carbon core structure with single-layer or less than 5-layer graphene, the size of the carbon core structure is usually less than 100 nanometers, the size of the carbon dots is determined by a layered structure to have typical anisotropy, the transverse size is larger than the longitudinal height, and the size of the carbon dots is the transverse size and has a typical carbon lattice structure.
Carbon dots have important applications in the fields of biosensors, medical imaging devices, and light emitting diodes. Carbon dots as a light emitting material are generally spherical structures, and can be classified into carbon nanodots with distinct lattices and carbon nanodots without lattices. Due to the diversity of the carbon nano-dot structure, the carbon nano-dot luminescent center, the luminescent mechanism and the luminescent efficiency prepared in different modes are greatly different. Generally, the luminous peak of the luminous carbon dot is relatively wide, and the luminous efficiency is not high, which limits the application, the luminous efficiency of the carbon dot is not controlled by the carbon nucleus, and the surface group of the carbon dot has non-negligible influence on the luminous efficiency.
Disclosure of Invention
The invention aims to provide a preparation method of a green luminescent carbon dot with high brightness and good monochromaticity, the method has simple operation process, good repeatability and convenient industrial production, and the obtained carbon dot can emit single green light, has high brightness and luminous efficiency and stronger application potential.
The invention takes coffee grounds as raw materials, firstly carries out high-temperature carbonization on the raw materials, and then carries out special acid-base water heat treatment on the raw materials after high-temperature carbonization to obtain green luminous carbon dots, the brightness of the carbon dots is high, and the brightness of the carbon dots is closely related to the combination of the two steps of the high-temperature carbonization and the acid-base water heat treatment.
The coffee grounds used in the invention refer to residues left on filter paper after coffee making, and the coffee grounds contain elements such as carbon, nitrogen, phosphorus and the like, and can be used as raw materials for doping carbon dots with nitrogen and phosphorus, thereby improving the luminescence property of the carbon dots.
Further, the high-temperature carbonization according to the present invention means that coffee grounds containing nitrogen and phosphorus are subjected to high-temperature calcination in an inert atmosphere to be carbonized. The inert gas atmosphere may be an inert gas such as nitrogen or argon. The purpose of the calcination is to fully carbonize the coffee grounds, and the temperature and time are selected to meet this requirement. For example, the conventional carbonization temperature is generally 600-800 ℃, and at the high temperature, the coffee grounds can be rapidly converted into the highly crystalline nitrogen and phosphorus co-doped graphite phase carbon, and the calcination time is generally 0.5-2 hours. The existence of nitrogen and phosphorus in the coffee grounds is beneficial to improving the luminous brightness of carbon dots, and the obtained carbon dots have narrow spectrum and good monochromaticity.
Further, the special alkali water heat treatment of the invention comprises the following steps: firstly, the raw material carbonized at high temperature is subjected to hydrothermal treatment (acid treatment for short) under an acidic condition, and then is subjected to hydrothermal treatment (alkali treatment for short) under an alkaline condition. The specific operation mode of the acidic hydrothermal treatment is as follows: grinding the raw material obtained by high-temperature carbonization and oleic acid together, and then dispersing the ground mixture into a hydrochloric acid solution for hydrothermal treatment. The raw material obtained by high-temperature carbonization and the oleic acid are jointly ground to increase the dispersibility of the raw material, and the dosage relationship of the raw material and the oleic acid after high-temperature carbonization is 2-10 g: 0.5-3 mL. The acid treatment aims to reduce the particle size of larger carbon particles and provide a prerequisite for the next alkali treatment, the concentration of the hydrochloric acid solution is 0.05-0.15mol/L, the temperature of the acid treatment is 50-80 ℃, and the treatment time is 0.5-1 hour. When the acid treatment is carried out, the dosage of the sample and the hydrochloric acid solution has no special requirement, as long as the sample can be completely immersed in the hydrochloric acid solution, and the whole acid treatment process can be carried out under the ultrasonic condition for the sufficient reaction of the sample and the acid.
Further, the sample after high temperature carbonization is firstly ground into fine powder and then mixed with oleic acid. After acid treatment, the treated sample is washed to neutrality, dried and then subjected to alkali treatment.
Further, the specific operation mode of the hydrothermal treatment under the alkaline condition is as follows: and adding the acid-treated sample into a sodium hydroxide solution for hydrothermal treatment. The purpose of the alkali treatment is to enable sodium ions and hydroxide ions to enter layers in an intercalation mode, the number of layers of carbon points is reduced, the crystallinity and the dispersity of the carbon points can be increased through hydrothermal treatment, high-brightness luminescence is obtained, the concentration of a NaOH solution is 0.05-0.15mol/L, the temperature of the alkali treatment is 120-200 ℃, and the treatment time is 1-5 hours. In the alkali treatment, the dosage of the sample and the sodium hydroxide solution has no special requirement, as long as the sample can be completely immersed in the sodium hydroxide solution.
Further, after alkali treatment, the sample is washed to be neutral, then dried and dispersed into a mercaptoacetic acid water solution, and the green luminescent carbon dots with good dispersibility are obtained. The aqueous solution of thioglycolic acid enables better dispersion of the carbon dots and prevents agglomeration of the carbon dots, and the concentration of the thioglycolic acid is generally 0.5 to 2 wt%.
In one embodiment of the present invention, a method for preparing a specific green luminescent carbon dot is provided, which comprises the following steps:
(1) calcining 10g of coffee grounds containing nitrogen and phosphorus at the temperature of 600 ℃ and 800 ℃ for 0.5-2 hours under the inert condition, and grinding the coffee grounds into fine powder for later use;
(2) taking 2-10g of the fine powder obtained in the step (1), dropwise adding 0.5-3 mL of oleic acid, grinding in an agate mortar, dispersing into 0.1M hydrochloric acid solution, ultrasonically dispersing for 0.5 h at 50-80 ℃, then centrifugally separating, washing to neutrality, and drying;
(3) taking 2-10g of the fine powder in the step (2), putting the fine powder into 0.1M NaOH solution, reacting for 1-5 hours at the temperature of 120-200 ℃, then centrifugally separating, washing to be neutral, drying, and dispersing the dried powder into aqueous solution containing 1wt% of thioglycolic acid to obtain the green luminescent carbon dot.
The carbon dots are prepared by a special method, the particle size of the obtained carbon dot particles is less than 20 nanometers, the single green light can be emitted, the luminous brightness is high, the luminous efficiency is high, bright green can be observed under the condition of a common photo, the carbon dots can be assisted to obtain better luminous property, and the carbon dots have strong application potential in the fields of imaging probes and luminescence.
According to the invention, the high-crystallinity graphite phase carbon is obtained by taking coffee grounds containing nitrogen and phosphorus as raw materials by using a high-temperature carbonization method for the first time, the crystallinity of the graphite phase carbon is enhanced, and then the graphite phase carbon is subjected to acid-base hydrothermal treatment to obtain the green luminous carbon dots with high luminous brightness. The preparation method is simple and easy to implement, the carbon dots have high brightness, good monochromaticity and excellent luminescence property, and the carbon dots can be assisted to obtain better luminescence property, thereby showing strong application potential in the fields of image probes, fluorescent tracing, luminescence and the like.
Drawings
FIG. 1 is a photoluminescence spectrum and a picture under normal lighting conditions of a product obtained in example 1 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which should be understood as being merely illustrative and not limiting.
Example 1
1.1 calcining 10g of coffee grounds containing nitrogen and phosphorus for 1 hour at 700 ℃ under an inert condition, and then grinding into fine powder for later use;
1.2, 5 g of the fine powder obtained in the step 1.1 is taken, 1 mL of oleic acid is dropwise added, the fine powder is ground in an agate mortar for 10 minutes, then the fine powder is dispersed in 0.1M (mol/L, the same below) hydrochloric acid solution, ultrasonic dispersion is carried out for 0.5 hour at 60 ℃, and then centrifugal separation, washing to be neutral and drying are carried out;
1.3 taking 5 g of the fine powder obtained in the step 1.2, dispersing the fine powder into a 0.1M NaOH solution, reacting for 3 hours at 150 ℃, then carrying out centrifugal separation, washing to be neutral, drying, dispersing the dried powder into an aqueous solution containing 1wt% of thioglycolic acid, and obtaining a solution containing green luminescent carbon dots, wherein the powder is well dispersed in the thioglycolic acid aqueous solution and does not agglomerate. The solution containing carbon dots was photographed directly under ordinary laboratory lighting conditions, and the picture is shown in fig. 1, where the solution is bright green. The solution is shot under a common illuminating lamp in a laboratory, the obtained photoluminescence spectrogram is shown in figure 1, and as can be seen from the graph, a sample shows bright green fluorescence, which indicates that the sample can be excited under the common illuminating lamp and has high brightness, and further indicates that the carbon dots synthesized by the method have good luminescent properties.
Example 2
2.1 calcining 10g of coffee grounds containing nitrogen and phosphorus for 1 hour at 600 ℃ under an inert condition, and then grinding the coffee grounds into fine powder for later use;
2.2, taking 2 g of the fine powder obtained in the step 1.1, dropwise adding 1 mL of oleic acid, grinding in an agate mortar for 10 minutes, dispersing in 0.1M (mol/L, the same below) hydrochloric acid solution, ultrasonically dispersing for 0.5 hour at 60 ℃, then centrifugally separating, washing to neutrality, and drying;
2.3 taking 4 g of the fine powder obtained in the step 1.2, dispersing the fine powder into a 0.1M NaOH solution, reacting for 3 hours at the temperature of 150 ℃, then carrying out centrifugal separation, washing to be neutral, drying, dispersing the dried powder into an aqueous solution containing 1wt% of thioglycolic acid, and obtaining a solution containing green luminescent carbon dots, wherein the powder is well dispersed in the aqueous solution of the thioglycolic acid and does not agglomerate. The carbon dot performance was similar to that of example 1, and the solution also exhibited the same green color as in fig. 1 directly under ordinary laboratory lighting conditions.
Example 3
3.1 calcining 10g of coffee grounds containing nitrogen and phosphorus for 2 hours at 600 ℃ under an inert condition, and then grinding into fine powder for later use;
3.2 taking 2 g of the fine powder obtained in the step 3.1, dropwise adding 0.5 mL of oleic acid, grinding in an agate mortar for 10 minutes, dispersing in 0.1M hydrochloric acid solution, ultrasonically dispersing at 50 ℃ for 0.5 hour, then centrifugally separating, washing to neutrality, and drying;
3.3 taking 2 g of the fine powder obtained in the step 3.2, dispersing the fine powder into a 0.1M NaOH solution, reacting for 1 hour at 120 ℃, then carrying out centrifugal separation, washing to be neutral, drying, dispersing the dried powder into an aqueous solution containing 1wt% of thioglycolic acid, and obtaining the green luminescent carbon dots, wherein the powder is well dispersed in the aqueous solution of the thioglycolic acid and does not agglomerate. The carbon dot performance was similar to that of example 1, and the solution also exhibited the same green color as in fig. 1 directly under ordinary laboratory lighting conditions.
Example 4
4.1 calcining 10g of coffee grounds containing nitrogen and phosphorus at 800 ℃ for 0.5 hour under an inert condition, and then grinding into fine powder for later use;
4.2 taking 10g of the fine powder obtained in the step 4.1, dropwise adding 3 mL of oleic acid, grinding in an agate mortar for 10 minutes, dispersing in a 0.05M hydrochloric acid solution, ultrasonically dispersing at 80 ℃ for 0.5 hour, then performing centrifugal separation, washing to neutrality, and drying;
4.3 taking 10g of the fine powder obtained in the step 4.2, dispersing the fine powder into 0.1M NaOH solution, reacting for 5 hours at the temperature of 200 ℃, then centrifugally separating, washing to be neutral, drying, and dispersing the dried powder into aqueous solution containing 1wt% of thioglycolic acid to obtain the green luminous carbon dots. The carbon dot performance was similar to example 1, and the solution also exhibited the same green color as in fig. 1 directly under ordinary laboratory lighting conditions.
Example 5
5.1 calcining 10g of coffee grounds containing nitrogen and phosphorus for 1 hour at 750 ℃ under an inert condition, and then grinding into fine powder for later use;
5.2, 6 g of the fine powder obtained in the step 5.1 is taken, 2 mL of oleic acid is dropwise added, the fine powder is ground in an agate mortar for 10 minutes, then the fine powder is dispersed in 0.15M hydrochloric acid solution, ultrasonic dispersion is carried out at 75 ℃ for 0.5 hour, and then centrifugal separation, washing to be neutral and drying are carried out;
5.3 taking 6 g of the fine powder obtained in the step 5.2, dispersing the fine powder into 0.1M NaOH solution, reacting for 3 hours at 180 ℃, then centrifugally separating, washing to be neutral, drying, and dispersing the dried powder into 1wt% of thioglycolic acid-containing aqueous solution to obtain the green luminous carbon dots. The carbon dot performance was similar to that of example 1, and the solution also exhibited the same green color as in fig. 1 directly under ordinary laboratory lighting conditions.
Comparative example 1
Carbon dots were prepared according to the method of example 1, except that: directly carrying out alkali treatment on the fine powder subjected to high-temperature carbonization, and specifically operating as follows:
calcining 10g of coffee grounds containing nitrogen and phosphorus for 1 hour at 700 ℃ under an inert condition, and then grinding into fine powder for later use;
taking 5 g of the fine powder, dispersing the fine powder into a 0.1M NaOH solution, reacting for 3 hours at 150 ℃, then centrifugally separating, washing to be neutral, drying, dispersing the dried powder into an aqueous solution containing 1wt% of thioglycolic acid, wherein the powder is well dispersed in the aqueous solution of the thioglycolic acid without agglomeration, and the solution is dark blue-green under the common illumination condition of a laboratory and does not show high-brightness green.
Comparative example 2
Carbon dots were prepared as in example 1, except that: in the step 1.1, the high-temperature calcination temperature is 500 ℃, the product is not completely carbonized, and the finally obtained product does not emit light under the irradiation of a strong ultraviolet lamp.
Comparative example 3
Carbon dots were prepared according to the method of example 1, except that: no NaOH is added in the hydrothermal process of the step 1.3, and the specific operation is as follows:
calcining 10g of coffee grounds containing nitrogen and phosphorus for 1 hour at 700 ℃ under an inert condition, and then grinding into fine powder for later use;
taking 5 g of the fine powder, dropwise adding 1 mL of oleic acid, grinding in an agate mortar for 10 minutes, dispersing in 0.1M (mol/L, the same below) hydrochloric acid solution, ultrasonically dispersing for 0.5 hour at 60 ℃, then centrifugally separating, washing to neutrality, and drying;
taking 5 g of the acid-treated fine powder, dispersing the acid-treated fine powder into water, reacting for 3 hours at the temperature of 150 ℃, then centrifugally separating and drying, dispersing the dried powder into an aqueous solution containing 1wt% of thioglycolic acid, and enabling the powder to be agglomerated together in the aqueous solution of the thioglycolic acid and not to emit light under the irradiation of a strong ultraviolet lamp.
Comparative example 4
Carbon dots were prepared according to the method of example 1, except that: the acid-base treatment sequence of steps 1.2 and 1.3 is changed, and the specific operations are as follows:
calcining 10g of coffee grounds containing nitrogen and phosphorus for 1 hour at 700 ℃ under an inert condition, and then grinding the coffee grounds into fine powder for later use;
taking 5 g of the fine powder, dispersing the fine powder into 0.1M NaOH solution, reacting for 3 hours at the temperature of 150 ℃, then centrifugally separating, washing to be neutral, and drying;
taking 5 g of the alkali-treated fine powder, dropwise adding 1 mL of oleic acid, grinding in an agate mortar for 10 minutes, dispersing in 0.1M (mol/L, the same below) hydrochloric acid solution, ultrasonically dispersing at 60 ℃ for 0.5 hour, then centrifugally separating, washing to neutrality, and drying;
the dried powder was dispersed in an aqueous solution containing 1wt% of thioglycolic acid, the powder did not disperse well in the aqueous thioglycolic acid solution, and the sample did not emit light under the irradiation of an ultraviolet lamp.
Claims (10)
1. A preparation method of green luminescent carbon dots is characterized by comprising the following steps: the method comprises the steps of taking coffee grounds as raw materials, firstly carrying out high-temperature carbonization on the raw materials, then carrying out hydrothermal treatment on the raw materials subjected to high-temperature carbonization under an acidic condition, and then carrying out hydrothermal treatment under an alkaline condition to obtain green luminescent carbon dots.
2. The method of claim 1, wherein: the temperature of the high-temperature carbonization is 600-800 ℃.
3. The method according to claim 1 or 2, characterized in that: the high-temperature carbonization is carried out under an inert atmosphere.
4. The method of claim 1, wherein: the specific operation mode of the hydrothermal treatment under the acidic condition is as follows: grinding the raw material obtained by high-temperature carbonization and oleic acid together, and then dispersing the ground mixture into a hydrochloric acid solution for hydrothermal treatment.
5. The method according to claim 4, wherein: when the hydrothermal treatment is carried out under the acidic condition, the dosage relationship of the raw material after high-temperature carbonization and oleic acid is 2-10 g: 0.5-3 mL.
6. The method for preparing a polycarbonate according to claim 4 or 5, wherein: when the hydrothermal treatment is carried out under acidic conditions, the concentration of the hydrochloric acid solution is 0.05-0.15mol/L, the treatment temperature is 50-80 ℃, and the treatment time is 0.5-1 hour.
7. The method of claim 1, wherein: the specific operation mode of the hydrothermal treatment under the alkaline condition is as follows: and adding the sample subjected to hydrothermal treatment under acidic conditions into a sodium hydroxide solution for hydrothermal treatment.
8. The method for preparing a polycarbonate resin composition according to claim 7, wherein: when the hydrothermal treatment is carried out under the alkaline condition, the concentration of the NaOH solution is 0.05-0.15mol/L, the treatment temperature is 120-200 ℃, and the treatment time is 1-5 hours.
9. The method of claim 1, 4 or 5, wherein: after hydrothermal treatment under acidic conditions, the sample is washed to neutrality, and then hydrothermal treatment is carried out under alkaline conditions.
10. The method of claim 1, wherein: the sample after the alkaline hydrothermal treatment is washed to be neutral and then dispersed into the thioglycolic acid aqueous solution.
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