CN113278415A - Preparation method and application of sulfur-nitrogen co-doped yellow fluorescent carbon dots - Google Patents
Preparation method and application of sulfur-nitrogen co-doped yellow fluorescent carbon dots Download PDFInfo
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Abstract
A preparation method and application of a sulfur-nitrogen co-doped yellow fluorescent carbon dot relate to a preparation method and application of a yellow carbon dot, and the preparation method comprises the following specific steps: dissolving o-phenylenediamine and lipoic acid in deionized water to form a mixed solution, putting the mixed solution into a polytetrafluoroethylene high-temperature reaction kettle, and putting the polytetrafluoroethylene high-temperature reaction kettle into an oven to react to obtain a solution A; secondly, putting the solution A into a centrifuge tube for centrifugation, and taking supernatant fluid as solution B; and thirdly, putting the solution B into a dialysis bag for dialysis, and freeze-drying to obtain a carbon dot solid, namely the target product yellow fluorescent carbon dot. Compared with the prior art, the carbon dots prepared by the method have good fluorescence performance, are uniform in size, less in impurities and simple and convenient in synthesis process, have a fluorescence detection function on Cr6+, and have wide application prospects in environmental monitoring and management.
Description
Technical Field
The invention relates to a preparation method and application of a sulfur-nitrogen co-doped yellow fluorescent carbon dot.
Background
With the rapid development of economy, the discharge amount of pollutants in industrial production is continuously increased, so that the heavy metal pollution problem is more and more serious, the environmental quality is influenced, and the human health is greatly damaged. Chromium is a common element in nature, the symbol of the element is Cr, and the common ionic valence is 0, +2, +3, + 6. Hexavalent chromium is a heavy metal with strong toxicity and can be produced in industrial production and manufacturing processes, particularly in industrial waste residues and wastewater. The discharge of hexavalent chromium causes serious pollution hazard to the ecological environment, the hexavalent chromium not only pollutes soil and water sources, but also has physiological toxicity and immunotoxicity and poses threat to human health, and the hexavalent chromium is classified as a first-grade carcinogen by the international agency for research on cancer (IARC). Therefore, the rapid detection technology of hexavalent chromium is an important research aspect in the related fields of environmental monitoring, food, tobacco and medicine detection and the like, and has practical significance for site detection of polluted environment, control of industrial pollution sources and protection of human health.
At present, the hexavalent chromium analysis methods mainly include ion chromatography, colorimetry, atomic absorption spectrophotometry, ICP-MS and the like, but the methods are complicated in operation, low in sensitivity, expensive in instrument price and difficult to popularize. Because various methods have different defects, the application range of the methods is limited, and therefore, a novel detection method which is simple to operate, high in sensitivity and low in cost needs to be developed. In recent years, a technology for detecting heavy metal ions by using fluorescent carbon dots attracts wide attention, and the method is convenient and rapid, generally has high selectivity and sensitivity, and becomes a great hotspot of current research.
Carbon Dots (CDs), an emerging member of the Carbon nanofamily, has attracted considerable attention from researchers since the first discovery by Xiaoyou Xu et al, university of south Carolina, 2004, and the first naming by Ya-Ping Sun, university of Cramerson, 2006. The grain diameter of the carbon dots is less than 10nm, and the carbon dots are a nano material with a carbon skeleton structure. The carbon dots are rich in functional groups such as carboxyl, hydroxyl, carboxyl and the like on the surface, so that the carbon dots have excellent water solubility and are easy to functionalize. The carbon dot also has the excellent characteristics of excitation wavelength dependence, high luminous efficiency, strong light tolerance, low biotoxicity and the like, and further widens the application range of the carbon dot in the fields of nano sensors, immunoassay, drug delivery, photoelectric devices, fluorescent probes, biological imaging, photocatalysis and the like.
Since the discovery of CDs, there have been a variety of manufacturing techniques, and depending on the manufacturing process, the manufacturing methods can be broadly divided into two broad categories: the Top-down (Top-down) and Bottom-up (Bottom-up) approaches. The Top-down approach means that CDs are formed or stripped in a larger carbon structure material, and comprises an electric arc cutting method, a laser ablation method and an electrochemical method, wherein the electric arc cutting method and the laser ablation method need to consume too much electric energy; the electrochemical method is one of the most traditional synthetic methods, a strong oxidant (strong base or acid) is required in the synthetic process, and the traditional synthetic method is not in accordance with the green chemical requirement and the sustainable development requirement in raw materials or synthetic technology because the excessive oxidant is difficult to completely remove and the environmental problem is increased. The Bottom-up approach is to finally obtain CDs through a series of reactions by using small molecular organic matters as precursors, such as glucose, sucrose, citric acid, amino acids, even food residues, and the like, and mainly includes a microwave-assisted method, a pyrolysis synthesis method, a hydrothermal synthesis method, and the like, wherein raw materials adopted in the methods are all organic compounds and biomass materials, and the Bottom-up approach is an important direction for developing a 'greener' method to synthesize the CDs.
Compared with the traditional fluorescent material, the carbon dots have potential application value due to excellent performances of good water solubility, stable fluorescence, low toxicity and the like, and can be widely applied to a plurality of fields such as chemical sensors, biological imaging, analysis and detection and the like, so that the carbon dots can be used as novel fluorescent probes. At present, carbon dots are reported in documents to detect heavy metal pollutants in wastewater, but the reports related to the use of the carbon dots in a fluorescent probe for detecting hexavalent chromium are less. Therefore, the sulfur-nitrogen co-doped yellow fluorescent carbon dot is prepared by a hydrothermal method, and the method has the characteristics of rapidness, simplicity, good selectivity and high sensitivity, and has certain research significance and potential application value.
Disclosure of Invention
In order to make up the defects of the prior art, the invention aims to provide a sulfur-nitrogen co-doped yellow fluorescent carbon dot and a preparation method thereof, wherein the carbon dot can be used for detecting Cr6+The application is as follows. The preparation method is simple, the needed raw materials are cheap and easy to obtain, the needed time is shorter than that of the traditional hydrothermal method, and the preparation method has strong controllability and is easy to realize batch production.
In order to achieve the purpose, the invention adopts the technical scheme that:
the first purpose of the invention is to provide a preparation method of a sulfur and nitrogen co-doped yellow fluorescent carbon dot, which comprises the following steps: and uniformly mixing o-phenylenediamine and lipoic acid in proportion, reacting in an oven at a high temperature for several hours, and centrifuging, filtering, dialyzing and freeze-drying reactants after the reaction is finished to obtain the carbon dots.
In order to further optimize the preparation method, the technical measures adopted by the invention also comprise the following steps:
further, the preparation method of the sulfur and nitrogen co-doped yellow fluorescent carbon dot comprises the following specific steps:
dissolving o-phenylenediamine and lipoic acid in deionized water, ultrasonically dissolving at room temperature to form a uniform mixed solution, putting the mixed solution into a polytetrafluoroethylene high-temperature reaction kettle, putting the polytetrafluoroethylene high-temperature reaction kettle into an oven for high-temperature carbonization reaction at the reaction temperature of 120-220 ℃, finishing the reaction for 2-12h, and obtaining a solution A after the reaction is finished;
secondly, putting the solution A obtained in the step one into a centrifugal tube, carrying out high-speed centrifugation for 3-5 times, removing impurities such as large-size particles at the bottom, and taking supernatant as solution B;
and thirdly, filling the solution B obtained in the step two into a dialysis bag, carrying out dialysis treatment for 3-4 days under the condition of aqueous solution, removing impurities which do not participate in carbonization reaction, and carrying out freeze drying to obtain a carbon dot solid, thereby obtaining the target product yellow fluorescent carbon dot.
Further, the molar ratio of the o-phenylenediamine to the lipoic acid in the first step is 1: 1 to 6.
Furthermore, in the first step, the ultrasonic power is 60-100W.
Further, in the first step, the reaction temperature is 200 ℃, and the reaction time is 6 hours.
Further, the volume of the polytetrafluoroethylene high-temperature reaction kettle in the first step is 50 mL.
Further, the centrifugation speed in the second step is 6000 r/min-12000 r/min.
Further, the dialysis bag in step three has a cut-off molecular weight of 10000D.
The sulfur-nitrogen co-doped yellow fluorescent carbon dot prepared by the method can detect Cr in an environmental water sample6+The use of (1). Can also be used for Cr in industrial wastewater6+Detection of (3).
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, o-phenylenediamine and lipoic acid (as C, N and S sources respectively) are mixed, a sulfur-nitrogen co-doped yellow fluorescent carbon dot is prepared by a simple one-step hydrothermal method, insoluble substances are centrifugally removed after reaction, macromolecular substances are removed by dialysis, and a solvent is removed by freeze-drying, so that the target product yellow fluorescent carbon dot is obtained. The carbon dots prepared by the method have uniform size and dispersibility, the synthesis method is simple, the raw materials are cheap and easy to obtain, the cost is low, the prepared product is nontoxic, has good fluorescence property and can treat environmental pollutants Cr6+Has the function of fluorescence detection. Has wide application prospect in environmental monitoring and management.
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FIG. 1 is a graph showing an ultraviolet absorption spectrum, a fluorescence excitation spectrum and a fluorescence emission spectrum of a fluorescent carbon dot prepared in example 1;
FIG. 2 is a Fourier infrared spectrum of the fluorescent carbon dots prepared in example 1;
FIG. 3 shows the selective detection of heavy metals by the fluorescent carbon dots prepared in example 1Data of experimental results, wherein, Ca2 +, Ni2+ ,Co2+ ,Cr3+ ,Cr6+, Cu2+, Fe2+,Fe3+, K+, Mg2+, Na+And Ag+The concentration is 100 MuM;
FIG. 4 shows the fluorescent carbon dots prepared in example 1 at different Cr concentrations6+(0-1000. mu.M) fluorescence spectrum in the presence of the compound.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
The first embodiment is as follows: the method for preparing the fluorescent carbon dot is characterized by comprising the following steps:
dissolving o-phenylenediamine and lipoic acid in deionized water, ultrasonically dissolving at room temperature to form a uniform mixed solution, putting the mixed solution into a polytetrafluoroethylene high-temperature reaction kettle, putting the polytetrafluoroethylene high-temperature reaction kettle into an oven for high-temperature carbonization reaction at the reaction temperature of 200 ℃, finishing the reaction for 6 hours, and obtaining a solution A after the reaction is finished;
secondly, putting the solution A obtained in the step one into a centrifugal tube, carrying out high-speed centrifugation for 3-5 times, removing impurities such as large-size particles at the bottom, and taking supernatant as solution B;
and thirdly, filling the solution B obtained in the step two into a dialysis bag, carrying out dialysis treatment for 3-4 days under the condition of aqueous solution, removing impurities which do not participate in carbonization reaction, and carrying out freeze drying to obtain a carbon dot solid, thereby obtaining the target product yellow fluorescent carbon dot.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: step one, the molar ratio of o-phenylenediamine to lipoic acid is 1: 1-6. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: in the first step, the ultrasonic power is 60-100W. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: in the first step, the reaction temperature is 120-220 ℃. The others are the same as in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and finishing the reaction for 2-12h in the step one. The other is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: and the centrifugation speed in the second step is 6000 r/min-12000 r/min. The other is the same as one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: and the centrifugation speed in the second step is 10000 r/min. The other is the same as one of the first to sixth embodiments.
The specific implementation mode is eight: the embodiment of the method for detecting Cr in the environmental water sample by using the fluorescent carbon dots6+The use of (1).
The following examples are given to illustrate the present invention, and the following examples are carried out on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
Example 1:
firstly, 0.1g of o-phenylenediamine and 0.038g of thioctic acid are weighed and dissolved in 10mL of deionized water, the mixture is dissolved under 100W ultrasound at room temperature to form a uniform mixed solution, the mixed solution is put into a 50mL of polytetrafluoroethylene high-temperature reaction kettle, and the mixture is put into a 200 ℃ oven to react for 6 hours, so that a yellow fluorescent carbon dot solution A is obtained.
And secondly, putting the solution obtained in the step one into a centrifugal tube, centrifuging for 3 times at a high speed of 10000r/min, removing impurities such as large-size particles at the bottom, and taking supernatant to obtain clear yellow fluorescent carbon dot solution B.
And thirdly, filling the solution obtained in the second step into a dialysis bag, carrying out dialysis treatment for 3 days in the dialysis bag with the molecular weight cut-off of 10000 under the condition of aqueous solution, removing impurities which do not participate in the carbonization reaction, and carrying out freeze drying to obtain the carbon dot solid with the detection function.
The ultraviolet absorption spectrum, fluorescence excitation spectrum and fluorescence emission spectrum of the fluorescent carbon dots prepared in this example are shown in fig. 1. The prepared fluorescent carbon dot has a large absorption area in an ultraviolet light area of 300nm-480nm, and the central absorption peak is 420 nm. The fluorescence excitation peak is 411nm, and the fluorescence emission peak is 565 nm.
The fluorescent carbon dots are in a yellow water solution state under natural illumination, and the fluorescent carbon dots show strong yellow fluorescence under 365 nm ultraviolet illumination.
Fig. 2 is a fourier infrared spectrum of a fluorescent carbon dot, and it can be seen that the prepared carbon dot contains C ═ C, C — N, C — O, N — H, and C — H.
FIG. 3 is a data chart showing the results of the selective detection experiment of heavy metals by using fluorescent carbon dots prepared in example 1, wherein Ca is present2 +, Ni2+ ,Co2+ ,Cr3+ ,Cr6+, Cu2+, Fe2+,Fe3+, K+, Mg2+, Na+And Ag+The concentration is 100 MuM; as shown in FIG. 3, the fluorescence intensity of the fluorescent carbon dots cannot be changed significantly by the common heavy metal ions, when the common heavy metal ions are combined with Cr6+When the effect is generated, the fluorescence intensity is obviously enhanced, which shows that the effect is on Cr6+Has selective detection performance and can realize the detection of Cr6+Selective detection of (2).
FIG. 4 shows the fluorescent carbon dots prepared in example 1 at different Cr concentrations6+(0-1000. mu.M) fluorescence spectrum in the presence of; with Cr6+The concentration is increased, the fluorescence intensity of the carbon dots is gradually enhanced, and Cr can be treated6+Intelligent detection of (2).
The fluorescent carbon dots prepared by the embodiment have better fluorescence intensity, and the fluorescence efficiency can reach 86%.
Example 2:
firstly, 0.1g of o-phenylenediamine and 0.047g of thioctic acid are weighed and dissolved in 10mL of deionized water, the mixture is dissolved under the ultrasonic condition of 80W at room temperature to form a uniform mixed solution, the mixed solution is put into a 50mL of polytetrafluoroethylene high-temperature reaction kettle, and the mixture is put into a 180 ℃ oven to react for 12 hours, so that the yellow fluorescent carbon dot solution A is obtained.
And secondly, putting the solution obtained in the step one into a centrifuge tube, centrifuging at a high speed of 12000r/min for 3 times, removing impurities such as large-size particles at the bottom, and taking supernatant liquid which is a clear yellow fluorescent carbon dot solution B.
And thirdly, filling the solution obtained in the second step into a dialysis bag, carrying out dialysis treatment for 3 days in the dialysis bag with the molecular weight cut-off of 10000 under the condition of aqueous solution, removing impurities which do not participate in the carbonization reaction, and carrying out freeze drying to obtain the carbon dot solid with the detection function.
Example 3:
firstly, 0.1g of o-phenylenediamine and 0.019g of thioctic acid are weighed and dissolved in 10mL of deionized water, the mixture is dissolved under the ultrasonic condition of 80W at room temperature to form a uniform mixed solution, the mixed solution is put into a 50mL of polytetrafluoroethylene high-temperature reaction kettle, and the mixture is put into a 120 ℃ oven to react for 10 hours, so that the yellow fluorescent carbon dot solution A is obtained.
And secondly, putting the solution obtained in the step one into a centrifuge tube, centrifuging at a high speed of 12000r/min for 3 times, removing impurities such as large-size particles at the bottom, and taking supernatant liquid which is a clear yellow fluorescent carbon dot solution B.
And thirdly, filling the solution obtained in the second step into a dialysis bag, carrying out dialysis treatment for 3 days in the dialysis bag with the molecular weight cut-off of 10000 under the condition of aqueous solution, removing impurities which do not participate in the carbonization reaction, and carrying out freeze drying to obtain the carbon dot solid with the detection function.
Example 4:
firstly, 0.1g of o-phenylenediamine and 0.006g of thioctic acid are weighed and dissolved in 10mL of deionized water, the mixture is dissolved under the ultrasonic condition of 80W at room temperature to form a uniform mixed solution, the mixed solution is put into a 50mL of polytetrafluoroethylene high-temperature reaction kettle, and the mixture is put into a 220 ℃ oven to react for 8 hours, so that a yellow fluorescent carbon dot solution A is obtained.
And secondly, putting the solution obtained in the step one into a centrifugal tube, centrifuging at a high speed of 8000r/min for 3 times, removing impurities such as large-size particles at the bottom, and taking supernatant to obtain clear yellow fluorescent carbon dot solution B.
And thirdly, filling the solution obtained in the second step into a dialysis bag, carrying out dialysis treatment for 3 days in the dialysis bag with the molecular weight cut-off of 10000 under the condition of aqueous solution, removing impurities which do not participate in the carbonization reaction, and carrying out freeze drying to obtain the carbon dot solid with the detection function.
Claims (9)
1. A preparation method of a sulfur-nitrogen co-doped yellow fluorescent carbon dot is characterized by comprising the following steps:
dissolving o-phenylenediamine and lipoic acid in deionized water, ultrasonically dissolving at room temperature to form a uniform mixed solution, putting the mixed solution into a polytetrafluoroethylene high-temperature reaction kettle, putting the polytetrafluoroethylene high-temperature reaction kettle into an oven for high-temperature carbonization, reacting at 120-220 ℃ for 2-12 hours, and obtaining a solution A after the reaction is finished;
secondly, putting the solution A obtained in the step one into a centrifugal tube, carrying out high-speed centrifugation for 3-5 times, removing impurities such as large-size particles at the bottom, and taking supernatant as solution B;
and thirdly, filling the solution B obtained in the step two into a dialysis bag, carrying out dialysis treatment for 3-4 days under the condition of aqueous solution, removing impurities which do not participate in carbonization reaction, and carrying out freeze drying to obtain a carbon dot solid, thereby obtaining the target product yellow fluorescent carbon dot.
2. The method for preparing the sulfur-nitrogen co-doped yellow fluorescent carbon dot according to claim 1, which is characterized in that: the molar ratio of the o-phenylenediamine to the lipoic acid is 1: 1 to 6.
3. The preparation method of the sulfur and nitrogen co-doped yellow fluorescent carbon dot according to claim 1, characterized in that: in the first step, the ultrasonic power is 60-100W.
4. The preparation method of the sulfur and nitrogen co-doped yellow fluorescent carbon dot according to claim 1, characterized in that: the reaction temperature in step one was 200 ℃.
5. The preparation method of the sulfur and nitrogen co-doped yellow fluorescent carbon dot according to claim 1, characterized in that: and finishing the reaction for 6h in the step one.
6. The preparation method of the sulfur and nitrogen co-doped yellow fluorescent carbon dot according to claim 1, characterized in that: the volume of the polytetrafluoroethylene high-temperature reaction kettle in the first step is 50 mL.
7. The preparation method of the sulfur and nitrogen co-doped yellow fluorescent carbon dot according to claim 1, characterized in that: and the centrifugation speed in the second step is 6000 r/min-12000 r/min.
8. The method for preparing the sulfur-nitrogen co-doped yellow fluorescent carbon dot as claimed in claim 1, wherein the method comprises the following steps: the dialysis bag in step three has a cut-off molecular weight of 10000D.
9. The sulfur and nitrogen co-doped yellow fluorescent carbon dot of claim 1 capable of being coated with Cr6+The method is applied to measurement.
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| CN114316962A (en) * | 2021-12-02 | 2022-04-12 | 山西大学 | N, S co-doped carbon dot, preparation method thereof and Cr-doped carbon dot6+Applications in assays |
| CN114316966A (en) * | 2021-12-30 | 2022-04-12 | 杭州电子科技大学 | Preparation method and application of nitrogen-sulfur co-doped three-wavelength fluorescent carbon dots |
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