CN113025314B - Simple method for rapidly preparing sulfur quantum dots - Google Patents
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Abstract
The invention discloses a simple method for rapidly preparing sulfur quantum dots, which adopts pulse laser to irradiate a sodium dodecyl sulfate aqueous solution so as to prepare the sulfur quantum dots. The method has the advantages of short reaction time, capability of quickly preparing the sulfur quantum dots with good water dispersibility and stability, less varieties of required raw materials, simple preparation steps, mild reaction conditions, low preparation cost, environmental friendliness and high efficiency.
Description
Technical Field
The invention relates to the technical field of sulfur quantum dot preparation, in particular to a simple method for quickly preparing sulfur quantum dots.
Background
The quantum dots generally have quantum size effect, excellent magnetism and good photoelectric property, and are widely applied in the fields of biomarkers, antibacterial drugs, light emitting diodes, displays and the like. However, quantum dots containing heavy metals have limited their application due to their potential toxicity and their environmental hazards. Therefore, in recent years, researchers have been working on finding nontoxic or heavy metal-free quantum dots, especially some pure element quantum dots such as carbon quantum dots, silicon quantum dots, phosphorus quantum dots, sulfur quantum dots, and the like. Among the reported pure element quantum dots, sulfur quantum dots are receiving more and more attention due to their unique fluorescence characteristics, good water dispersibility, stability, luminescence characteristics, low toxicity, excellent chemical properties and good biological activity. A large number of documents prove that the sulfur quantum dots are widely applied to the fields of sensing, cell imaging, photocatalysis, light-emitting diodes, polymer nano composite materials, antibiosis and the like.
At present, the preparation methods of the sulfur quantum dots mainly comprise two methods: one is acid etching oxidation of metal sulfides, and the other is separation of sulfur quantum dots from sublimed sulfur. In 2014, sulfur quantum dots are successfully reported to be synthesized by taking CdS quantum dots as raw materials through an acid etching oxidation method for the first time; the synthesis mainly comprises 3 steps: physical contact, oil-water phase interface reaction and in-situ precipitation dissolution, wherein the reaction time is 36 hours; the size of the sulfur quantum dot synthesized by the method is about 1.6nm, and the sulfur quantum dot has excellent water dispersibility and obvious fluorescence characteristic; however, the method has the disadvantages of harsh reaction conditions, complex operation, high cost and the like, which limits the preparation and application of the method. No significant research progress was made in the direction of sulfur quantum dots for the next 4 years. Until 2018, there have been reported methods of separating sulfur quantum dots from sublimed sulfur; the separation of the sulfur quantum dots from the sublimed sulfur is actually an assembly and fission of the sublimed sulfur; using massive sublimed sulfur as a raw material, and performing three steps of dissolution, assembly and fission to obtain a product, wherein polyethylene glycol (PEG) is used as a stabilizer to prevent sulfur quantum dots from aggregating into large particles in the process; the size of the sulfur quantum dots is related to the reaction time, and 125 hours are required to obtain the sulfur quantum dots with the target size. From 2018 to the present, most of reported novel synthetic methods of sulfur quantum dots are improved on the basis of the method. It has been reported that the reaction is accelerated and the reaction time is reduced by using the high temperature and high pressure conditions created by the hydrothermal method, but at least 4 hours are required to complete the reaction. Currently, most synthetic methods use sublimed sulfur, naOH and PEG as raw materials to prepare sulfur quantum dots; in this type of synthesis, the major elemental sulfur is converted to polysulfides, sulfonates and sulfates rather than sulfur quantum dots. The reported sulfur quantum dot preparation method generally has the problems of long reaction time, harsh reaction conditions, complex operation process, higher cost and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a simple method for rapidly preparing the sulfur quantum dots, which has the advantages of short reaction time, capability of rapidly preparing the sulfur quantum dots with good water dispersibility and stability, less varieties of required raw materials, simple preparation steps, mild reaction conditions, low preparation cost, environmental protection and high efficiency.
The purpose of the invention is realized by the following technical scheme:
a simple method for rapidly preparing sulfur quantum dots comprises the following steps: and irradiating the lauryl sodium sulfate aqueous solution by adopting pulse laser to prepare the sulfur quantum dots.
Preferably, the wavelength of the pulse laser is 355nm, 532nm or 1064nm, the energy of the pulse laser is 50-500 mJ, and the frequency of the pulse laser is 5-50 Hz.
Preferably, the pulsed laser is used to irradiate the aqueous solution of sodium dodecyl sulfate at room temperature.
Preferably, the aqueous sodium lauryl sulfate solution is stirred during irradiation of the aqueous sodium lauryl sulfate solution with the pulsed laser.
Preferably, the stirring speed of the stirring is 50 to 1500rpm.
Preferably, the average particle size of the sulfur quantum dots is 1.87nm.
According to the technical scheme provided by the invention, the simple method for rapidly preparing the sulfur quantum dots adopts sodium dodecyl sulfate (SDS: C) 12 H 25 SO 4 Na) is used as a reaction source, and the SDS absorbs the high-temperature metastable condition generated by energy when the laser acts on the SDS in water, so that the SDS is subjected to in-situ thermal decomposition and nucleation to form elemental sulfur, meanwhile, the heat of nucleation points is effectively dispersed in the presence of a liquid phase environment, the elemental sulfur is prevented from further curing and growing, and finally, sulfur quantum dots with the average size of 1.87nm are formed. Because the raw material is only the sodium dodecyl sulfate aqueous solution, the required raw material variety is less, and the preparation cost of the sulfur quantum dots is low; the preparation steps are simple because the reaction conditions are only laser irradiation; meanwhile, the solvent water under stirring dissipates heat generated in the reaction process rapidly, so that the whole reaction can be carried out at room temperature, and the danger caused by high temperature, strong alkali and the like is effectively avoided. The invention expands the application of liquid-phase laser processing in the preparation technology in the aspect of material synthesis on one hand, and provides a new idea and basis for the deep research of the preparation and application of the sulfur quantum dots on the other hand.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a schematic diagram illustrating a principle of a simple method for rapidly preparing sulfur quantum dots according to embodiment 1 of the present invention.
FIG. 2 is an XRD pattern of the sulfur quantum dots prepared in example 1 of the present invention.
FIG. 3 is a TEM image of the sulfur quantum dots prepared in example 1 of the present invention.
FIG. 4 is a fluorescence emission spectrum of the sulfur quantum dot prepared in example 1 of the present invention at an excitation wavelength of 360 nm.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The simple method for rapidly preparing the sulfur quantum dots provided by the present invention is described in detail below. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to a person skilled in the art.
A simple method for rapidly preparing sulfur quantum dots is characterized in that pulsed laser is adopted to irradiate a sodium dodecyl sulfate aqueous solution at room temperature, and the sodium dodecyl sulfate aqueous solution is stirred in the irradiation process, so that Sulfur Quantum Dots (SQDs) with the average particle size of 1.87nm are prepared.
Wherein, the wavelength of the pulse laser can be 1064nm or 355nm, but is preferably 532nm; the energy of the pulse laser may be 50 to 500mJ, but is preferably 120mJ, and the frequency of the pulse laser is preferably 5 to 50Hz.
Specifically, the sodium dodecyl sulfate aqueous solution with any concentration can be used for preparing sulfur quantum dots after being irradiated by pulse laser, and only the number of the sulfur quantum dots is different from the size of the sulfur quantum dots, that is, the number of the prepared sulfur quantum dots and the size of the sulfur quantum dots can be changed by adjusting the concentration of the sodium dodecyl sulfate aqueous solution; in practical application, the concentration of the sodium dodecyl sulfate aqueous solution can be 0.01mol/L. The sulfur quantum dots can be prepared by irradiating the sodium dodecyl sulfate aqueous solution by adopting the pulse laser at any time, only the number of the sulfur quantum dots is different from the size of the sulfur quantum dots, namely, the number of the prepared sulfur quantum dots and the size of the sulfur quantum dots can be changed by adjusting the irradiation time of the pulse laser to the sodium dodecyl sulfate aqueous solution; in practical application, the irradiation time of the pulsed laser to the sodium dodecyl sulfate aqueous solution may be 30 minutes. The stirring speed for stirring the aqueous solution of sodium lauryl sulfate during irradiation is preferably 50 to 1500rpm, which allows the aqueous solution to more effectively disperse the heat generated during the reaction.
Further, sodium dodecyl sulfate (SDS: C) 12 H 25 SO 4 Na) is easily dissolved in water, has low price and is environment-friendly, and the decomposition temperature is only 200 ℃. The method utilizes the characteristics of the sodium dodecyl sulfate, takes the aqueous solution of the sodium dodecyl sulfate as a source material, adopts laser to directly irradiate the aqueous solution of the sodium dodecyl sulfate, and automatically decomposes the aqueous solution of the sodium dodecyl sulfate into a sulfur simple substance through the heat generated by the absorption of SDS to light, and finally obtains a sulfur quantum dot (with the average particle size of 1.87 nm) with good water dispersibility and stability. In the process, no other chemical reagent is needed to be added, the requirement on the amount of raw materials is avoided, the operation is simple, the reaction time is short, the reaction condition is mild, the cost is low, and the method is green and efficient. SDS molecules in a liquid phase environment uniformly absorb laser with proper wavelength to form an independent high-temperature metastable reaction system, and the SDS molecules are automatically decomposed into elemental sulfur along with the accumulation of photo-thermal energy. Meanwhile, the existence of the solvent water in a stirring state in the system effectively disperses the heat generated in the reaction process and avoids further curing and growth of the elemental sulfur. Fluorescence spectrum analysis shows that the sulfur quantum dot can show fluorescence characteristics at 510nm under the excitation of 360nm wavelength, and is expected to show different potentials in the fields of electricity, optics and biology. The method not only provides a new way and thought for the preparation and application of the sulfur quantum dots, but also expands the new application of the liquid-phase laser processing and preparation technology.
In conclusion, the method provided by the embodiment of the invention has the advantages of short reaction time, capability of quickly preparing the sulfur quantum dots with good water dispersibility and stability, less raw material types, simple preparation steps, mild reaction conditions, low preparation cost, environmental friendliness and high efficiency.
In order to more clearly show the technical solutions and the technical effects provided by the present invention, the following detailed description is provided with specific examples of a simple method for rapidly preparing sulfur quantum dots provided by the embodiments of the present invention.
Example 1
As shown in fig. 1, a simple method for rapidly preparing sulfur quantum dots comprises the following steps: preparing 0.01mol/L sodium dodecyl sulfate aqueous solution (namely SDS aqueous solution) as a raw material, taking 20mL of the SDS aqueous solution, filling the SDS aqueous solution into a 25mL glass bottle, stirring the SDS aqueous solution in the glass bottle by using a magnetic stirrer at the stirring speed of 50-1500 rpm, then continuously irradiating the SDS aqueous solution in the glass bottle at room temperature by using ultraviolet pulse laser under a laser with the ultraviolet band wavelength of 532nm, the energy of 120mJ and the frequency of 20Hz, and only continuously irradiating for 30min to obtain the sulfur quantum dots with the average particle size of 1.87nm.
Specifically, the preparation process of embodiment 1 of the invention has the advantages of short reaction time, capability of being carried out at room temperature, low cost, simple process and environmental protection, and the subsequent storage can be carried out only by covering the glass bottle with a bottle cap and placing the bottle cap indoors.
Further, the following analysis and detection were performed on the sulfur quantum dots prepared in example 1 of the present invention:
(1) In order to determine the phase of the product of example 1, the sulfur quantum dots prepared in example 1 were subjected to X-ray diffraction (XRD) analysis, so that an XRD pattern as shown in fig. 2 could be obtained. As can be seen from fig. 2: the sulfur quantum dots and S prepared in example 1 of the present invention 8 The standard card JCPDS NO.74-1465 characteristic diffraction peaks of the sulfur quantum dots of the structure are matched.
(2) The sulfur quantum dots prepared in example 1 of the present invention were observed with a transmission electron microscope, so that a transmission electron microscope photograph (TEM photograph) as shown in fig. 3 was obtained; wherein, fig. 3a is the high resolution lattice spacing of the sulfur quantum dots prepared in example 1 of the present invention at a scale of 2nm, fig. 3b is the TEM morphology and size distribution of the sulfur quantum dots prepared in example 1 of the present invention at a scale of 20nm, and fig. 3c is the TEM morphology of the sulfur quantum dots prepared in example 1 of the present invention at a scale of 10 nm. As can be seen from fig. 3: the sulfur quantum dots prepared in the embodiment 1 of the invention are in the form of quantum dots with the average particle size of 1.87nm, and are uniform in size; analyzing the high-resolution crystal lattice, and measuring that the interplanar spacing is 0.21nm and corresponds to a (353) plane of a sulfur quantum dot; this also shows that the sulfur quantum dot obtained in example 1 of the present invention is expected to exhibit specific properties in the optical, biological fields, and the like.
(3) The fluorescence characteristics of the sulfur quantum dots prepared in example 1 of the present invention were investigated, and it was found that when the excitation wavelength was 360nm, a significant fluorescence characteristic was observed around 510nm, and the fluorescence emission spectrum of the sulfur quantum dots prepared in example 1 of the present invention at the excitation wavelength of 360nm is shown in fig. 4.
In conclusion, the embodiment of the invention has the advantages of short reaction time, capability of quickly preparing the sulfur quantum dots with good water dispersibility and stability, less raw material types, simple preparation steps, mild reaction conditions, low preparation cost, environmental protection and high efficiency.
The above description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (3)
1. A simple method for rapidly preparing sulfur quantum dots is characterized by comprising the following steps: irradiating the lauryl sodium sulfate aqueous solution by adopting pulse laser to prepare sulfur quantum dots;
the wavelength of the pulse laser is 532nm, the energy of the pulse laser is 50-500 mJ, and the frequency of the pulse laser is 5-50 Hz;
irradiating the sodium dodecyl sulfate aqueous solution by adopting pulse laser at room temperature;
stirring the lauryl sodium sulfate aqueous solution in the irradiation process of the lauryl sodium sulfate aqueous solution by adopting pulse laser.
2. The simple method for rapidly preparing the sulfur quantum dots according to claim 1, wherein the stirring speed of the stirring is 50-1500 rpm.
3. The simple method for rapidly preparing sulfur quantum dots according to claim 1, wherein the average particle size of the sulfur quantum dots is 1.87nm.
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| CN113480998B (en) * | 2021-08-19 | 2023-03-21 | 河南师范大学 | Preparation method based on bottom-up fluorescent sulfur quantum dots |
| CN115044368B (en) * | 2022-06-22 | 2023-10-13 | 成都理工大学 | Method for synthesizing sulfur quantum dots by photocatalytic oxidation |
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