CN109337682B - Method for preparing fluorescent carbon quantum dots at room temperature - Google Patents
Method for preparing fluorescent carbon quantum dots at room temperature Download PDFInfo
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- CN109337682B CN109337682B CN201811601840.8A CN201811601840A CN109337682B CN 109337682 B CN109337682 B CN 109337682B CN 201811601840 A CN201811601840 A CN 201811601840A CN 109337682 B CN109337682 B CN 109337682B
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Abstract
The invention discloses a method for preparing fluorescent carbon quantum dots at room temperature, which comprises the following steps: mixing carbohydrate with organic solvent to obtain carbohydrate solution or suspension; dissolving inorganic base in water to prepare inorganic base solution; dropwise adding the solution or suspension of the carbohydrate into the inorganic alkali solution at room temperature, and violently stirring for 12 hours to obtain a reaction product mixed solution; and pouring the reaction product into a separating funnel, standing for 2 hours, and separating to remove water to obtain the fluorescent carbon quantum dots dispersed in the organic solvent. The method has the advantages of simple process, room-temperature reaction, mild reaction conditions, low energy consumption, good product dispersibility and high fluorescence efficiency of the prepared carbon quantum dots. The method realizes the simple and low-cost synthesis of the carbon quantum dots, and is favorable for the popularization and application of the carbon quantum dots.
Description
Technical Field
The invention relates to the field of carbon quantum dot synthesis, in particular to a method for preparing fluorescent carbon quantum dots at room temperature.
Background
The carbon quantum dot is a carbon-based zero-dimensional material with the particle size less than 10nm and photoluminescence property. The carbon quantum dots have the advantages of excellent optical properties, good water solubility, low toxicity, environmental friendliness, wide raw material source, low cost, good biocompatibility and the like. Therefore, the carbon quantum dots have important application prospects in the fields of dye-sensitized solar cells, light-emitting diodes, biological imaging, sensors and catalysis. Compared with the traditional quantum dots, the carbon quantum dots have higher application value in biotechnology and environment application due to the non-toxicity.
The synthesis methods of carbon quantum dots are mainly divided into two categories: the first type is to obtain carbon quantum dots from top to bottom, and mainly prepares the carbon quantum dots by large-particle carbon structures. Generally, such methods have relatively severe reaction conditions and long post-separation time, such as electrochemical oxidation, plasma discharge, laser ablation, and the like. The second method is to obtain carbon quantum dots from bottom to top. The carbon quantum dots prepared by using the molecules containing carbon elements as the carbon source can generally control the size and the shape of the prepared nano carbon, but the preparation steps are relatively complex.
At present, most of the prepared water-soluble carbon quantum dots are water-soluble carbon quantum dots, and most of the preparation methods have low yield, complex operation and expensive equipment, so that the method has important value on promoting wide application by simply, economically and efficiently synthesizing and dispersing the water-soluble carbon quantum dots in an organic solvent.
Disclosure of Invention
Based on the problems of the prior art, the present invention aims to provide a method for preparing fluorescent carbon quantum dots at room temperature, which can prepare fluorescent carbon quantum dots dispersed in an organic solvent with relative simplicity and low cost.
The purpose of the invention is realized by the following technical scheme:
the embodiment of the invention provides a method for preparing carbon quantum dots at room temperature, which comprises the following steps:
mixing carbohydrate with organic solvent to obtain carbohydrate solution or suspension;
dissolving inorganic base in water to prepare inorganic base solution;
dropwise adding the solution or suspension of the carbohydrate into the inorganic alkali solution at room temperature, and violently stirring for 12 hours to obtain a reaction product mixed solution;
and pouring the reaction product into a separating funnel, standing for 2 hours, and separating to remove water to obtain the fluorescent carbon quantum dots dispersed in the organic solvent.
According to the technical scheme provided by the invention, the embodiment of the invention provides the method for preparing the fluorescent carbon quantum dots at room temperature, and the method has the following beneficial effects:
the method has the advantages of simple process, room-temperature reaction, mild reaction conditions, low energy consumption, good product dispersibility and high fluorescence efficiency of the prepared carbon quantum dots. The fluorescent carbon quantum dots dispersed in the organic solvent are synthesized simply and at low cost, and the popularization and application of the carbon quantum dots are facilitated.
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 fluorescence spectrum of a fluorescent carbon quantum dot prepared in example 1 of the present invention;
FIG. 2 is a high resolution TEM image of the fluorescent carbon quantum dots prepared in example 2 of the present invention;
fig. 3 is a high-resolution transmission electron microscope image of the fluorescent carbon quantum dot prepared in example 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the specific contents 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. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art.
The embodiment of the invention provides a method for preparing fluorescent carbon quantum dots at room temperature, which can be used for preparing carbon quantum dots dispersed in various solvents and comprises the following steps:
mixing carbohydrate with organic solvent to obtain carbohydrate solution or suspension;
dissolving inorganic base in water to prepare inorganic base solution;
adding the solution or suspension of carbohydrate into inorganic alkali solution at room temperature, and stirring vigorously for 12 hours to obtain a reaction product mixed solution;
and pouring the reaction product into a separating funnel, standing for 2 hours, and separating to remove water to obtain the fluorescent carbon quantum dots dispersed in the organic solvent.
The method comprises the step of dropwise adding a carbohydrate solution or suspension into an inorganic alkali solution at room temperature, wherein the mass ratio of the carbohydrate to the inorganic alkali is 1: 200-10: 1.
In the above method, the carbohydrate is at least one of sucrose, glucose, fructose and starch; in the method, the used organic solvent adopts at least one of toluene, xylene, benzene, chloroform, dichloromethane, petroleum ether and tetrahydrofuran;
the concentration of the inorganic alkali solution is 6-0.1 mol/L, and the used inorganic alkali is at least one of sodium hydroxide, potassium hydroxide and calcium hydroxide.
The particle size of the fluorescent carbon quantum dot prepared by the method is 3-10 nm.
The embodiments of the present invention are described in further detail below.
The method for preparing the fluorescent carbon quantum dots at room temperature comprises the steps of dropwise adding an organic solution or suspension of carbohydrate into an inorganic alkali solution (the mass ratio of the carbohydrate to the inorganic alkali is 1: 200-10: 1), and violently stirring for 12 hours; the concentration of the inorganic alkali solution is 6-0.1 mol/L; and pouring the obtained reactant into a separating funnel, standing for 2 hours, separating and removing water to obtain the fluorescent carbon quantum dots dispersed in the organic solvent, wherein the particle size of the prepared fluorescent carbon quantum dots is 3-10 nm.
In the above method, the carbohydrate used in the carbohydrate solution or suspension includes, but is not limited to, sucrose, glucose, fructose, starch. The organic solvent is at least one of toluene, xylene, benzene, chloroform, dichloromethane, petroleum ether and tetrahydrofuran;
inorganic bases used in the inorganic base solution include, but are not limited to, sodium hydroxide, potassium hydroxide, calcium hydroxide.
The preparation method provided by the embodiment of the invention has the advantages of simple process, mild reaction conditions, low energy consumption and good product dispersibility, and is beneficial to large-scale preparation of carbon quantum dots dispersed in various solvents.
Example 1
The embodiment provides a method for preparing fluorescent carbon quantum dots at room temperature, which comprises the following steps:
weighing 1.8g of glucose, and adding the glucose into 50ml of toluene to prepare toluene suspension of the glucose;
weighing 8g of sodium hydroxide, and adding the sodium hydroxide into 100ml of water to prepare an inorganic alkali solution;
dripping the glucose toluene suspension into an inorganic alkaline solution under the condition, and violently stirring for 12 hours to obtain a reaction product mixed solution;
and then pouring the reaction product into a separating funnel, standing for 2 hours, and separating and removing water to obtain carbon quantum dots dispersed in toluene, wherein the particle size of the carbon quantum dots is 3-10 nm.
The fluorescence spectrum of the fluorescent carbon quantum dot prepared in example 1 is shown in fig. 1, and it can be seen from the fluorescence spectrum that the fluorescent carbon quantum dot has high fluorescence efficiency.
Example 2
The embodiment provides a method for preparing fluorescent carbon quantum dots at room temperature, which comprises the following steps:
weighing 1g of fructose, and adding the fructose into 100ml of tetrahydrofuran to prepare a tetrahydrofuran solution of the fructose;
weighing 10g of potassium hydroxide, and adding the potassium hydroxide into 100ml of water to prepare an inorganic alkali solution;
dripping a tetrahydrofuran solution of fructose into an inorganic alkali solution, and violently stirring for 12 hours to obtain a reaction product mixed solution;
and then pouring the reaction product into a separating funnel, standing for 2 hours, and separating and removing water to obtain carbon quantum dots dispersed in tetrahydrofuran, wherein the particle size of the carbon quantum dots is 3-10 nm.
The high-resolution transmission electron microscope image of the fluorescent carbon quantum dot prepared in this example 2 is shown in fig. 2, and it can be seen from the image that the dispersibility of the fluorescent carbon quantum dot is good.
Example 3
The embodiment provides a method for preparing fluorescent carbon quantum dots at room temperature, which comprises the following steps:
weighing 10g of sucrose, adding into 100ml of xylene, and preparing into xylene suspension of sucrose;
weighing 3g of calcium hydroxide, and adding the calcium hydroxide into 100ml of water to prepare inorganic alkali solution;
adding the xylene suspension of sucrose into the calcium hydroxide solution dropwise under the condition, and stirring vigorously for 12 hours to obtain a reaction product mixed solution;
and then pouring the reaction product into a separating funnel, standing for 2 hours, and separating to remove water to obtain the fluorescent carbon quantum dots dispersed in the xylene, wherein the particle size of the fluorescent carbon quantum dots is 5-10 nm.
The high-resolution transmission electron microscope image of the fluorescent carbon quantum dot prepared in this example 3 is shown in fig. 3, and it can be seen from the image that the dispersibility of the carbon quantum dot is good.
The above description is only for the 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 included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (2)
1. A method for preparing fluorescent carbon quantum dots at room temperature is characterized by comprising the following steps:
mixing carbohydrate with organic solvent to obtain carbohydrate solution or suspension; the carbohydrate is at least one of sucrose, glucose, fructose and starch; the organic solvent is at least one of toluene, xylene, benzene, chloroform, dichloromethane, petroleum ether and tetrahydrofuran;
dissolving inorganic base in water to prepare inorganic base solution; the preparation method of the inorganic alkali solution comprises the following steps: weighing 10g of potassium hydroxide, and adding the potassium hydroxide into 100ml of water to prepare an inorganic alkali solution; or weighing 10g of potassium hydroxide, and adding 100ml of water to prepare inorganic alkali solution; or weighing 3g of calcium hydroxide, and adding into 100ml of water to prepare inorganic alkali solution;
dropwise adding the solution or suspension of the carbohydrate into the inorganic base solution at room temperature, wherein the mass ratio of the carbohydrate to the inorganic base is 10:1, stirring vigorously for 12 hours to obtain a reaction product mixed solution;
and pouring the reaction product into a separating funnel, standing for 2 hours, and separating to remove water to obtain the fluorescent carbon quantum dots dispersed in the organic solvent.
2. The method for preparing the fluorescent carbon quantum dots at room temperature according to claim 1, wherein the particle size of the prepared fluorescent carbon quantum dots is 3-10 nm.
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| CN104386666B (en) * | 2014-10-22 | 2017-01-11 | 纪效波 | Method for preparing carbon quantum dots through alcohol decomposition |
| CN104528684B (en) * | 2014-12-10 | 2016-08-17 | 中南大学 | A kind of method that under the conditions of alkalescence, carbon quantum dot is prepared in ketone carbonization |
| CN104591129A (en) * | 2015-01-12 | 2015-05-06 | 四川大学 | Method for preparing hydrophobic carbon quantum dots on large scale under ambient temperature condition |
| CN107619034B (en) * | 2017-10-16 | 2018-06-29 | 赵方浩 | The preparation method of green fluorescence carbon quantum dot |
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