CN111547704B - Method and device for preparing carbon quantum dots based on liquid phase pulse plasma effect - Google Patents

Method and device for preparing carbon quantum dots based on liquid phase pulse plasma effect Download PDF

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CN111547704B
CN111547704B CN202010374407.6A CN202010374407A CN111547704B CN 111547704 B CN111547704 B CN 111547704B CN 202010374407 A CN202010374407 A CN 202010374407A CN 111547704 B CN111547704 B CN 111547704B
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CN111547704A (en
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刘慧�
孙冰
沈雨涵
朱小梅
信延彬
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Dalian Maritime University
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    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/08Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in rotating vessels; Atomisation on rotating discs
    • B01D3/085Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in rotating vessels; Atomisation on rotating discs using a rotary evaporator
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
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    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
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    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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Abstract

The invention discloses a method and a device for preparing carbon quantum dots based on the action of liquid-phase pulsed plasma, wherein the method comprises the following steps: preparing an aqueous solution of urea and citric acid as a reaction solution, immersing two electrodes into the reaction solution, and electrifying the electrodes to generate plasma between the two electrodes to obtain a carbon quantum dot mixed solution; dialyzing the obtained carbon quantum dot mixed solution, and performing rotary evaporation and concentration to obtain a carbon quantum dot solution, and also comprises a device for preparing the carbon quantum dots by applying the method. The invention adopts the needle and plate electrodes, improves the discharge capacity, increases the area of plasma generation, has short reaction time and low energy consumption, and the process of preparing the carbon quantum dots is carried out in an aqueous solution system, thereby facilitating the subsequent purification.

Description

Method and device for preparing carbon quantum dots based on liquid phase pulse plasma effect
Technical Field
The invention relates to the field of carbon quantum dot preparation, in particular to a method and a device for preparing carbon quantum dots based on liquid phase pulse plasma action.
Background
Carbon quantum dots are a very popular novel nano material in recent years, have the advantages of unique luminescence (PL) property, good water solubility, low toxicity, light stability, good biocompatibility and the like, and have more and more extensive application in the fields of biological imaging, photocatalysis, chemical sensors, biosensors and the like.
In the traditional preparation method of the carbon quantum dots, the synthesis method can be divided into a Top-down synthesis method and a Bottom-up synthesis method according to carbon source substances required by synthesis. The Top-down (Top-down) synthesis method refers to the extraction of carbon quantum dot nanoparticles after stripping from carbon source macromolecular substances by a physical method, and the main methods are arc discharge, laser ablation and electrochemical synthesis. The "Bottom-up" synthesis method is just the opposite of the "Top-down" synthesis method, which uses carbon material in molecular or ionic state to form nano-particle material through chemical reaction polymerization, and the main methods are hydrothermal/solvothermal method, combustion method, chemical oxidation method and microwave synthesis method.
Among them, the arc method purifies arc discharge bituminous coal, then uses nitric acid and sodium hydroxide to process and obtain carbon quantum dots, the carbon quantum dots obtained by the method have good fluorescence, but the yield is low, the grain diameter is not uniform, and the method is not suitable for mass production; the laser ablation method is to dissolve the carbon nano material in a solvent and irradiate the solvent with laser, and supernatant liquor is the carbon quantum dots, and the method has uneven particle size distribution and high equipment requirement and is not suitable for industrial production; the electrochemical synthesis method uses the multi-arm carbon nano tube as an electrode material, and strips the carbon material through electrolysis to generate the carbon quantum dot solution, and the method has the advantages of simple operation, rich raw materials, large production potential, low cost and complicated purification process; the yield of carbon quantum dots generated by the chemical oxidation method is high, the particle size is uniform, the reaction conditions are mild, but the suitable reaction is less, and special equipment is needed; the combustion method comprises the steps of combusting organic matters, collecting products (carbon powder) after combustion, and oxidizing to obtain carbon quantum dots, wherein the obtained carbon quantum dots are low in yield and uneven in particle size; the microwave synthesis method is characterized in that carbon source substances are put into a microwave reactor to carry out microwave reaction to generate carbon quantum dots, and the microwave synthesis method has the advantages of no toxicity, simplicity, convenience, low cost and the like, but the size of synthesized particles is not easy to control; the hydrothermal/solvothermal method is the most common carbon quantum dot preparation method at present, the method is simple to manufacture, safe and efficient, no environmentally destructive substances are generated, and the prepared carbon source substances have many choices, but a long-time heating process is needed, so that the time consumption is long and the energy consumption is high. The carbon quantum dots can also be prepared by discharging in absolute ethyl alcohol, but the subsequent purification procedure is complicated by synthesizing the carbon quantum dots in an organic solvent system, so that a simple, rapid and environment-friendly method for preparing the carbon quantum dots is required to be found.
Disclosure of Invention
Aiming at the problems, the invention researches and designs a method and a device for preparing carbon quantum dots based on the action of liquid phase pulse plasmas to solve the problems of long time consumption and complex subsequent purification in the traditional method for preparing the carbon quantum dots. The technical means adopted by the invention are as follows:
a method for preparing carbon quantum dots based on liquid phase pulse plasma effect comprises the following steps:
s1, preparing an aqueous solution of urea and citric acid as a reaction solution, immersing two electrodes into the reaction solution, and electrifying the electrodes to generate plasma between the two electrodes to obtain a carbon quantum dot mixed solution;
and S2, dialyzing the obtained carbon quantum dot mixed solution, and performing rotary evaporation and concentration to obtain a carbon quantum dot solution.
Preferably, in step S1, the molar ratio of urea to citric acid in the reaction solution is (2-10): 1.
preferably, in step S1, the power supply is a high voltage pulse power supply, the voltage of which is 15 to 30kV, and the frequency of which is 30 to 40Hz.
Preferably, in step S1, the time of the discharge reaction is 8-30min.
Preferably, in step S1, the distance between the two electrodes is 3-8mm.
Preferably, in step S1, the two electrodes are respectively a plate electrode and a needle electrode, and the plate electrode and the needle electrode are made of stainless steel.
The device for preparing the carbon quantum dots by applying the method comprises a liquid-phase reaction chamber, a needle electrode, a plate electrode and a power supply, wherein reaction liquid is arranged in the liquid-phase reaction chamber, the needle electrode and the plate electrode are immersed in the reaction liquid, the needle electrode and the plate electrode are oppositely arranged, the needle electrode is connected with the power supply, the plate electrode is grounded, and when the power supply is electrified, plasma is formed by discharging between the needle electrode and the plate electrode.
Preferably, the liquid phase reaction chamber comprises a reaction chamber main body, a top plate and a bottom plate, the top plate and the bottom plate are respectively and fixedly connected with the top and the bottom of the reaction chamber main body, the top plate, the bottom plate and the reaction chamber main body are matched to form an accommodating space, a plate electrode fixing hole and a liquid changing hole are formed in the top plate, the plate electrode extends into the reaction chamber main body through the plate electrode fixing hole, a needle electrode fixing hole is formed in the bottom plate, and the needle electrode extends into the reaction chamber main body through the needle electrode fixing hole.
Preferably, the reaction chamber main body, the top plate and the bottom plate are all made of organic glass materials.
Compared with the prior art, the method and the device for preparing the carbon quantum dots based on the liquid phase pulse plasma effect have the following beneficial effects:
1. the invention adopts the needle and plate electrodes, improves the discharge capability, increases the area of plasma generation, has high reaction efficiency and shorter time consumption, does not need long-time high-temperature conditions and has lower energy consumption.
2. The process of preparing the carbon quantum dots is carried out in an aqueous solution system, and the subsequent purification is easier.
3. The device for preparing the carbon quantum dots has the advantages of simple structure, no need of a catalyst in the reaction process, no generation of toxic and harmful gases, and environmental friendliness.
Drawings
Fig. 1 is a schematic view of the overall structure of an apparatus for manufacturing carbon quantum dots in example 1 of the present invention.
FIG. 2a is a schematic view of the overall structure of a liquid phase reaction chamber in example 1 of the present invention.
Fig. 2b is a schematic structural view of the top plate in embodiment 1 of the present invention.
Fig. 2c is a schematic structural diagram of the base plate in embodiment 1 of the present invention.
Fig. 2d is a schematic side view of a plate electrode in embodiment 1 of the present invention.
FIG. 2e is a schematic side view of the main body of the reaction chamber in example 1 of the present invention.
FIG. 3 is a graph showing fluorescence intensity vs. wavelength distribution of the carbon quantum dot solution prepared in example 2 of the present invention at different excitation wavelengths.
Fig. 4 is a TEM image of the carbon quantum dot prepared in example 2 of the present invention.
Fig. 5 is a particle size distribution diagram of carbon quantum dots prepared in example 2 of the present invention.
FIG. 6 is a graph of the fluorescence intensity of carbon quantum dots prepared from urea and citric acid at different molar ratios in example 3 of the present invention at ex =340 nm.
Fig. 7 is a graph of the fluorescence intensity of ex =340nm for carbon quantum dots prepared from urea and citric acid at different voltage frequencies (i.e., different discharge modes) prepared in example 4 of the present invention.
In fig. 1 and fig. 2a-2e, 1, a liquid phase reaction chamber; 2. a needle electrode; 3. a plate electrode; 4. a power source; 5. a reaction chamber body; 6. a top plate; 7. a base plate; 8. a plate electrode fixing hole; 9. a needle electrode fixing hole; 10. and (4) liquid changing holes.
Detailed Description
Example 1:
as shown in fig. 1 and fig. 2a-2e, an apparatus for preparing carbon quantum dots based on liquid phase pulsed plasma effect comprises a liquid phase reaction chamber 1, a needle electrode 2, a plate electrode 3 and a power supply 4, wherein a reaction liquid is injected into the liquid phase reaction chamber 1, and the needle electrode 2 and the plate electrode 3 are both immersed into the reaction liquid. The electrodes are respectively set as a needle electrode 2 and a plate electrode 3, and the plate electrode 3 can increase the area of plasma generation and improve the reaction efficiency of the reaction liquid; the tip of the needle electrode 2 facilitates the generation of high energy, facilitating the generation of plasma.
The liquid phase reaction chamber 1 comprises a reaction chamber main body 5, and a top plate 6 and a bottom plate 7 which are matched and connected with the top and the bottom of the reaction chamber main body 5, wherein the reaction chamber main body 5, the top plate 6 and the bottom plate 7 are made of organic glass materials, and generally do not react with reactants, and the organic glass materials are insulating and high-temperature resistant and do not influence the preparation process of carbon quantum dots. The top plate 6 is provided with a plate electrode fixing hole 8 and a liquid changing hole 10, and the bottom plate 7 is provided with a needle electrode fixing hole 9. In this embodiment, two liquid change holes 10 are provided in the top plate 6, and the liquid change holes 10 can be used for adding the reaction liquid and taking out the reacted liquid, respectively, and can be used as vent holes at ordinary times. The plate electrode 3 extends into the reaction chamber main body 5 through the plate electrode fixing hole 8, the reaction chamber main body 5 is of a cylindrical structure, the main body of the plate electrode 3 is cylindrical, and the diameter of the plate electrode 3 is smaller than the inner diameter of the reaction chamber main body 5, so that the plate electrode 3 can be discharged in the reaction chamber main body 5 in a whole body, and solution is prevented from splashing. The needle electrode 2 extends into the reaction chamber main body 5 through the needle electrode fixing hole 9, the sealing between the needle electrode 2 and the needle electrode fixing hole 9 is good, and liquid leakage is avoided. The plate electrode 3 and the needle electrode 2 are oppositely arranged, the needle electrode 2 is arranged below the liquid phase reaction chamber 1 and is connected with the power supply 4, the plate electrode 3 is arranged above the liquid phase reaction chamber 1 and is connected with the ground wire, and plasma is formed by discharging between the needle electrode 3 and the plate electrode 2.
The power supply 4 is a high-voltage pulse power supply, the voltage of the high-voltage pulse power supply is 15-30 kV, and the frequency of the high-voltage pulse power supply is 30-40 Hz. Changing the discharge conditions can lead to different discharge forms (can be corona discharge or spark discharge), thereby regulating and controlling the appearance and the fluorescence characteristic of the carbon quantum dots.
The distance between the pin electrode 2 and the plate electrode 3 is 3-8mm, and the change of the electrode distance can influence the distribution of the electric field so as to influence the generation of plasma. The light-emitting characteristic of the carbon quantum dots can be adjusted and controlled in an auxiliary mode by adjusting the electrode distance, and the generation of plasma is not facilitated due to the overlarge electrode distance.
The needle electrode 2 and the plate electrode 3 are both made of stainless steel. The stainless steel material is not decomposed due to discharge, has small loss in high-voltage discharge, can discharge for multiple times, does not influence the fluorescence of the carbon quantum dot solution, and can cause the quenching effect of the carbon quantum dots due to other metal materials.
Example 2:
a method for preparing carbon quantum dots based on liquid phase pulse plasma effect comprises the following steps: urea, citric acid and pure water are made into a mixed solution, and the mixed solution is added into a liquid phase reaction chamber to enable the mixed solution to submerge a needle electrode and a plate electrode. And opening the high-voltage pulse power supply to generate liquid phase plasma at the needle electrode in the liquid phase reaction chamber, and reacting the citric acid and the urea under the action of the plasma to generate carbon quantum dots. After discharging for 10min, the power supply is turned off, and the solution in the liquid phase reaction chamber is taken out. And pouring the discharged solution into a 500D dialysis bag, carrying out dialysis purification treatment for 24h by using pure water, and carrying out water change once at 5 h. And adding the dialyzed solution into a rotary evaporator for concentration, and obtaining the carbon quantum dot solution after concentration.
Wherein, the purity of the raw material urea is more than or equal to 99 percent, and the urea is easy to dissolve in water, so that the content of nitrogen element in the carbon quantum dots can be increased, and the fluorescence effect is more obvious. The solvent is pure water, the solubility of urea in the pure water is high, the urea and the citric acid cannot react due to the stability of the aqueous solution, and the complexity of subsequent purification is reduced by using water as the solvent, so that the preparation process is more convenient. The discharge reaction time is 8-30min, in this embodiment, the discharge reaction time is 10min, and the morphology and the fluorescence characteristic of the prepared carbon quantum dots can be regulated and controlled according to the discharge time.
The fluorescence intensity of the carbon quantum dots obtained in the embodiment under different excitation wavelengths is shown in fig. 3, and it is found that the emission wavelength of the generated carbon quantum dots depends on the excitation wavelength, when ex =310nm, the em =400nm fluorescence intensity is strongest, and the emission wavelength is red-shifted to 450nm along with the red-shift of the excitation wavelength, so that the carbon quantum dots have the performance of tunable emission wavelength; the TEM image is shown in FIG. 4, and the carbon quantum dots are clearly seen to be spherical, have good dispersibility and uniform size; the particle size distribution is shown in FIG. 5, and the carbon quantum dot particle sizes are mainly concentrated in the range of 2-6 nm.
Example 3:
a method for preparing carbon quantum dots based on liquid phase pulse plasma effect comprises the following steps: taking molar concentration ratios of 2: 1. 4: 1. 6: 1. 8:1 and 10:1, preparing a mixed aqueous solution of urea and citric acid as a reaction solution, and adding a certain volume of the reaction solution into a liquid-phase reaction chamber to enable the reaction solution to submerge a needle electrode and a plate electrode. And turning on a high-voltage pulse power supply, setting the voltage to be 26kV and the frequency to be 30Hz, and generating liquid phase plasma at the needle electrode in the reactor. After discharging for 10min, the power supply is turned off, and the solution in the liquid phase reaction chamber is taken out. Pouring the discharged solution into a 500D dialysis bag, carrying out dialysis purification treatment for 24h by using pure water, and carrying out water change once at 5 h. And adding the dialyzed solution into a rotary evaporator for concentration, and obtaining the carbon quantum dot solution after concentration.
The fluorescence of the obtained carbon quantum dots is shown in fig. 6, and it can be seen that the liquid phase plasma promotes the formation of the carbon quantum dots in the range of the used concentration ratio.
Example 4:
a method for preparing carbon quantum dots based on liquid phase pulse plasma effect comprises the following steps: taking the molar ratio of 10:1, and adding a certain volume of mixed liquor into a discharge reactor to enable the mixed liquor to submerge a needle electrode and a plate electrode. And (3) turning on a high-voltage pulse power supply, and setting the voltage to be 26kV, the frequency to be 30Hz and the voltage to be 30kV and the frequency to be 40Hz to respectively discharge so as to generate liquid phase plasma at the needle electrode in the reactor. After discharging for 10min, the power supply was turned off and the solution in the reactor was taken out. Pouring the discharged solution into a 500D dialysis bag, carrying out dialysis purification treatment for 24h by using pure water, and carrying out water change once at 5 h. And adding the dialyzed solution into a rotary evaporator for concentration, and obtaining the carbon quantum dot solution after concentration.
The obtained carbon quantum dot fluorescence is shown in FIG. 7, when the discharge condition is 26kV and 30Hz and the electrode spacing is 5mm, the fluorescence of the generated carbon quantum dot is strong, and the central emission wavelength is at 420 nm; when the discharge condition is 30kV,40Hz and the electrode spacing is 3mm, the fluorescence of the generated carbon quantum dots is weakened, but the central emission wavelength is red-shifted to 440nm, which shows that the light-emitting characteristics of the carbon quantum dots can be controlled by controlling the discharge condition.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention made by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.

Claims (4)

1. A method for preparing carbon quantum dots based on liquid phase pulse plasma action is characterized in that: the method comprises the following steps:
s1, preparing an aqueous solution of urea and citric acid as a reaction solution, immersing two electrodes into the reaction solution, electrifying the electrodes to generate plasma between the two electrodes to obtain a carbon quantum dot mixed solution, wherein the two electrodes are respectively a plate electrode and a needle electrode, the distance between the two electrodes is 3-8mm, the electrifying power supply is a high-voltage pulse power supply, the voltage of the high-voltage pulse power supply is 26kV, and the frequency of the high-voltage pulse power supply is 30Hz;
and S2, dialyzing the obtained carbon quantum dot mixed solution, and performing rotary evaporation and concentration to obtain a carbon quantum dot solution.
2. The method for preparing the carbon quantum dots based on the liquid phase pulse plasma effect as claimed in claim 1, wherein: in step S1, the molar ratio of urea to citric acid in the reaction solution is (2-10): 1.
3. the method for preparing the carbon quantum dots based on the liquid phase pulse plasma effect as claimed in claim 1, wherein: in step S1, the time of the discharge reaction is 8-30min.
4. The method for preparing carbon quantum dots based on liquid phase pulsed plasma action according to any one of claims 1 to 3, wherein: in step S1, both the plate electrode and the pin electrode are made of stainless steel.
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