CN109988570A - A kind of preparation facilities and preparation method of carbon quantum dot - Google Patents
A kind of preparation facilities and preparation method of carbon quantum dot Download PDFInfo
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- CN109988570A CN109988570A CN201910080621.8A CN201910080621A CN109988570A CN 109988570 A CN109988570 A CN 109988570A CN 201910080621 A CN201910080621 A CN 201910080621A CN 109988570 A CN109988570 A CN 109988570A
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- quantum dot
- carbon quantum
- dehydrated alcohol
- power supply
- conductive pins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
Abstract
The present invention relates to a kind of preparation facilities of carbon quantum dot and preparation methods, comprising: discharge container, dehydrated alcohol, two conductive pins and power supply；Dehydrated alcohol is set in discharge container；Two conductive pins are respectively placed in dehydrated alcohol, and wherein a conductive pin connects to power supply, another conductive pin external ground；Wherein, power supply, so that generating plasma between two conductive pins, is discharged when being powered to conductive pin with puncturing dehydrated alcohol.The present invention prepares carbon quantum dot while hydrogen from ethanol reforming, and device is simple, and equipment requirement is low, reacts without catalyst, reaction condition is simple.In addition, dehydrated alcohol is electrolysed by conductive pin, hydrogen and carbon quantum dot are made simultaneously, the carbon quantum dot of generation can play photocatalysis to the electrolysis of dehydrated alcohol again, the yield of hydrogen and carbon quantum dot is improved, positive feedback is formed, kills two birds with one stone, time cost and financial resources is greatly saved, improves the utilization rate of ethyl alcohol and the energy.
Description
Technical field
The present invention relates to carbon quantum dot preparation technical fields, preparation facilities and preparation more particularly to a kind of carbon quantum dot
Method.
Background technique
Carbon quantum dot is a kind of novel carbon-based zero dimension material.Carbon quantum dot has outstanding optical property, good water
Dissolubility, hypotoxicity, environmental-friendly, raw material sources are wide, at low cost, good biocompatibility, chemical property stablize many advantages, such as, answer
With extensive, the field of many such as medical imaging technology, environmental monitoring, chemical analysis, catalyst preparation, energy development have compared with
Good application prospect.Since carbon quantum dot by since finding for the first time, it has been developed that many synthetic methods, including arc discharge
Method, laser corrode method, electrochemical synthesis, chemical oxidization method, combustion method, hydrothermal synthesis method, microwave process for synthesizing, template etc..
But requirement height, cumbersome, cost of manufacture height of the current carbon quantum dot preparation method to equipment.
One kind due to Hydrogen Energy as new energy, due to having many advantages, such as combustion heat value height, no pollution to the environment, by people
Great attention, but various hydrogen from ethanol reforming methods be also it is single be used to manufacture hydrogen, byproduct is mostly carbon oxygen
Compound (such as to the harmful carbon monoxide of hydrogen utilization), hydrocarbon, carbon distribution etc., ethyl alcohol cannot be fully utilized,
Carbon distribution can also pollute and block the ethyl alcohol circulatory system and gas gathering system simultaneously.
Summary of the invention
The present invention provides the preparation facilities and preparation method of a kind of carbon quantum dot, to solve carbon quantum dot in the prior art
The high problem of preparation cost.
The technical scheme to solve the above technical problems is that a kind of preparation facilities of carbon quantum dot, comprising: electric discharge
Container, dehydrated alcohol, two conductive pins and power supply；
The dehydrated alcohol is set in the discharge container；
Two conductive pins are respectively placed in the dehydrated alcohol, and wherein a conductive pin and the power supply connect
It connects, another conductive pin external ground；
Wherein, the power supply to the conductive pin when being powered, so that plasma is generated between two conductive pins,
It is discharged with puncturing the dehydrated alcohol.
The beneficial effects of the present invention are: the present invention is from green, economy, the angle of sustainable development, in ethanol reformation
Carbon quantum dot is prepared while hydrogen manufacturing, device is simple, and equipment requirement is low, reacts without catalyst, reaction condition is simple.In addition,
It is electrolysed dehydrated alcohol by conductive pin, while obtained hydrogen and carbon quantum dot, the carbon quantum dot of generation again can be to dehydrated alcohols
Photocatalysis is played in electrolysis, improves the yield of hydrogen and carbon quantum dot, is formed positive feedback, is killed two birds with one stone, when being greatly saved
Between cost and financial resources, improve the utilization rate of ethyl alcohol and the energy.
Based on the above technical solution, the present invention can also be improved as follows.
Further, the power supply is AC power source, DC power supply or the pulse power.
Further beneficial effect of the invention is: as long as power supply enables to it when being powered to conductive pin between conductive pin
Electric discharge, therefore, the device are suitable for multiple power sources, have a wide range of application.
Further, the angle between two conductive pins is 0~180 degree.
Further beneficial effect of the invention is: the angle between two conductive pins can be any angle, device installation
Simply, structure is simple.
Further, the syringe needle spacing of electric discharge one end of two conductive pins is 0~5mm.
Further beneficial effect of the invention is: the spacing between two conductive pins can be any spacing, in order to improve
Discharge effect and energy consumption is reduced, the spacing between two conductive pins should not be too far.It preferably can be 0.6mm.
Further, two conductive pins are independently are as follows: stainless pin or tungsten needle.
Further beneficial effect of the invention is: due to the good conductivity of stainless pin and tungsten needle, reducing the energy consumption of power supply.
Further, the discharge container is quartz container.
Further beneficial effect of the invention is: not reacting with ethyl alcohol and its product and the appearance for the high pressure resistant high temperature that insulate
Device is preferred.
It further, further include oscillograph；
The oscillograph is connect with two conductive pins respectively.
Further beneficial effect of the invention is: whether oscillograph discharges and puts for detecting to have between two conductive pins
The mode of electricity, convenient for according to actual needs, angle and spacing between two conductive pins of adjustment supply frequency, amplitude or adjustment are tied
Structure is simple, facilitates experiment, and user experience is strong.
The present invention also provides a kind of carbon quantum dot preparation methods based on preparation facilities as described above, comprising:
Build the preparation facilities of carbon quantum dot as described above；
The switch of the power supply is opened, the power supply is powered to the conductive pin connected to it, two conductive pins
Between generate plasma, the plasma punctures the dehydrated alcohol, and the dehydrated alcohol, which decomposes, generates hydrogen and carbon amounts
Sub- point.
The beneficial effects of the present invention are: the present invention is from green, economy, the angle of sustainable development, in ethanol reformation
Carbon quantum dot is prepared while hydrogen manufacturing, device is simple, and equipment requirement is low, and it is simple to build operating process.By being electrolysed dehydrated alcohol,
Hydrogen and carbon quantum dot, the carbon quantum dot of generation are made simultaneously can play photocatalysis to the electrolysis of dehydrated alcohol again, improve
The yield of hydrogen and carbon quantum dot forms positive feedback, kills two birds with one stone, is greatly saved time cost and financial resources, improve ethyl alcohol with
And the utilization rate of the energy.
Further, the oscillograph detects the discharge mode generated between two conductive pins and exports display.
Further beneficial effect of the invention is: whether oscillograph discharges and puts for detecting to have between two conductive pins
The mode of electricity, convenient for according to actual needs, angle and spacing between two conductive pins of adjustment supply frequency, amplitude or adjustment are tied
Structure is simple, facilitates experiment, and user experience is strong.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the preparation facilities of carbon quantum dot provided by one embodiment of the present invention；
Fig. 2 is a kind of structural schematic diagram of the preparation facilities for carbon quantum dot that another embodiment of the present invention provides；
Fig. 3 is a kind of flow diagram of the preparation method of carbon quantum dot provided by one embodiment of the present invention；
Fig. 4 is a kind of flow diagram of the preparation method for carbon quantum dot that another embodiment of the present invention provides；
Fig. 5 is the electric discharge phenomena figure for the conductive needle-discharging that another embodiment of the present invention provides；
Fig. 6 is the conductive pin discharge voltage current waveform figure that another embodiment of the present invention provides；
Fig. 7 is a kind of carbon quantum dot for carbon quantum dot preparation method preparation that another embodiment of the present invention provides not
With the fluorescence intensity emitted under excitation wavelength with the distribution map of wavelength；
Fig. 8 is that a kind of carbon quantum dot for carbon quantum dot preparation method preparation that another embodiment of the present invention provides is transmiting
The TEM and grain size distribution measured under electron microscope；
Fig. 9 is that a kind of light of the carbon quantum dot for carbon quantum dot preparation method preparation that another embodiment of the present invention provides is inhaled
Receive curve.
In attached drawing, element representated by each label is listed as follows:
1, discharge container, 2, dehydrated alcohol, 3, conductive pin, 4, power supply, 5, oscillograph.
Specific embodiment
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
Embodiment one
A kind of preparation facilities 100 of carbon quantum dot, as shown in Figure 1, comprising: discharge container 1, dehydrated alcohol 2, two conductions
Needle 3 and power supply 4；
The dehydrated alcohol is set in the discharge container；
Two conductive pins are respectively placed in the dehydrated alcohol, and wherein a conductive pin and the power supply connect
It connects, another conductive pin external ground；
Wherein, the power supply to the conductive pin when being powered, so that plasma is generated between two conductive pins,
It is discharged with puncturing the dehydrated alcohol.
For example, wherein one end of every conductive pin is contacted with dehydrated alcohol, wherein the other end and high pressure of a conductive pin
The high-pressure stage of AC power source connects, wherein the other end ground connection of another conductive pin.By the frequency and electricity that adjust AC power source
Pressure amplitude value discharges to dehydrated alcohol liquid, and dehydrated alcohol, which can be decomposed, generates hydrogen, while the carbon in dehydrated alcohol then can
Carbon quantum dot is aggregated under the action of plasma.
In the existing device for preparing hydrogen, reactant is generally ethanol water or alcohol vapour, when for alcohol vapour
When, catalyst and heating condition are needed, complicated condition needed for reacting.In addition, in the existing device for preparing hydrogen, two conductive electricity
Structure is complicated for pole, for example, it is desired to which conductive pin and needle plate collocation constitute electrode etc..
And the present embodiment prepares carbon while hydrogen from ethanol reforming from green, economy, the angle of sustainable development
Quantum dot, device is simple, and equipment requirement is low, reacts without catalyst, reaction condition is simple.In addition, being electrolysed nothing by conductive pin
Water-ethanol, while hydrogen and carbon quantum dot is made, the carbon quantum dot of generation can play photocatalysis work to the electrolysis of dehydrated alcohol again
With, the yield of hydrogen and carbon quantum dot is improved, positive feedback is formed, kills two birds with one stone, time cost and financial resources is greatly saved, raising
The utilization rate of ethyl alcohol and the energy.
In addition, it is necessary to which explanation, can observe by the naked eye the methods of electric spark and judge whether put between two conductive pins
Electricity, it is simple and convenient.
Preferably, power supply is AC power source, DC power supply or the pulse power.
As long as power supply enables to it to generate plasma between conductive pin when being powered to conductive pin and discharge, because
This, which is suitable for multiple power sources, has a wide range of application.
Preferably, the angle between two conductive pins is 0~180 degree.
Since two electrode angles can produce the discharge mode within the scope of 0~180 degree, so wide adaptation range, device
Simple to install, structure are simple.
Preferably, the spacing of electric discharge one end of two conductive pins is 0~5mm.
Spacing between two conductive pins can be any spacing, in order to improve discharge effect and reduce energy consumption, two
Spacing between conductive pin should not be too far.It is further preferably 0.6mm.
Preferably, two conductive pins are independently are as follows: stainless pin or tungsten needle.
Due to the good conductivity of stainless pin and tungsten needle, the energy consumption of power supply is reduced.The gold of other good conductivities can also be used
Belong to.
Preferably, discharge container is quartz container.
It does not react with ethyl alcohol and its product and the container for the high pressure resistant high temperature that insulate is preferred.
Preferably, as shown in Fig. 2, device 100 further includes oscillograph 5, oscillograph is connect with two conductive pins respectively.
Oscillograph is for the mode for whether having electric discharge and electric discharge between two conductive pins to be detected, convenient for according to practical need
It wants, the angle and spacing, simple structure between two conductive pins of adjustment supply frequency, amplitude or adjustment facilitate experiment, user experience
Sense is strong.
It should be noted that the level height between two conductive pins can be different, to realize better discharge effect.
Embodiment two
A kind of carbon quantum dot preparation method 200 based on any preparation facilities described in embodiment one, such as Fig. 3 and Fig. 4
It is shown, comprising:
Step 210, the preparation facilities for building any carbon quantum dot described in embodiment one as above；
Step 220, the switch for opening power supply, power supply are powered to conductive pin connected to it；
Step 230, the frequency and amplitude for adjusting power supply, so that generating plasma, plasma between two conductive pins
Puncture dehydrated alcohol, dehydrated alcohol, which decomposes, generates hydrogen and carbon quantum dot.
The present embodiment prepares carbon amounts while hydrogen from ethanol reforming from green, economy, the angle of sustainable development
Sub-, device is simple, and equipment requirement is low, and it is simple to build operating process.By being electrolysed dehydrated alcohol, while hydrogen and carbon amounts is made
Sub-, the carbon quantum dot of generation can play photocatalysis to the electrolysis of dehydrated alcohol again, improve the production of hydrogen and carbon quantum dot
Amount forms positive feedback, kills two birds with one stone, and time cost and financial resources is greatly saved, and improves the utilization rate of ethyl alcohol and the energy.
Preferably, oscillograph detects the discharge mode generated between two conductive pins and exports display.
Oscillograph is for the mode for whether having electric discharge and electric discharge between two conductive pins to be detected, convenient for according to practical need
It wants, the angle and spacing, simple structure between two conductive pins of adjustment supply frequency, amplitude or adjustment facilitate experiment, user experience
Sense is strong.
For example, using the AC power source of 40KHZ, discharge mode is needle-needle-discharging (i.e. discharging between two conductive pins), two
Electrode angle is set as 60 degree, and discharge container uses quartz container, built with dehydrated alcohol liquid, between two electrode needle points
Away from for 0.6mm.
Power supply is gradually adjusted to increase the alternating voltage between the two poles of the earth, when voltage magnitude is 17KV, between two conductive pins
Disruptive discharge is generated, is visually observed as spark discharge shown in fig. 5, oscillograph detects the discharge mode between two conductive pins, such as
Shown in Fig. 6, known by observation oscilloscope waveform, every half period has multiple pulses electric discharge.
Two conductive pin angles are successively changed to 180 degree, 120 degree, 30 degree again, supply frequency is all made of 40KHZ, these three angles
It spends lower device and generates above-mentioned discharge mode as shown in FIG. 6 when voltage magnitude is added to 29KV, 23KV, 15KV respectively, at electrode
Hydrogen is generated, and after a period of time of discharging, can detecte carbon quantum dot generation.
As shown in fig. 7, distribution of the fluorescence intensity that carbon quantum dot emits under different excitation wavelengths with wavelength, wherein every
The corresponding number of curve represents excitation wavelength.What the carbon quantum dot emitted under the ultraviolet excitation of 320nm as seen from the figure is glimmering
Luminous intensity is most strong, and fluorescence intensity can all weaken when excitation wavelength is larger or smaller, this is the fluorescence of typical carbon quantum dot
Spectral characteristic.
Further, as shown in figure 8, being carried out carbon quantum dot it has been observed that using the present embodiment using transmission electron microscope
The size of the carbon quantum dot that the method obtains, single carbon quantum dot is lower than 10nm.In addition the distribution of its diameter is provided, shows it
Diameter is located at 3nm between 1~5nm, diameter peak value.
In addition, the carbon quantum dot to generation carries out light absorption test, as shown in Figure 9, it is known that carbon quantum dot is less than wavelength
The ultraviolet light of 350nm has stronger absorption, and with the increase of wavelength, absorption intensity gradually weakens.
It should be noted that discharge mode is that every half period once put by pulsed discharge or the lesser pulse of multiple amplitude
When electric, carbon quantum dot generation is had.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation facilities of carbon quantum dot characterized by comprising discharge container, dehydrated alcohol, two conductive pins, with
And power supply；
The dehydrated alcohol is set in the discharge container；
Two conductive pins are respectively placed in the dehydrated alcohol, and wherein a conductive pin is connect with the power supply,
Another conductive pin external ground；
Wherein, the power supply to the conductive pin when being powered, so that plasma is generated between two conductive pins, to hit
It wears the dehydrated alcohol and discharges.
2. the preparation facilities of carbon quantum dot according to claim 1, which is characterized in that the power supply is AC power source, directly
Galvanic electricity source or the pulse power.
3. a kind of preparation facilities of carbon quantum dot according to claim 1, which is characterized in that between two conductive pins
Angle be 0~180 degree.
4. a kind of preparation facilities of carbon quantum dot according to claim 1, which is characterized in that two conductive pins are put
The syringe needle spacing of electric one end is 0~5mm.
5. a kind of preparation facilities of carbon quantum dot according to claim 1, which is characterized in that two conductive pins difference
It is independently: stainless pin or tungsten needle.
6. a kind of preparation facilities of carbon quantum dot according to claim 1, which is characterized in that the discharge container is quartz
Glass container.
7. a kind of preparation facilities of carbon quantum dot according to any one of claims 1 to 6, which is characterized in that further include showing
Wave device；
The oscillograph is connect with two conductive pins respectively.
8. a kind of carbon quantum dot preparation method based on the described in any item preparation facilities of claim 1 to 7, which is characterized in that
Include:
Build the preparation facilities of carbon quantum dot as described in any one of claim 1 to 7；
The switch of the power supply is opened, the power supply is powered to the conductive pin connected to it；
The frequency and amplitude of the power supply are adjusted, so that generating plasma, the plasma between two conductive pins
Puncture the dehydrated alcohol, the dehydrated alcohol, which decomposes, generates hydrogen and carbon quantum dot.
9. a kind of carbon quantum dot preparation method according to claim 8, which is characterized in that the oscillograph detection described two
The discharge mode that generates between root conductive pin simultaneously exports display.
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| CN201910080621.8A CN109988570B (en) | 2019-01-28 | 2019-01-28 | Hydrogen production device and method for producing carbon quantum dots while preparing hydrogen |
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| CN201910080621.8A CN109988570B (en) | 2019-01-28 | 2019-01-28 | Hydrogen production device and method for producing carbon quantum dots while preparing hydrogen |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111547704A (en) * | 2020-05-06 | 2020-08-18 | 大连海事大学 | Method and device for preparing carbon quantum dots based on liquid phase pulse plasma effect |
| CN113462384A (en) * | 2021-07-02 | 2021-10-01 | 西安交通大学 | Method for preparing fluorescent carbon quantum dots by gas-liquid two-phase plasma technology |
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| CN106270836A (en) * | 2016-09-05 | 2017-01-04 | 常州大学 | Spark discharge prepares the method for fluorescent carbon quantum dot |
| CN107254309A (en) * | 2017-07-01 | 2017-10-17 | 中国科学院兰州化学物理研究所 | A kind of preparation method of carbon quantum dot |
| CN108085711A (en) * | 2017-12-21 | 2018-05-29 | 西安科技大学 | A kind of preparation method of the carbon quantum dot to glow |
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2019
- 2019-01-28 CN CN201910080621.8A patent/CN109988570B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102942170A (en) * | 2012-10-22 | 2013-02-27 | 上海交通大学 | Preparation method of carbon quantum dots based on atmospheric pressure micro-plasma technology |
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| CN106270836A (en) * | 2016-09-05 | 2017-01-04 | 常州大学 | Spark discharge prepares the method for fluorescent carbon quantum dot |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111547704A (en) * | 2020-05-06 | 2020-08-18 | 大连海事大学 | Method and device for preparing carbon quantum dots based on liquid phase pulse plasma effect |
| CN111547704B (en) * | 2020-05-06 | 2022-11-01 | 大连海事大学 | Method and device for preparing carbon quantum dots based on liquid phase pulse plasma effect |
| CN113462384A (en) * | 2021-07-02 | 2021-10-01 | 西安交通大学 | Method for preparing fluorescent carbon quantum dots by gas-liquid two-phase plasma technology |
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