CN108128767A - A kind of method and its application that carbon quantum dot is quickly prepared in room temperature environment - Google Patents
A kind of method and its application that carbon quantum dot is quickly prepared in room temperature environment Download PDFInfo
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- CN108128767A CN108128767A CN201810004273.1A CN201810004273A CN108128767A CN 108128767 A CN108128767 A CN 108128767A CN 201810004273 A CN201810004273 A CN 201810004273A CN 108128767 A CN108128767 A CN 108128767A
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Abstract
The present invention relates to a kind of method and its application that carbon quantum dot is quickly prepared in room temperature environment.The technical solution adopted is that:Ethylenediamine is added in organic acid or inorganic acid, at room temperature, after very exothermic reaction, obtains solid crude product;Solid crude product is cooled to room temperature, and be dissolved in distilled water, is dialysed;By the solution after dialysis, concentrated by rotary evaporation, freeze-drying obtains pure carbon quantum dot powder.The method that the present invention prepares carbon dots is simple, and quickly, the uniform particle sizes of carbon dots, fluorescence property is good, has very high quantum yield.
Description
Technical field
The invention belongs to organic fluorescence field of nanometer material technology, and in particular to a kind of side that carbon dots are quickly prepared in room temperature environment
Method and its application.
Background technology
Fluorescent carbon point is a kind of new material in carbon nanomaterial.Due to its excellent optics, chemistry and biological property, draw
The extensive concern of people is played.Compared with traditional fluorescence semiconductor quantum dots and heavy metal are as main luminescent device, carbon
Point has the advantages that green syt and biocompatibility.Carbon dots are commonly used for biological field, including bio-imaging, biosensor
Etc..It, can be from various carbon sources using various environmentally sound physics and chemical method (including even some useless carbon sources)
Prepare a large amount of carbon dots.Therefore, carbon dots are considered as a kind of ideal nano material, meet the principle of Green Chemistry, maximum
Its application performance is improved to limit, reduces its adverse effect.Due to its extensive use in applied technical field, there is difference
Various preparation methods under technology path are closed including laser irradiation, hydrothermal synthesis, electrochemical etching, ultrasonic wave and microwave radiation technology
Into etc..Although these methods are simple and quick, complicated experimental provision makes which create high energy consumption, and such as relatively high temperature supplies
It should.The most ideal method for preparing carbon dots is synthesis at room temperature and need not additional energy supply.In this kind of method, chemical oxidation
Method is most common method, but there is requirement in relatively low quantum yield (QY < 5%) and reaction process to use a large amount of strong acid for it
And highly basic, it is difficult to remove extra oxidant completely so as to cause environmental problem after reaction.Therefore, exploitation it is a kind of simple, it is quick,
It is green, energy saving, suitable for large-scale production room temperature carbon dots method it is still very necessary.
Invention content
In order to solve the problems in the prior art, the purpose of the present invention is to provide one kind simply, fast, green is energy saving, is applicable in
In carbon dots uniform particle sizes prepared by the preparation method of the carbon dots of large-scale production, the present invention, fluorescence property is good, available for preparing
The materials such as fluorescence organic glass.
To achieve these goals, the technical solution adopted by the present invention is:One kind quickly prepares carbon quantum in room temperature environment
The method of point, includes the following steps:
1) ethylenediamine is added in organic acid or inorganic acid, at room temperature, by system from heat release, very exothermic is reacted
Afterwards, solid crude product is obtained;
2) solid crude product is cooled to room temperature, and be dissolved in distilled water, dialysed;
3) by the solution after dialysis, concentrated by rotary evaporation is freeze-dried, obtains pure carbon quantum dot powder.
A kind of above-mentioned method for quickly preparing carbon quantum dot in room temperature environment, in mass ratio, ethylenediamine:Organic acid or nothing
Machine acid=1:1.
A kind of above-mentioned method for quickly preparing carbon quantum dot in room temperature environment, the organic acid is acrylic acid, ice vinegar
Acid, trifluoroacetic acid and formic acid.Preferably, the organic acid is acrylic acid.It is furthermore preferred that in mass ratio, ethylenediamine:Acrylic acid
=1:1.5.
A kind of above-mentioned method for quickly preparing carbon quantum dot in room temperature environment, the inorganic acid for phosphoric acid, sulfuric acid and
Hydrofluoric acid.
A kind of above-mentioned method for quickly preparing carbon quantum dot in room temperature environment, in step 2), bag filter used of dialysing
Molecular cut off be 100.
In order to change the fluorescence color of carbon dots, other substances can also be adulterated in carbon dots, above-mentioned one kind is in room temperature ring
The method that border quickly prepares carbon quantum dot, in step 1), after first ethylenediamine is mixed with doping carbon source again with organic acid or inorganic
Acid reaction.Preferably, the doping carbon source is o-phenylenediamine, m-phenylene diamine (MPD) and p-phenylenediamine.
Application of the carbon quantum dot prepared according to above-mentioned method in fluorescence organic glass or phosphor-coated light emitting diode is prepared.
Carbon dots prepared by the method according to the invention:Ethylenediamine is reacted with acrylic acid, after dialysis, can obtain pure yellowish
Color carbon dots.Sulfuric acid is blue-fluorescence with carbon dots prepared by ethylenediamine.Phosphoric acid and ethylenediamine, glacial acetic acid and ethylenediamine, hydrofluoric acid with
Dark green fluorescence is presented in carbon dots prepared by ethylenediamine, trifluoroacetic acid and ethylenediamine, formic acid and ethylenediamine.
The beneficial effects of the invention are as follows:The present invention is by system from heat release, you can generation carbon dots.The method letter of the present invention
Single, fast, green is energy saving, suitable for mass producing novel carbon dots.The preparation method of the present invention is simple for process, easily operated,
It without any equipment, can react at room temperature, and suitable for several kinds of carbon source, be highly susceptible to promoting.Carbon dots prepared by the present invention
Uniform particle sizes, fluorescence property is good, available for preparing the materials such as fluorescence organic glass, phosphor-coated light emitting diode.The present invention prepare third
Olefin(e) acid carbon dots even particle size, average grain diameter are about 4nm.Photoluminescent property is good, has stronger blue-fluorescence, quantum yield
Up to 25%.
Description of the drawings
Fig. 1 is the high-resolution-ration transmission electric-lens figure of carbon dots prepared by embodiment 1.
Fig. 2 is the grain size distribution of carbon dots prepared by embodiment 1.
Fig. 3 is the ultraviolet and fluorogram of carbon dots prepared by embodiment 1.
Fig. 4 is the fluorogram for the carbon dots that 3 trifluoroacetic acid of embodiment is prepared with ethylenediamine.
Fig. 5 is the fluorogram for the carbon dots that 3 phosphoric acid of embodiment is prepared with ethylenediamine.
Fig. 6 is the fluorogram for the carbon dots that 3 sulfuric acid of embodiment is prepared with ethylenediamine.
Fig. 7 is the fluorogram for the carbon dots that 3 hydrofluoric acid of embodiment is prepared with ethylenediamine.
Fig. 8 is the fluorogram for the carbon dots that 3 glacial acetic acid of embodiment is prepared with ethylenediamine.
Fig. 9 is the fluorogram for the carbon dots that 3 formic acid of embodiment is prepared with ethylenediamine.
Figure 10 is the fluorogram that 4 m-phenylene diamine (MPD) of embodiment adulterates the carbon dots that acrylic acid is prepared with ethylenediamine.
Specific embodiment
The present invention is further described below by way of non-limiting example.
1 ethylenediamine of embodiment is reacted with acrylic acid prepares carbon dots
6mL ethylenediamines are added in the beaker of 14mL acrylic acid.After very exothermic reaction, you can obtain orange red carbon dots
Solid.Room temperature is cooled to, is dissolved in 20mL distilled water, dialysis (molecular cut off of bag filter is 100) one day.After dialysing
Solution, concentrated by rotary evaporation, freeze-drying, you can obtain pure faint yellow carbon dots.
The formation of carbon dots is the electron microscope confirmation by them, and Fig. 1 shows a typical high-resolution-ration transmission electric-lens
(HRTEM) to prepared carbon dots image.As can be seen that carbon dots have good monodispersity.Fig. 2 shows its size distribution
For range from 2 nanometers to 5 nanometer, average diameter is about 4nm.
Fig. 3 is the photo of the ultraviolet and fluorogram and carbon dots of carbon dots in the UV lamp, due to the π-π of carbon dots*Transformation,
Occurs very wide ultraviolet-ray visible absorbing band on uv-spectrogram, it is found that from fluorogram, the excitation wavelength of sample is 320
There is Red Shift Phenomena in variation between 420nm, corresponding fluorescence emission peak, from 400nm red shifts to 470nm, illustrate amination
Carbon dots and the essence of other most of carbon dots be identical, there is dependence between fluorescent emission and excitation wavelength, this
May be due to its grain size of the carbon dots prepared by this method or being unevenly distributed for emission sites and caused by.
2 ethylenediamine of embodiment reacts the optimal proportion for preparing carbon dots with acrylic acid
It is respectively 1 that acrylic acid and the common 2mL of ethylenediamine, ratio are added in the beaker of 10ml:9,2:8,3:7,4:6,5:5,
6:4,7:3,8:2 and 9:1.At room temperature, after very exothermic reaction, you can obtain orange red carbon dots solid.Room temperature is cooled to, is dissolved
In 2mL distilled water, its fluorescence intensity curves is surveyed, determines maximum excitation wavelength and best launch wavelength, calculates fluorescent quantum production
Rate compares carbon dots performance with this.
Table 1 illustrates the production of carbon dots under different ratio, from table 1, it can be seen that increases with the ratio of ethylenediamine
Greatly, maximum excitation wavelength is gradually moved into 360nm from 340nm, and the best launch wavelength of carbon dots maintains 412nm or so always.
From table 1, it is evident that first plus acrylic acid adds ethylenediamine again, and the higher carbon dots of quantum yield can be made.
Table 1
Serial number | Ratio (ethylenediamine:Acrylic acid v:v) | Excitation wavelength nm | Launch wavelength nm | Quantum yield % |
1 | 1:9 | 340 | 394 | 1.945 |
2 | 2:8 | 350 | 414 | 12.450 |
3 | 3:7 | 345 | 416 | 24.798 |
4 | 4:6 | 345 | 416 | 25.017 |
5 | 5:5 | 345 | 411 | 14.447 |
6 | 6:4 | 360 | 418 | 10.504 |
7 | 7:3 | 360 | 418 | 0.234 |
8 | 8:2 | / | / | 0 |
9 | 9:1 | / | / | 0 |
Embodiment 3 replaces other carbon sources and prepares carbon dots
1mL trifluoroacetic acids, phosphoric acid, sulfuric acid, hydrofluoric acid, glacial acetic acid and formic acid are added in 1mL ethylenediamines respectively, room temperature
Under, after very exothermic reaction, you can obtain carbon dots solid.Room temperature is cooled to, is dissolved in 2mL distilled water, dialysis be (bag filter
Molecular cut off is 100) one day.By the solution after dialysis, concentrated by rotary evaporation, freeze-drying, you can obtain pure carbon dots.
The color under carbon dots ultraviolet light is observed, detects the fluorescence property of carbon dots, as shown in figures 4-9.From fig. 4, it can be seen that trifluoro
The carbon dots that acetic acid is prepared with ethylenediamine show dark green fluorescence, a length of 380nm of optimum excitation wave, the position of best emission peak
474nm.As seen from Figure 5, the carbon dots that prepared by phosphoric acid and ethylenediamine show dark green fluorescence, a length of 380nm of optimum excitation wave, most
The position 477nm of good emission peak.As seen from Figure 6, the fluorescence that the carbon dots that sulfuric acid is prepared with ethylenediamine are displayed in blue, optimum excitation wave
A length of 360nm, the position 430nm of best emission peak.As seen from Figure 7, hydrofluoric acid shows dark green with carbon dots prepared by ethylenediamine
Fluorescence, a length of 380nm of optimum excitation wave, the position 465nm of best emission peak.As seen from Figure 8, glacial acetic acid is prepared with ethylenediamine
Carbon dots show dark green fluorescence, a length of 380nm of optimum excitation wave, the position 463nm of best emission peak.As seen from Figure 9, first
The carbon dots that acid is prepared with ethylenediamine show dark green fluorescence, a length of 380nm of optimum excitation wave, the position of best emission peak
468nm。
Embodiment 4 adulterates other substances
O-phenylenediamine, m-phenylene diamine (MPD) and p-phenylenediamine as carbon source, are often many heterocyclic compounds of production and polymer
Important presoma, the present embodiment select m-phenylene diamine (MPD) as doping carbon source.1g m-phenylene diamine (MPD)s are added in 1mL ethylenediamines, make
It after it is completely dissolved, pours into 1.5mL acrylic acid, after very exothermic reaction, you can obtain carbon dots solid.Room temperature is cooled to, it is molten
Solution is in 2mL distilled water, dialysis (molecular cut off of bag filter is 100) one day.By the solution after dialysis, concentrated by rotary evaporation is cold
It is lyophilized dry, you can obtain pure carbon dots.
As seen from Figure 10, after adding in m-phenylene diamine (MPD), the fluorescence color of carbon dots becomes green from blue.
Claims (10)
- A kind of 1. method for quickly preparing carbon quantum dot in room temperature environment, it is characterised in that include the following steps:1) ethylenediamine is added in organic acid or inorganic acid, at room temperature, after very exothermic reaction, obtains solid crude product;2) solid crude product is cooled to room temperature, and be dissolved in distilled water, dialysed;3) by the solution after dialysis, concentrated by rotary evaporation is freeze-dried, obtains pure carbon quantum dot powder.
- 2. a kind of method for quickly preparing carbon quantum dot in room temperature environment according to claim 1, it is characterised in that:Press body Product ratio, ethylenediamine:Organic acid or inorganic acid=1:1.
- 3. a kind of method for quickly preparing carbon quantum dot in room temperature environment according to claim 1, it is characterised in that:It is described Organic acid be acrylic acid, glacial acetic acid, trifluoroacetic acid and formic acid.
- 4. a kind of method for quickly preparing carbon quantum dot in room temperature environment according to claim 3, it is characterised in that:It is described Organic acid be acrylic acid.
- 5. a kind of method for quickly preparing carbon quantum dot in room temperature environment according to claim 4, it is characterised in that:Press body Product ratio, ethylenediamine:Acrylic acid=1:1.5.
- 6. a kind of method for quickly preparing carbon quantum dot in room temperature environment according to claim 1, it is characterised in that:It is described Inorganic acid be phosphoric acid, sulfuric acid and hydrofluoric acid.
- 7. a kind of method for quickly preparing carbon quantum dot in room temperature environment according to claim 1, it is characterised in that:Step 2) in, the molecular cut off for bag filter used of dialysing is 100.
- 8. a kind of method for quickly preparing carbon quantum dot in room temperature environment according to claim 1, it is characterised in that:Step 1) in, first by ethylenediamine with doping carbon source mix after again with organic acid or inorganic acid reaction.
- 9. a kind of method for quickly preparing carbon quantum dot in room temperature environment according to claim 8, it is characterised in that:It is described Doping carbon source be o-phenylenediamine, m-phenylene diamine (MPD) and p-phenylenediamine.
- 10. the carbon quantum dot prepared according to the method for claim 1 is in fluorescence organic glass or phosphor-coated light emitting diode is prepared Application.
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Cited By (12)
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CN109336086A (en) * | 2018-11-30 | 2019-02-15 | 郑州大学 | A kind of method of quick large scale preparation solid state fluorescence carbon dots |
CN109486485A (en) * | 2018-11-27 | 2019-03-19 | 合肥工业大学 | A method of fluorescent carbon quantum dot is prepared using short chain volatile fatty acid as carbon-based material |
CN110208547A (en) * | 2019-06-27 | 2019-09-06 | 北京柏海达科技有限公司 | A kind of propepsin immunochromatographytest test kit and preparation method thereof based on carbon quantum dot |
CN110408389A (en) * | 2019-08-05 | 2019-11-05 | 深圳大学 | A kind of carbon quantum dot and its preparation method and application |
CN111205862A (en) * | 2020-01-08 | 2020-05-29 | 辽宁大学 | Application of carbon quantum dot with multiple fluorescence emission centers as optical sensor in visual detection of trace water in organic solvent |
CN111573654A (en) * | 2020-06-10 | 2020-08-25 | 山西大学 | Green fluorescent carbon quantum dot for detecting pH value in acidic environment and preparation method thereof |
CN112552903A (en) * | 2020-12-10 | 2021-03-26 | 辽宁科技大学 | Room-temperature phosphorescent material based on carbon dots in composite matrix and preparation method and application thereof |
CN113201331A (en) * | 2021-04-23 | 2021-08-03 | 宁波萃英化学技术有限公司 | Dual-mode excited room temperature phosphorescent carbon dot |
CN113502159A (en) * | 2021-08-17 | 2021-10-15 | 岭南师范学院 | Preparation method of pH activated carbon quantum dot emitting fluorescence in near-infrared region I, product and application thereof |
US20220033266A1 (en) * | 2019-02-28 | 2022-02-03 | Anhui University | Copper ion-doped carbon dots, preparation method and application thereof as photosensitizer for photodynamic therapy |
CN115924887A (en) * | 2022-12-29 | 2023-04-07 | 北京建工环境修复股份有限公司 | Preparation method of novel carbon dot material and application of novel carbon dot material in detection of perfluorinated compounds |
CN116426278A (en) * | 2023-02-20 | 2023-07-14 | 郑州大学 | Method for preparing full-color carbon dots on large scale under normal temperature and normal pressure |
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US12054398B2 (en) * | 2019-02-28 | 2024-08-06 | Anhui University | Copper ion-doped carbon dots, preparation method and application thereof as photosensitizer for photodynamic therapy |
US20220033266A1 (en) * | 2019-02-28 | 2022-02-03 | Anhui University | Copper ion-doped carbon dots, preparation method and application thereof as photosensitizer for photodynamic therapy |
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CN111573654A (en) * | 2020-06-10 | 2020-08-25 | 山西大学 | Green fluorescent carbon quantum dot for detecting pH value in acidic environment and preparation method thereof |
CN112552903A (en) * | 2020-12-10 | 2021-03-26 | 辽宁科技大学 | Room-temperature phosphorescent material based on carbon dots in composite matrix and preparation method and application thereof |
CN113201331A (en) * | 2021-04-23 | 2021-08-03 | 宁波萃英化学技术有限公司 | Dual-mode excited room temperature phosphorescent carbon dot |
CN113201331B (en) * | 2021-04-23 | 2023-02-21 | 宁波萃英化学技术有限公司 | Dual-mode excited room temperature phosphorescent carbon dot |
CN113502159A (en) * | 2021-08-17 | 2021-10-15 | 岭南师范学院 | Preparation method of pH activated carbon quantum dot emitting fluorescence in near-infrared region I, product and application thereof |
CN115924887B (en) * | 2022-12-29 | 2024-02-06 | 北京建工环境修复股份有限公司 | Preparation method of carbon dot material and application of carbon dot material in detection of perfluorinated compounds |
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