CN110079309A - A kind of green synthesis method of blue-light-emitting carbon quantum dot - Google Patents
A kind of green synthesis method of blue-light-emitting carbon quantum dot Download PDFInfo
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- CN110079309A CN110079309A CN201910347905.9A CN201910347905A CN110079309A CN 110079309 A CN110079309 A CN 110079309A CN 201910347905 A CN201910347905 A CN 201910347905A CN 110079309 A CN110079309 A CN 110079309A
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Abstract
The invention discloses a kind of green synthesis methods of blue-light-emitting carbon quantum dot, by the drying of aquatic products waste crucian squama, are fully ground, weigh crucian carp fish scale powder and be dissolved in aqueous solution, ultrasound is completely dissolved to form uniform crucian squama dispersion liquid to crucian carp fish scale powder;Crucian squama dispersion liquid is transferred in hydrothermal reaction kettle in 150 ~ 220 DEG C of 6 ~ 27h of reaction, cooled to room temperature obtains dark brown solution after reaction, obtained dark brown solution is removed into large particulate matter after being centrifuged, it filters to obtain blue-light-emitting carbon quantum dot solution with the filter membrane that aperture is 0.2 μm, it carries out rotary evaporation and obtains concentrate solution, then be freeze-dried to obtain powdered blue-light-emitting carbon quantum dot.Blue-light-emitting carbon quantum dot obtained by the present invention does not need purifies and separates, and fluorescence quantum yield is higher, can reach 6.9% in optimal conditions, and its synthesis process uses pure natural carbon source, expands application of the fluorescent carbon quantum dot in every field.
Description
Technical field
The invention belongs to the synthesis technical fields of carbon nanomaterial, and in particular to a kind of green of blue-light-emitting carbon quantum dot
Synthetic method.
Background technique
Global energy shortage, environmental degradation are got worse at present, are developed reliable, the sustainable efficient green energy and are compeled
The eyebrows and eyelashes.The various biomass waste materials of nature can prepare active carbon material by simple processing.Based on biomass
The carbon material of presoma has caused the extensive concern of people.Carbon quantum dot is a kind of novel fluorescence carbon nanomaterial, it is one
The approximate ball-type of kind and diameter are less than the zero-dimensional semiconductor nanocrystal of 10nm.In recent ten years bio-imaging, drug delivery,
Nanosensor, photoelectron and photocatalysis are widely used.Due to carbon quantum dot have brilliant water solubility, photostability and
The features such as good biocompatibility, and the inexpensive scale that is easy to is combined to.Therefore, carbon quantum dot can become a kind of novel
Alternative fluorescent nano probe.Fluorescence probe has high sensitivity, fast response time, good selective, can be right
Analyte carries out quantitative detection.Currently based on fluorescence probe detection various analysis substances such as metal ion, Medicine small molecule with
And large biological molecule etc., some detections make fluorescence by strong quenching, have by the photo induced electron transfer between donor-receiver
System controls the enhancing and decrease of fluorescence by identification competitive reaction, and some is carried out with a kind of mode of reversible fluorescent switch
Detection.Fluorescent small molecule would generally be in face of the difficulty and two aspect problem of cytotoxicity of synthesis.Therefore, find it is being easily obtained,
It is very necessary that reliable fluorescence probe, which carries out analysis detection,.
The preparation method of carbon quantum dot is roughly divided into (top-down) " from top to bottom " and " from bottom to top " (bottom-up)
Two kinds.The former mainly decomposes big carbon structure, such as graphite, carbon nanotube and carbon nano-fiber etc., and decomposition method includes object
Method of science, chemical method, electrochemical method etc..And bottom-to-top method is then by as small point of organic matter and polymer etc.
Sub- presoma is polymerized, and method is hydrothermal carbonization, oxidation polymerization effect, microwave assisting method, ultrasonic method etc..It explores and utilizes ring
It protects, green, predecessor cheap and easy to get, there is the carbon quantum dot of fluorescence property very using the preparation of simple and effective experimental method
It is necessary.Fish scale is usually scraped off when waste is directly thrown away, and is a kind of very common biomass waste material, can be used as a kind of honest and clean
The precursor preparation carbon quantum dot that valence is easy to get, the present invention, which is reported, prepares the new of carbon quantum dot using aquatic products waste as carbon source
Method, this carbon nanomaterial might have good performance as fluorescence probe and be widely applied in terms of analysis detection,
Therefore it is of great significance.
Summary of the invention
Prepare that simple, fluorescence property is excellent, cytotoxicity is small and suitable the technical problem to be solved by the present invention is to provide a kind of
It is suitable for the green synthesis method of the blue-light-emitting carbon quantum dot of large-scale production, this method is made with raw material crucian squama cheap and easy to get
For carbon source, using water as solvent, one-step synthesis blue-light-emitting carbon quantum dot, and by further confirming height made from this method
The significant effect of the blue-light-emitting carbon quantum dot of fluorescence quantum yield.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, and a kind of green of blue-light-emitting carbon quantum dot is closed
At method, it is characterised in that specific steps are as follows:
Step S1: by the drying of aquatic products waste crucian squama, being fully ground, weigh crucian carp fish scale powder and be dissolved in aqueous solution, wherein
The charge ratio of crucian carp fish scale powder and aqueous solution is 0.01 ~ 10g:1mL, and ultrasound is completely dissolved to be formed uniformly to crucian carp fish scale powder
Crucian squama dispersion liquid;
Step S2: the crucian squama dispersion liquid that step S1 is obtained is transferred in hydrothermal reaction kettle in 150 ~ 220 DEG C of 6 ~ 27h of reaction,
Cooled to room temperature obtains dark brown solution after reaction, then obtained dark brown solution is removed bulky grain after being centrifuged
Then substance filters to obtain blue-light-emitting carbon quantum dot solution with the filter membrane that aperture is 0.2 μm, blue-light-emitting carbon quantum dot is molten
Liquid carries out rotary evaporation and obtains concentrate solution, is finally freeze-dried concentrate solution to obtain powdered blue-light-emitting carbon quantum
Point.
Preferably, the charge ratio of crucian carp fish scale powder and aqueous solution described in step S1 is 0.04g:1mL, water in step S2
Thermal response temperature is 200 DEG C, the hydro-thermal reaction time 20h, the blue-light-emitting carbon amounts obtained under the above-mentioned condition of various concentration
Under the action of son point, cell is able to maintain higher survival rate, with the increase of blue-light-emitting carbon quantum dot concentration, cell survival
Rate do not generate conspicuousness reduction, when blue-light-emitting carbon quantum dot concentration reaches 500 μ g/mL, cell survival rate still 90% with
On, the cytotoxicity of blue-light-emitting carbon quantum dot obtained is low, biocompatibility is high, be suitable for cell in vitro, in-vivo tissue with
And the fluorescence imaging label in biological living.
Preferably, the aqueous solution is deionized water or distilled water.
Preferably, the temperature of the freeze-drying is -50 DEG C.
Raw material of the present invention is cheap and easy to get, and synthetic route is simple, and synthesis condition is mildly controllable, is not necessarily to pre-treatment and more purification
Deng operation, no coupling product;Obtained blue-light-emitting carbon quantum dot does not need purifies and separates, and fluorescence quantum yield is higher, most
It can reach 6.9% under the conditions of excellent, and its synthesis process uses pure natural carbon source, expands fluorescent carbon quantum dot in every field
In application.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of blue-light-emitting carbon quantum dot made from embodiment 1;
Fig. 2 is the Fourier transform infrared spectroscopy figure of blue-light-emitting carbon quantum dot made from embodiment 1;
Fig. 3 is the cell survival rate schematic diagram of blue-light-emitting carbon quantum dot made from embodiment 1.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
It by the drying of aquatic products waste crucian squama, is fully ground, weighs 0.8g crucian carp fish scale powder and be dissolved in 20mL distilled water, ultrasound
It is completely dissolved to form uniform crucian squama dispersion liquid to crucian carp fish scale powder;Obtained crucian squama dispersion liquid is transferred to hydro-thermal reaction
In 200 DEG C of reaction 20h in kettle, cooled to room temperature obtains dark brown solution after reaction, then obtained dark-brown is molten
Liquid removes large particulate matter after being centrifuged, and then filters to obtain blue-light-emitting carbon quantum dot solution with the filter membrane that aperture is 0.2 μm,
Blue-light-emitting carbon quantum dot solution progress rotary evaporation is obtained into concentrate solution, finally freezes concentrate solution in -50 DEG C
It is dried to obtain powdered blue-light-emitting carbon quantum dot.Resulting blue-light-emitting carbon quantum dot is configured to blue-light-emitting carbon quantum dot
Solution constant volume is in 10mL volumetric flask, 130ng mL-1With sepectrophotofluorometer, (FP-6500 type Fluorescence Spectrometer, Japanese Shimadzu are public
Department) measurement solution fluorescence intensity be 566.
The histogram of cell survival rate under the blue-light-emitting carbon quantum dot of Fig. 3 display various concentration, from the figure 3, it may be seen that not
Under the action of the blue-light-emitting carbon quantum dot of concentration, cell is able to maintain higher survival rate, with blue-light-emitting carbon quantum
The increase of point concentration, cell survival rate does not generate conspicuousness reduction, when blue-light-emitting carbon quantum dot concentration reaches 500 μ g/mL,
Cell survival rate illustrates that the cytotoxicity of blue-light-emitting carbon quantum dot made from the present embodiment is low, bio-compatible still 90% or more
Property high, the fluorescence imaging label suitable for cell in vitro, in-vivo tissue and biological living.
Embodiment 2
It by the drying of aquatic products waste crucian squama, is fully ground, weighs 0.8g crucian carp fish scale powder and be dissolved in 30mL distilled water, ultrasound
It is completely dissolved to form uniform crucian squama dispersion liquid to crucian carp fish scale powder;Obtained crucian squama dispersion liquid is transferred to hydro-thermal reaction
In 200 DEG C of reaction 20h in kettle, cooled to room temperature obtains dark brown solution after reaction, then obtained dark-brown is molten
Liquid removes large particulate matter after being centrifuged, and then filters to obtain blue-light-emitting carbon quantum dot solution with the filter membrane that aperture is 0.2 μm,
Blue-light-emitting carbon quantum dot solution progress rotary evaporation is obtained into concentrate solution, finally freezes concentrate solution in -50 DEG C
It is dried to obtain powdered blue-light-emitting carbon quantum dot.Resulting blue-light-emitting carbon quantum dot is configured to blue-light-emitting carbon quantum dot
Solution constant volume is in 10mL volumetric flask, 130ng mL-1With sepectrophotofluorometer, (FP-6500 type Fluorescence Spectrometer, Japanese Shimadzu are public
Department) measurement solution fluorescence intensity be 472.
Embodiment 3
It by the drying of aquatic products waste crucian squama, is fully ground, weighs 0.8g crucian carp fish scale powder and be dissolved in 40mL distilled water, ultrasound
It is completely dissolved to form uniform crucian squama dispersion liquid to crucian carp fish scale powder;Obtained crucian squama dispersion liquid is transferred to hydro-thermal reaction
In 200 DEG C of reaction 20h in kettle, cooled to room temperature obtains dark brown solution after reaction, then obtained dark-brown is molten
Liquid removes large particulate matter after being centrifuged, and then filters to obtain blue-light-emitting carbon quantum dot solution with the filter membrane that aperture is 0.2 μm,
Blue-light-emitting carbon quantum dot solution progress rotary evaporation is obtained into concentrate solution, finally freezes concentrate solution in -50 DEG C
It is dried to obtain powdered blue-light-emitting carbon quantum dot.Resulting blue-light-emitting carbon quantum dot is configured to blue-light-emitting carbon quantum dot
Solution constant volume is in 10mL volumetric flask, 130ng mL-1With sepectrophotofluorometer, (FP-6500 type Fluorescence Spectrometer, Japanese Shimadzu are public
Department) measurement solution fluorescence intensity be 376.
Embodiment 4
It by the drying of aquatic products waste crucian squama, is fully ground, weighs 0.8g crucian carp fish scale powder and be dissolved in 50mL distilled water, ultrasound
It is completely dissolved to form uniform crucian squama dispersion liquid to crucian carp fish scale powder;Obtained crucian squama dispersion liquid is transferred to hydro-thermal reaction
In 200 DEG C of reaction 20h in kettle, cooled to room temperature obtains dark brown solution after reaction, then obtained dark-brown is molten
Liquid removes large particulate matter after being centrifuged, and then filters to obtain blue-light-emitting carbon quantum dot solution with the filter membrane that aperture is 0.2 μm,
Blue-light-emitting carbon quantum dot solution progress rotary evaporation is obtained into concentrate solution, finally freezes concentrate solution in -50 DEG C
It is dried to obtain powdered blue-light-emitting carbon quantum dot.Resulting blue-light-emitting carbon quantum dot is configured to blue-light-emitting carbon quantum dot
Solution constant volume is in 10mL volumetric flask, 130ng mL-1With sepectrophotofluorometer, (FP-6500 type Fluorescence Spectrometer, Japanese Shimadzu are public
Department) measurement solution fluorescence intensity be 320.
Embodiment 5
0.8g crucian carp fish scale powder is taken to be dissolved in 20mL distilled water respectively, ultrasound to solid is completely dissolved, and then turns above-mentioned solution
It moves in hydrothermal reaction kettle and heats 5h, 10h, 15h, 20h, 25h and 30h respectively in 200 DEG C, natural cooling obtains after reaction
6 parts of dark brown solutions will be made after gained dark brown solution centrifugation removal bulky grain precipitating with aperture for 0.2 μm of filter membrane suction filtration
Carbon quantum dot solution progress rotary evaporation is obtained concentrate solution, finally by concentrate solution in -50 DEG C of conditions by carbon quantum dot solution
Lower freeze-drying obtains powdered blue-light-emitting carbon quantum dot.Resulting blue-light-emitting carbon quantum dot is configured to blue-light-emitting carbon
Quantum dot solution constant volume is in 10mL volumetric flask, 130ng mL-1With sepectrophotofluorometer (FP-6500 type Fluorescence Spectrometer, Japan
Shimadzu Corporation) measurement solution fluorescence intensity results it is as shown in table 1.
The influence that the 1 different heating time of table synthesizes blue-light-emitting carbon quantum dot
The hydro-thermal reaction time (h) | 5 | 10 | 15 | 20 | 25 | 30 |
Fluorescence intensity | 420 | 467 | 500 | 566 | 580 | 585 |
As shown in Table 1, the glimmering of almost complete, synthesized blue-light-emitting carbon quantum dot is reacted when the hydro-thermal reaction time is 20h
Luminous intensity is most strong;The hydro-thermal reaction time is too short, and not exclusively, fluorescence intensity is lower, with the extension of the hydro-thermal reaction time, instead for carbonization
Degree is answered to increase, fluorescence intensity increases;Then extend the hydro-thermal reaction time again, under the fluorescence intensity of blue-light-emitting carbon quantum dot
Drop.
Embodiment 6
0.8g crucian carp fish scale powder is taken to be dissolved in 20mL distilled water respectively, ultrasound to solid is completely dissolved, and then turns above-mentioned solution
It moves to successively in 160 DEG C, 180 DEG C, 200 DEG C and 220 DEG C heating 20h in hydrothermal reaction kettle, natural cooling obtains 6 after reaction
Part dark brown solution will be made after gained dark brown solution centrifugation removal bulky grain precipitating with aperture for 0.2 μm of filter membrane suction filtration
Carbon quantum dot solution progress rotary evaporation is obtained concentrate solution by carbon quantum dot solution, and concentrate solution is cold under the conditions of -50 DEG C
Jelly is dried to obtain powdered blue-light-emitting carbon quantum dot.Resulting blue-light-emitting carbon quantum dot is configured to blue-light-emitting carbon quantum
Point solution constant volume is in 10mL volumetric flask, 130ng mL-1With sepectrophotofluorometer (FP-6500 type Fluorescence Spectrometer, Japanese Shimadzu
Company) fluorescence intensity of solution is measured as the results are shown in Table 2.
The influence that 2 hydrothermal temperature of table synthesizes blue-light-emitting carbon quantum dot
Hydrothermal temperature (DEG C) | 160 | 180 | 200 | 220 |
Fluorescence intensity | 438 | 520 | 566 | 541 |
As shown in Table 2, when hydrothermal temperature is 200 DEG C, the fluorescence intensity of synthesized blue-light-emitting carbon quantum dot reaches
It is maximum;Not exclusively, fluorescence intensity is lower for the too low then carbonization of hydrothermal temperature.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (4)
1. a kind of green synthesis method of blue-light-emitting carbon quantum dot, it is characterised in that specific steps are as follows:
Step S1: by the drying of aquatic products waste crucian squama, being fully ground, weigh crucian carp fish scale powder and be dissolved in aqueous solution, wherein
The charge ratio of crucian carp fish scale powder and aqueous solution is 0.01 ~ 10g:1mL, and ultrasound is completely dissolved to be formed uniformly to crucian carp fish scale powder
Crucian squama dispersion liquid;
Step S2: the crucian squama dispersion liquid that step S1 is obtained is transferred in hydrothermal reaction kettle in 150 ~ 220 DEG C of 6 ~ 27h of reaction,
Cooled to room temperature obtains dark brown solution after reaction, then obtained dark brown solution is removed bulky grain after being centrifuged
Then substance filters to obtain blue-light-emitting carbon quantum dot solution with the filter membrane that aperture is 0.2 μm, blue-light-emitting carbon quantum dot is molten
Liquid carries out rotary evaporation and obtains concentrate solution, is finally freeze-dried concentrate solution to obtain powdered blue-light-emitting carbon quantum
Point.
2. the green synthesis method of blue-light-emitting carbon quantum dot according to claim 1, it is characterised in that: institute in step S1
The charge ratio for stating crucian carp fish scale powder and aqueous solution is 0.04g:1mL, and hydrothermal temperature is 200 DEG C in step S2, and hydro-thermal is anti-
It is 20h between seasonable, under the above-mentioned condition of various concentration under the action of blue-light-emitting carbon quantum dot obtained, cell is able to maintain
Higher survival rate, with the increase of blue-light-emitting carbon quantum dot concentration, cell survival rate does not generate conspicuousness reduction, in blue
When luminous carbon quantum dot concentration reaches 500 μ g/mL, cell survival rate still 90% or more, blue-light-emitting carbon quantum dot obtained
Cytotoxicity is low, biocompatibility is high, the fluorescence imaging label suitable for cell in vitro, in-vivo tissue and biological living.
3. the green synthesis method of blue-light-emitting carbon quantum dot according to claim 1, it is characterised in that: the aqueous solution
For deionized water or distilled water.
4. the green synthesis method of blue-light-emitting carbon quantum dot according to claim 1, it is characterised in that: the freezing is dry
Dry temperature is -50 DEG C.
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CN114214064A (en) * | 2021-12-20 | 2022-03-22 | 重庆文理学院 | Biomass carbon quantum dot and preparation method thereof |
CN115043393A (en) * | 2022-07-15 | 2022-09-13 | 武汉纺织大学 | Ultralong phosphorescent keratin derived carbon quantum dot and preparation method thereof |
CN115043393B (en) * | 2022-07-15 | 2023-11-10 | 武汉纺织大学 | Super-long phosphorescent keratin derived carbon quantum dot and preparation method thereof |
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