CN109321238A - A kind of preparation method and application of the carbon quantum dot base fluorescent optical sensor with hexavalent chromium detection function - Google Patents
A kind of preparation method and application of the carbon quantum dot base fluorescent optical sensor with hexavalent chromium detection function Download PDFInfo
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Abstract
A kind of preparation method and application of the carbon quantum dot base fluorescent optical sensor with hexavalent chromium detection function, is related to a kind of preparation method and application of carbon quantum dot base fluorescent optical sensor.It is to solve the problem of that the launch wavelength of fluorescent carbon quantum dot in the existing method using fluorescent carbon quantum dot detection heavy metal is lower to cannot achieve visualization fluorescence detection.Carbon source: one, being dissolved in n,N-Dimethylformamide by method, and ultrasonic treatment forms uniform mixed solution A；Two, solution A is poured into reaction kettle, reacts to obtain solution B；Three, solution B is fitted into centrifuge tube, is centrifuged repeatedly, retain supernatant；Four, supernatant is dialysed using bag filter, carbon quantum dot solution, as carbon quantum dot base fluorescent optical sensor is obtained after dialysis.The launch wavelength of the fluorescent carbon quantum dot of this method preparation can reach 530~550nm, can be realized the visualization fluorescence detection of heavy metal ion.The present invention is used for heavy metal analysis field.
Description
Technical field
The present invention relates to a kind of preparation method and applications of carbon quantum dot base fluorescent optical sensor.
Background technique
The problem of environment, has become a history long-standing problem, human lives and socio-economic development by the direct shadow of environment
It rings, is the significant problem of today's society extensive concern, importance is self-evident.Current environmental problem becomes and restricts China's warp
The a great problem of Ji and social development.The fast development of world economy and urbanization keeps the toxic pollutant of global low concentration anxious
Increase severely and add, harm is generated to the mankind and the ecosystem.Environment common contaminant includes organic pollutant, heavy metal contaminants, micro-
The three categories such as biology, the environmental pollution in China have showed the feature based on trace organic contamination, thus to environmental pollutants
Effective analysis detection is carried out to have a very important significance.
Hexavalent chromium [Cr (VI)] is used as a kind of huge heavy metal ion of toxicity, to human health and ecological environment meeting
It causes greatly to threaten.Cr (VI) is easy to be absorbed by the body, it can be invaded by digestion, respiratory tract, skin and mucous membrane
Human body.Cr (VI) compound has carcinogenesis in vivo, can also cause other many health problems, such as sucks certain higher
Cr (VI) compound of concentration can cause rhinorrhea, sneezing, itch, nosebleed, ulcer and perforation of nasal septum.Short-term large dosage
Contact, adverse consequences can be generated in contact site, including the stimulation of ulcer, schneiderian membrance and perforation of nasal septum.Take in over much dosage
Chromium to will lead to the damage of kidney and liver, nausea, GI irritation, gastric ulcer, spasm even dead.Skin contact will cause routed
Ulcer or allergic reaction.It factually tests studies have shown that Cr (VI) can be absorbed by the cell of many tissues and organ in vivo and can be in body
Interior accumulation endangers human physical and mental health huge.
Fluorescent carbon quantum dot is a kind of approximate ball-type and the zero-dimensional semiconductor nanocrystal of diameter < 10nm, by few molecule
Or former molecular nanocluster.It shows many superior optical functions, such as electrochemical luminescence, luminescence generated by light and photo-induction
Lead electronics transfer etc..Similar to traditional various heavy metal quantum dots, carbon quantum dot can issue bright in the case where illumination
Light.For universal, containing functional groups such as a large amount of carboxyl, hydroxyls on the surface of carbon quantum dot, to impart carbon quantum
The excellent water solubility of point, and be easy to then using all kinds of organic, polymeric, inorganic or biological segments by its function
Change.Meanwhile being contrasted with semiconductor-quantum-point, carbon dots have many characteristics such as chemical inertness, hypotoxicity, biocompatibility,
Environmental contaminants, biomolecule, cell imaging, photocatalysis and photoelectric device etc. oneself widely applied.
However, the launch wavelength of existing fluorescent carbon quantum dot is below 500nm, visualization fluorescence detection cannot achieve.
Summary of the invention
The present invention is to solve the hairs of fluorescent carbon quantum dot in the existing method using fluorescent carbon quantum dot detection heavy metal
The problem of ejected wave length is lower, cannot achieve visualization fluorescence detection, provides a kind of carbon amounts with hexavalent chromium detection function
The preparation method and application of son point base fluorescent optical sensor.
The present invention has the preparation method of the carbon quantum dot base fluorescent optical sensor of hexavalent chromium detection function, including following
Step:
One, carbon source is dissolved in n,N-Dimethylformamide, and is ultrasonically treated, form uniform mixed solution A；
Wherein carbon source and the molar ratio of N,N-dimethylformamide are 1:(50~130 in step 1)；
Two, the solution A for obtaining step 1 is poured into the reaction kettle that polytetrafluoroethylene (PTFE) is liner, and reaction kettle is put into baking oven
In react to obtain solution B；
Three, the solution B for obtaining step 2 is fitted into centrifuge tube, is centrifuged repeatedly 3-5 times, and the big bulk in removal bottom is solid
Body retains supernatant；
Four, the supernatant for obtaining step 3 is further purified carbon quantum dot solution, is gone using bag filter dialysis 48h
Except the reaction monomers not being carbonized, carbon quantum dot solution, as carbon quantum dot base fluorescent optical sensor are obtained after dialysis, are stored at 4 DEG C.
Further, carbon source described in step 1 is ethylenediamine tetra-acetic acid, sodium citrate or anti-sepsis acid.These types of carbon source
Can dissolve with n,N-Dimethylformamide becomes uniform mixed solution, helps further to generate size uniformity, stabilization, glimmering
The carbon quantum dot of the excellent fluorescent orange of optical property.
Further, the power being ultrasonically treated in step 1 is 60~80W, and the time of ultrasonic treatment is 10~30min.Choosing
Suitable ultrasonic power is selected, is conducive to the quick dissolution of carbon source, and do not destroy to the molecular structure of selected carbon source.Ultrasound
10~30min can guarantee that carbon source is completely dissolved in n,N-Dimethylformamide, be conducive to prepare size uniformity, stabilization, glimmering
The carbon quantum dot of the excellent fluorescent orange of optical property.
Further, the temperature of reaction described in step 2 is at 140~200 DEG C, and the reaction time is 6~for 24 hours.
Further, centrifugation rate described in step 3 is 8000~12000r/min.
Further, each centrifugation time is 20~40min in step 3.
Further, every 8h changes a deionized water in dialysis procedure in step 4.
Application of the carbon quantum dot base fluorescent optical sensor prepared by the above method in hexavalent chromium detection.
Further, when carrying out hexavalent chromium detection, carbon quantum dot solution is mixed with deionized water, then is examined
It surveys；Wherein the volume ratio of carbon quantum dot solution and deionized water is 1:6.To carbon quantum dot dilution after purification, be conducive to carbon amounts
The dispersion of son point, improves its detection sensitivity.
The principle of the present invention:
The principle of the present invention is mainly prepared carbon quantum dot surface containing carboxyl, amino isoreactivity group, so that
Prepared carbon quantum dot is easily complexed with Cr (VI), since the strong electron-withdrawing ability of Cr (VI) makes carbon quantum dot due to losing
Electronics and fluorescent quenching occurs, to realize highly sensitive detection of the quantum dot-based fluorescent optical sensor to Cr (VI).
Beneficial effects of the present invention:
The method of the present invention is common are machine molecule as raw material, the method being carbonized by solvent heat or Microwave-assisted firing,
Synthesize the carbon quantum dot based sensor of fluorescent functional.
The carbon quantum dot base fluorescent optical sensor size uniformity of hexavalent chromium detection function prepared by this method, size 3-
6nm, good dispersion.
The main electron-withdrawing ability strong according to hexavalent chromium of this method, causes carbon quantum dot sensor due to losing electronics
And leading to the principle of fluorescent quenching to realize the highly sensitive detection to hexavalent chromium, carbon quantum dot based sensor is for Cr VI
The detection sensitivity of ion is high, and minimal detectable concentration can reach 10-9mol/L.And having fluorescence efficiency high, fluorescence property is excellent
Advantage, fluorescence efficiency is up to 52.4%.
This method selects n,N-Dimethylformamide to make solvent, and n,N-Dimethylformamide not only plays the work of solvent
With, the effect of surface passivator and dressing agent is also acted as, a large amount of N heteroatom is contained on the surface of prepared carbon quantum dot,
There is humidification to the fluorescence property of carbon quantum dot, be conducive to the red shift of wavelength.The transmitted wave of the fluorescent carbon quantum dot of preparation
Length can reach 530~550nm, there is fluorescent orange function, have higher launch wavelength compared with traditional fluorescent carbon quantum dot,
It can be realized the visualization fluorescence detection of heavy metal ion.
This method synthetic method is simple, and raw material is cheap and easy to get, at low cost, and product obtained is nontoxic, can be mass-produced.
The present invention is applied to the fields such as heavy metal ion Cr (VI) highly sensitive detection.In environmental monitoring and improvement, materialized
Field has broad application prospects.
Detailed description of the invention
Fig. 1 is the TEM image of carbon quantum dot based sensor prepared by embodiment 1
Fig. 2 is the XRD spectra of carbon quantum dot based sensor prepared by embodiment 1；
Fig. 3 is the FTIR spectrum figure of carbon quantum dot based sensor prepared by embodiment 1；
Fig. 4 is the fluorescence excitation and emission spectra of carbon quantum dot based sensor prepared by embodiment 1；
Fig. 5 is the carbon quantum dot based sensor of the preparation of embodiment 1 to Cr (VI) fluorescence detection spectrum.
Specific embodiment
The technical solution of the present invention is not limited to the following list, further includes between each specific embodiment
Any combination.
Specific embodiment 1: present embodiment has the carbon quantum dot base fluorescent optical sensor of hexavalent chromium detection function
Preparation method, comprising the following steps:
One, carbon source is dissolved in n,N-Dimethylformamide, and is ultrasonically treated, form uniform mixed solution A；
Wherein carbon source and the molar ratio of N,N-dimethylformamide are 1:(50~130 in step 1)；
Two, the solution A for obtaining step 1 is poured into the reaction kettle that polytetrafluoroethylene (PTFE) is liner, and reaction kettle is put into baking oven
In react to obtain solution B；
Three, the solution B for obtaining step 2 is fitted into centrifuge tube, is centrifuged repeatedly 3-5 times, and the big bulk in removal bottom is solid
Body retains supernatant；
Four, the supernatant for obtaining step 3 is further purified carbon quantum dot solution, is gone using bag filter dialysis 48h
Except the reaction monomers not being carbonized, carbon quantum dot solution, as carbon quantum dot base fluorescent optical sensor are obtained after dialysis.
This method selects n,N-Dimethylformamide to make solvent, and n,N-Dimethylformamide not only plays the work of solvent
With, the effect of surface passivator and dressing agent is also acted as, a large amount of N heteroatom is contained on the surface of prepared carbon quantum dot,
There is humidification to the fluorescence property of carbon quantum dot, be conducive to the red shift of wavelength.The transmitted wave of the fluorescent carbon quantum dot of preparation
Length can reach 530~550nm, there is fluorescent orange function, have higher launch wavelength compared with traditional fluorescent carbon quantum dot,
It can be realized the visualization fluorescence detection of heavy metal ion.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: carbon source described in step 1 is
Ethylenediamine tetra-acetic acid, sodium citrate or anti-sepsis acid.It is other same as the specific embodiment one.
These types of carbon source can be dissolved with n,N-Dimethylformamide becomes uniform mixed solution, facilitates further life
At the carbon quantum dot of the excellent fluorescent orange of size uniformity, stabilization, fluorescence property.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: in step 1 at ultrasound
The power of reason is 60~80W, and the time of ultrasonic treatment is 10~30min.It is other the same as one or two specific embodiments.
The suitable ultrasonic power of selection, is conducive to the quick dissolution of carbon source, and not to the molecular structure of selected carbon source into
Row destroys.10~30min of ultrasound can guarantee that carbon source is completely dissolved in n,N-Dimethylformamide, and it is equal to be conducive to preparation size
One, stablize, the carbon quantum dot for the fluorescent orange that fluorescence property is excellent.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: institute in step 2
The temperature of reaction is stated at 140~200 DEG C, the reaction time is 6~for 24 hours.It is other identical as one of specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: institute in step 3
Stating centrifugation rate is 8000~12000r/min.It is other identical as one of specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: every in step 3
Secondary centrifugation time is 20~40min.It is other identical as one of specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: in step 4 thoroughly
Every 8h changes a deionized water during analysis.It is other identical as one of specific embodiment one to six.
Specific embodiment 8: present embodiment carbon quantum dot base fluorescent optical sensor answering in hexavalent chromium detection
With.
Specific embodiment 9: present embodiment is unlike specific embodiment eight: carrying out hexavalent chromium detection
When, carbon quantum dot solution is mixed with deionized water, then is detected；The wherein volume ratio of carbon quantum dot solution and deionized water
For 1:6.It is other identical as specific embodiment eight.
To carbon quantum dot dilution after purification, is conducive to the dispersion of carbon quantum dot, improves its detection sensitivity.
Elaborate below to the embodiment of the present invention, following embodiment under the premise of the technical scheme of the present invention into
Row is implemented, and gives detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following realities
Apply example.
Embodiment 1:
The preparation method of carbon quantum dot base fluorescent optical sensor of the present embodiment with hexavalent chromium detection function, including with
Lower step:
One, 0.5g ethylenediamine tetra-acetic acid is dissolved in 20mL n,N-Dimethylformamide, in the ultrasound that power is 60W
Middle dissolution forms uniform mixed solution.
Two, it is to put reaction kettle in the reaction kettle of liner that the solution for obtaining step 1, which pours into the polytetrafluoroethylene (PTFE) of 25mL,
Enter to react 12h in 200 DEG C of baking ovens and obtains carbon quantum dot solution.
Three, the carbon quantum dot solution that step 2 obtains is fitted into centrifuge tube, is centrifuged under the revolving speed of 10000r/min
30min is centrifuged repeatedly-dissolves, and carries out 3 times, and the big blocks of solid in removal bottom retains supernatant.
Four, the solution for obtaining step 3 is dialysed 48h (every 8h changes a deionized water) using bag filter, to carbon quantum
Point solution is further purified, and removes the reaction monomers not being carbonized, and carbon quantum dot solution after purification is stored at 4 DEG C.
Five, the carbon quantum dot solution that step 4 obtains is taken into 0.5mL, is mixed with 3mL deionized water, by it in various concentration
Cr (VI) effect, test the fluorescence intensity of mixed solution, realize the highly sensitive detection to Cr (VI).
Fig. 1 is the transmission electron microscope of the carbon quantum dot base fluorescent optical sensor of hexavalent chromium detection function manufactured in the present embodiment
Image, as shown in Figure 1, the particle size of the carbon quantum dot base fluorescent optical sensor of prepared hexavalent chromium detection function is about
4nm, size is than more uniform, favorable dispersibility.
Fig. 2 is the carbon quantum dot base XRD spectrum of hexavalent chromium detection function manufactured in the present embodiment；As shown in Fig. 2, institute
A wide diffraction maximum, explanation is presented in 20-30o in the carbon quantum dot base fluorescent optical sensor of the hexavalent chromium detection function of preparation
Prepared carbon quantum dot is the carbon structure of no crystal form.
Fig. 3 is the infrared spectrogram of the carbon quantum dot base fluorescent optical sensor of hexavalent chromium detection function, it can be seen that institute
The carbon quantum dot base fluorescent optical sensor surface of preparation is rich in groups such as-OH ,-NH ,-C=O ,-C-H.
Fig. 4 is the fluorescence excitation and emission spectra of the carbon quantum dot base fluorescent optical sensor of hexavalent chromium detection function, such as
Shown in Fig. 4, the fluorescence excitation peak that prepared carbon quantum dot base fluorescent optical sensor surface is rich in is in 450nm or so, fluorescent emission
Peak is in 539nm or so.It can be realized the visualization fluorescence detection of heavy metal ion.
Fig. 5 is the carbon quantum dot base fluorescent optical sensor of hexavalent chromium detection function to Cr (VI) fluorescence detection spectrum (Fig. 5
Middle curve is followed successively by 0,10 by concentration under upper-9mol/L、10-8mol/L、10-7mol/L、10-6mol/L、10-5mol/L、10- 4mol/L、10-3mol/L、10-2mol/L、10-1Mol/L), as shown in figure 5, with Cr (VI) concentration increase, carbon quantum dot is molten
The fluorescence intensity of liquid is gradually reduced, and minimal detectable concentration can be down to 10-9mol/L.And having fluorescence efficiency high, fluorescence property is excellent
Different advantage, fluorescence efficiency is up to 52.4%.
Embodiment 2:
The preparation method of carbon quantum dot base fluorescent optical sensor of the present embodiment with hexavalent chromium detection function, including with
Lower step:
One, 0.5g sodium citrate is dissolved in 20mL n,N-Dimethylformamide, it is molten in the ultrasound that power is 80W
Solution, forms uniform mixed solution.
Two, it is to put reaction kettle in the reaction kettle of liner that the solution for obtaining step 1, which pours into the polytetrafluoroethylene (PTFE) of 25mL,
Enter to react 16h in 140 DEG C of baking ovens and obtains carbon quantum dot solution.
Three, the carbon quantum dot solution that step 2 obtains is fitted into centrifuge tube, is centrifuged under the revolving speed of 10000r/min
30min is centrifuged repeatedly-dissolves, and carries out 3 times, and the big blocks of solid in removal bottom retains supernatant.
Four, the solution for obtaining step 3 is dialysed 48h (every 8h changes a deionized water) using bag filter, to carbon quantum
Point solution is further purified, and removes the reaction monomers not being carbonized, and carbon quantum dot solution after purification is stored up at 4 DEG C.
Five, the carbon quantum dot solution that step 4 obtains is taken into 0.5mL, is mixed with 3mL deionized water, by it in various concentration
Cr (VI) effect, test the fluorescence intensity of mixed solution, realize the highly sensitive detection to Cr (VI).
The particle size of the carbon quantum dot base fluorescent optical sensor of hexavalent chromium detection function manufactured in the present embodiment is about
4nm, size is than more uniform, favorable dispersibility.
In 450nm or so, fluorescence emission peak exists the fluorescence excitation peak that carbon quantum dot base fluorescent optical sensor surface is rich in
545nm.It can be realized the visualization fluorescence detection of heavy metal ion.
It is minimum pick up survey concentration can be down to 10-9mol/L.And there is fluorescence efficiency height, the excellent advantage of fluorescence property.
Embodiment 3:
The preparation method of carbon quantum dot base fluorescent optical sensor of the present embodiment with hexavalent chromium detection function, including with
Lower step:
One, 0.5g sodium citrate is dissolved in 20mL n,N-Dimethylformamide, it is molten in the ultrasound that power is 60W
Solution, forms uniform mixed solution.
Two, it is to put reaction kettle in the reaction kettle of liner that the solution for obtaining step 1, which pours into the polytetrafluoroethylene (PTFE) of 25mL,
Enter to react 18h in 140 DEG C of baking ovens and obtains carbon quantum dot solution.
Three, the carbon quantum dot solution that step 2 obtains is fitted into centrifuge tube, is centrifuged under the revolving speed of 10000r/min
30min is centrifuged repeatedly-dissolves, and carries out 3 times, and the big blocks of solid in removal bottom retains supernatant.
Four, the solution for obtaining step 3 is dialysed 48h (every 8h changes a deionized water) using bag filter, to carbon quantum
Point solution is further purified, and removes the reaction monomers not being carbonized, and carbon quantum dot solution after purification is stored up at 4 DEG C.
Five, the carbon quantum dot solution that step 4 obtains is taken into 0.5mL, is mixed with 3mL deionized water, by it in various concentration
Cr (VI) effect, test the fluorescence intensity of mixed solution, realize the highly sensitive detection to Cr (VI).
The particle size of the carbon quantum dot base fluorescent optical sensor of hexavalent chromium detection function manufactured in the present embodiment is about
4nm, size is than more uniform, favorable dispersibility.
In 450nm or so, fluorescence emission peak exists the fluorescence excitation peak that carbon quantum dot base fluorescent optical sensor surface is rich in
550nm.It can be realized the visualization fluorescence detection of heavy metal ion.
It is minimum pick up survey concentration can be down to 10-9mol/L.And there is fluorescence efficiency height, the excellent advantage of fluorescence property.
Claims (9)
1. a kind of preparation method of the carbon quantum dot base fluorescent optical sensor with hexavalent chromium detection function, it is characterised in that should
Method the following steps are included:
One, carbon source is dissolved in n,N-Dimethylformamide, and is ultrasonically treated, form uniform mixed solution A；Wherein
Carbon source and the molar ratio of N,N-dimethylformamide are 1:(50~130 in step 1)；
Two, the solution A for obtaining step 1 is poured into the reaction kettle that polytetrafluoroethylene (PTFE) is liner, and reaction kettle is put into baking oven instead
Deserved solution B；
Three, the solution B for obtaining step 2 is fitted into centrifuge tube, is centrifuged repeatedly 3-5 times, and the big blocks of solid in removal bottom is protected
Stay supernatant；
Four, the supernatant for obtaining step 3 obtains carbon quantum dot solution, as carbon amounts using bag filter dialysis 48h after dialysis
Son point base fluorescent optical sensor.
2. a kind of system of carbon quantum dot base fluorescent optical sensor with hexavalent chromium detection function according to claim 1
Preparation Method, it is characterised in that carbon source described in step 1 is ethylenediamine tetra-acetic acid, sodium citrate or anti-sepsis acid.
3. a kind of carbon quantum dot base fluorescent optical sensor with hexavalent chromium detection function according to claim 1 or 2
Preparation method, it is characterised in that the power being ultrasonically treated in step 1 is 60~80W, time of ultrasonic treatment is 10~
30min。
4. a kind of system of carbon quantum dot base fluorescent optical sensor with hexavalent chromium detection function according to claim 3
Preparation Method, it is characterised in that the temperature of reaction described in step 2 is at 140~200 DEG C, and the reaction time is 6~for 24 hours.
5. a kind of system of carbon quantum dot base fluorescent optical sensor with hexavalent chromium detection function according to claim 4
Preparation Method, it is characterised in that centrifugation rate described in step 3 is 8000~12000r/min.
6. a kind of system of carbon quantum dot base fluorescent optical sensor with hexavalent chromium detection function according to claim 5
Preparation Method, it is characterised in that each centrifugation time is 20~40min in step 3.
7. a kind of system of carbon quantum dot base fluorescent optical sensor with hexavalent chromium detection function according to claim 6
Preparation Method, it is characterised in that every 8h changes a deionized water in dialysis procedure in step 4.
8. application of the carbon quantum dot base fluorescent optical sensor of claim 1 the method preparation in hexavalent chromium detection.
9. application according to claim 8, it is characterised in that carry out hexavalent chromium detection when, by carbon quantum dot solution with
Deionized water mixing, then detected；Wherein the volume ratio of carbon quantum dot solution and deionized water is 1:6.
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| CN111088032A (en) * | 2019-12-13 | 2020-05-01 | 临沂大学 | Preparation method of fluorescent polymer for simultaneously detecting trivalent chromium ions and hexavalent chromium ions |
| CN112499616A (en) * | 2020-12-14 | 2021-03-16 | 广西大学 | Method for synthesizing fluorescent carbon quantum dots by taking marine product deep processing wastewater as raw material |
| WO2021077458A1 (en) * | 2019-10-22 | 2021-04-29 | 广东药科大学 | S,se-cqds and method therefor for efficiently detecting cr(vi) contaminant |
| CN113355090A (en) * | 2021-06-02 | 2021-09-07 | 东北林业大学 | Fluorescent wood sponge, preparation method thereof and application thereof in hexavalent chromium ion detection and adsorption |
| CN113916844A (en) * | 2020-07-08 | 2022-01-11 | 长春工业大学 | Preparation method of blue-red light dual-emission nano hybrid probe and application of blue-red light dual-emission nano hybrid probe in ion detection |
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| YIJUN ZHANG等: "Multicolour nitrogen-doped carbon dots: tunable photoluminescence and sandwich fluorescent glass-based light-emitting diodes", 《NANOSCALE》 * |
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