CN108795421A - A kind of Preparation method and use of chlorine doped graphene quantum dot - Google Patents
A kind of Preparation method and use of chlorine doped graphene quantum dot Download PDFInfo
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- CN108795421A CN108795421A CN201810324109.9A CN201810324109A CN108795421A CN 108795421 A CN108795421 A CN 108795421A CN 201810324109 A CN201810324109 A CN 201810324109A CN 108795421 A CN108795421 A CN 108795421A
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Abstract
The invention discloses a kind of Preparation method and uses for mixing chlorine graphene quantum dot, belong to inorganic material preparation process technical field.This method is by by the Sucralose electrochemical polymerization of small molecule, having prepared chlorine doped graphene quantum dot.And the type for mixing the oxygen-containing functional group in chlorine quantum dot can be adjusted by changing voltage and time.This chlorine doped graphene quantum dot can effective scavenging capacity oxygen radical, there is excellent antioxygenic property.In illumination, chlorine doped graphene quantum energy effectively generates active oxygen radical, shows excellent prooxidant energy.Preparation method of the present invention is simple, easy to operate; raw material is easy to get; suitable for large-scale production, in radicals scavenging (such as intracellular anti-oxidant, fuel protection) field and generates free radicals (such as optical dynamic therapy is sterilized) field is gathered around and have broad application prospects.
Description
Technical field
The present invention relates to a kind of Preparation method and uses of chlorine doped graphene quantum dot.The quantum dot prepared has
Excellent anti-oxidant and prooxidant energy, belongs to inorganic material preparation process technical field.
Background technology
Active oxygen radical refers to having chemically active free radical and some molecules, including list by what oxygen molecule derived from
Line state oxygen, hydrogen peroxide, superoxide radical and hydroxyl radical free radical.Active oxygen radical is anti-in food preservation, cosmetics, metal
Structural damage (cell membrane, protein and DNA etc.) etc. is all played the part of in rotten, high molecular material and biological medicine and organisms
Drill important role.
Much research shows that there is carbon nanomaterial the ability of scavenging capacity oxygen radical, such as carbon nanotube, fullerene to spread out
Biology, Graphene derivative etc..It is compound to form stable free radical by the way that electronics transfer occurs with free radical for carbon nanomaterial
Object plays the role of removing free radical, can also inhibit the generation of free radical with the metal ion-chelant in Fenton's reaction.?
In carbon nanomaterial, graphene quantum dot has good bio-compatibility, excellent photoluminescence performance and electrophilic energy
Power is widely paid close attention to.
It is worth noting that, electron donor and electron acceptor molecule there are when, graphene quantum dot solution it is glimmering
Light can all be quenched, this shows that graphene quantum dot exists simultaneously enzymatic oxidation (generating active oxygen radical when illumination) and resists
Aoxidize the performance of (scavenging capacity oxygen radical).However only active oxygen is removed and generated to the graphene quantum dot of oxygen doping certainly
Limited by the ability of base, we are a greater degree of to change in graphene quantum dot by the larger chlorine atom of doping electronegativity
Electron density distribution degree, and probed by changing the content of the oxygen-containing functional group in graphene quantum dot, chlorine atom doping
The influence of active oxygen radical ability is generated to graphene quantum dot illumination with oxygen-containing functional group type.
Invention content
For the deficiency of existing preparation method, an object of the present invention is to provide a kind of graphene amount of chlorine doping
Son point preparation method.Using the Sucralose of small molecule, the graphene of chlorine doping has been prepared by the method for electrochemical polymerization
Quantum dot.And the time by changing electropolymerization, regulate and control the type of oxygen-containing functional group.Anti-oxidant and rush oxygen is finally obtained
Change all more excellent chlorine doped graphene quantum dot of performance.
The second object of the present invention is to provide a kind of purposes of chlorine doped graphene quantum dot, the chlorine doped graphene
Quantum dot is as described in purpose one.The chlorine doped graphene quantum is used to generate free radicals oxidation when dye protection and illumination anti-
Bad hematic acid field.
The present invention provides a kind of preparation of chlorine doped graphene quantum dot and application processes, using cheap trichlorine sugarcane
Sugar is that raw material has obtained chlorine doped graphene quantum in strong caustic with the method for electrochemical workstation electropolymerization
Point.The quantum dot prepared has excellent anti-oxidant (with reference to figure 4) and enzymatic oxidation (with reference to figure 6) performance.It is provided by the invention
Preparation method is simple, low energy consumption, pollutes less and has excellent performance, will be in radicals scavenging (as intracellular anti-oxidant, dyestuff is protected
Shield etc.) it field and generates free radicals (such as optical dynamic therapy, sterilization) field is gathered around and have broad application prospects.
A kind of preparation method of chlorine doped graphene quantum dot, it is characterised in that electrochemically Sucralose exists
It is polymerized to the graphene quantum dot of chlorine doping in sodium hydroxide electrolyte, by adjusting voltage and polymerization time, has prepared not
With the chlorine doped graphene quantum dot of oxygen-containing functional group type.
Further, the preparation method of the chlorine doped graphene quantum dot, specific preparation process include following step
Suddenly：
Step 1) uses two platinum electrodes, wherein one is used as working electrode, another as reference electrode and to electricity
1g Sucraloses are added, using 10ml sodium hydroxides as electrolyte in pole；
Step 2) uses electrochemical workstation, carries out electropolymerization with potentiostatic mode, application voltage is 5~10v, time
For 45min~4h；
Step 3) acquired solution is dialysed 3 days with the bag filter of 0.22 μm of 3500Da, after removing the electrolyte in solution,
The aqueous solution of graphene quantum dot is obtained, graphene quantum dot powder is obtained after freeze-drying.
Further, it is 4M that electrolyte, which is naoh concentration, in the step 1)；Apply electricity described in the step 2)
Pressure is 7.5v, time 45min.
Further, the dialysis described in step 3) is to carry out the complete solution of electropolymerization with the water system filtering head of 220nm
Filter, the bag filter for being then 3500Da with molecular cut off are dialysed, and extra ion and unreacted trichlorine sugarcane are removed
Sugar, dialysis time are 3 days, and a deionized water was changed every 3 hours.
The as described above chlorine doped graphene quantum dot has an ability for removing free radical, and when illumination, which has, to be produced from
By the ability of base, the chlorine doped graphene quantum is applied to intracellular anti-oxidant, dye protection and visible light is led according to sterilization
Domain.
Preferably, the electrode is two platinum electrodes, wherein one is used as working electrode, another as reference electricity
Pole and to electrode, platinum electrode distance is 6~10mm.
Preferably, the electrolyte is to be placed in 10ml beakers with 10ml sodium hydroxides (4M).
Preferably, the Sucralose dosage is 1g.
Preferably, the voltage is 5~10v, such as 5v, 7.5v, 10v etc..
Preferably, the reaction time is 45min~4h, such as 45min, 2h, 4h etc..
Advantageous effect
(1) preparation method of the present invention is simple, of low cost and environmental-friendly, has certain commericially feasible
Property.
(2) the chlorine doped graphene quantum dot that the method for the invention obtains is compared with undoped graphene quantum dot,
It is removed the ability generated free radicals when free radical and illumination and been significantly enhanced.
Description of the drawings
Fig. 1 is the synthesis mechanism figure of chlorine doped graphene quantum dot of the present invention.
Fig. 2 is the transmission electron microscope (a) and high-resolution-ration transmission electric-lens figure of chlorine doped graphene quantum dot prepared by embodiment 1
(b)。
Fig. 3 is the C1s swarming fitted figures of chlorine doped graphene quantum dot XPS tests prepared by 1 different condition of embodiment.
The current potential used in left figure is 5v, 7.5v, 10v, and it is 2h and 4h that the current potential used in right figure, which is the 5v times,.
Fig. 4 is the active oxygen radical cleaning performance figure of chlorine doped graphene quantum dot prepared by embodiment 2.
Fig. 5 is the dye protection performance map of chlorine doped graphene quantum dot prepared by embodiment 2.
Fig. 6 is that chlorine doped graphene quantum dot prepared by embodiment 2 generates active oxygen radical oxidation when visible light shines
The performance map of ascorbic acid.
Specific implementation mode
With reference to specific embodiment, the invention will be further elaborated.
Embodiment one
1g Sucraloses are weighed, are added in the beaker of 10ml, 10ml sodium hydroxides (4M) are added, use two platinum filament electricity
Pole, wherein one is working electrode, another is, using electrochemical workstation, to apply 5- to electrode and reference electrode simultaneously
10v voltages, electropolymerization 45min-4h, obtained solution are dialysed 3 days with 0.22 μm of bag filter (3500Da), are removed in solution
Electrolyte after, obtain the aqueous solution of chlorine doped graphene quantum dot.
The obtained chlorine doped graphene quantum dot of preparation is tested as follows：
Transmission electron microscope and high-resolution-ration transmission electric-lens characterization are prepared from the high-resolution-ration transmission electric-lens it can be seen from the figure that of Fig. 2
The chlorine doped graphene quantum dot gone out has the lattice fringe of graphite quantum dot.The GQDs aqueous solutions of above-mentioned preparation are taken respectively, are dripped
It is coated onto the clean silicon chip surface of 0.5 × 0.5cm, shows to increase voltage by infrared spectrum and x-ray photoelectron spectroscopy test
With extend the electropolymerization time, the hydroxyl in graphene quantum dot is oxidized to carboxyl, and degree of oxidation improves.
Embodiment two
1g Sucraloses are weighed, are added in the beaker of 10ml, 10ml sodium hydroxides (4M) are added, use two platinum filament electricity
Pole, wherein one is working electrode, another is, using electrochemical workstation, to apply 7.5v to electrode and reference electrode simultaneously
Voltage, electropolymerization 45min, obtained solution are dialysed 3 days with 0.22 μm of bag filter (3500Da), remove the electrolysis in solution
After liquid, the aqueous solution of chlorine doped graphene quantum dot is obtained.
Antioxygenic property is tested：2mL solution includes the quantum dot of 100 μ g/mL, the TiO of 50 μ g/mL2, 25mM PBS and
10 μM of Luo Dan B (RhB).Under the conditions of magnetic agitation, after ultraviolet lighting 3h, pass through the characteristic absorption peak of absorption spectrum RhB
(554nm) determines the concentration of RhB.Graphene quantum dot is free of in contrast test.In ultraviolet lighting, TiO2It will produce work
Property oxygen radical RhB is decomposed into water and carbon dioxide, we protect dyestuff by the way that antioxidant graphene quantum dot is added
The active oxygen radical generated by illumination is avoided to decompose.It, can be according to the characteristic absorption of RhB by detecting the absorption spectrum of RhB
Peak monitors the concentration of RhB.Under 3h ultraviolet lights, the RhB of antioxidant is not by TiO2The active oxygen of generation is free
Base degrades 97.37%.And the RhB of graphene quantum dot (Cl-GQDs-7.5v) protection of 7.5v electropolymerizations 45min is only dropped
Solve 19%.And the RhB of undoped graphene quantum point protection has been downgraded 90.19%.Description of test Cl element doping energy
Effectively improve the oxidation resistance of graphene quantum dot.
Enzymatic oxidation performance test：There are one characteristic absorption peaks at 265nm for ascorbic acid, can be by graphene quantum dot
The amount of the singlet oxygen oxidation generated when illumination, the active oxygen radical that graphene quantum dot generates when illumination can be by anti-
The degree of oxidation of bad hematic acid is weighed.2mL solution contains the graphene quantum dot and 100 μM of ascorbic acid of 50 μ g/mL,
1000W/m2Visible light after half an hour, inhaled by UV, visible light according to (450W xenon lamps have filtered 400nm ultraviolet lights below)
Concentration of the receipts spectrum in the 265nm characteristic absorption blob detection ascorbic acid gone out.Cl-GQDs-7.5v is can as can be seen from Figure 6
The ability that active oxygen radical is generated when light-exposed photograph is most strong, the efficient oxidation ascorbic acid.
Claims (5)
1. a kind of preparation method of chlorine doped graphene quantum dot, it is characterised in that electrochemically by Sucralose in hydrogen-oxygen
Change the graphene quantum dot for being polymerized to chlorine doping in sodium electrolyte, by adjusting voltage and polymerization time, has prepared difference and contained
The chlorine doped graphene quantum dot of oxygen functional group type.
2. the preparation method of chlorine doped graphene quantum dot according to claim 1, which is characterized in that the preparation process
Include the following steps：
Step 1) uses two platinum electrodes, wherein one is used as working electrode, another, as reference electrode and to electrode, adds
Enter 1g Sucraloses, using 10ml sodium hydroxides as electrolyte；
Step 2) uses electrochemical workstation, carries out electropolymerization with potentiostatic mode, applications voltage is 5~10v, and the time is
45min~4h；
Step 3) acquired solution is dialysed 3 days with the bag filter of 0.22 μm of 3500Da, after removing the electrolyte in solution, obtains stone
The aqueous solution of black alkene quantum dot, obtains graphene quantum dot powder after freeze-drying.
3. the preparation method of chlorine doped graphene quantum dot according to claim 2, which is characterized in that in the step 1)
Electrolyte is that naoh concentration is 4M；It is 7.5v, time 45min to apply voltage described in the step 2).
4. the preparation method of chlorine doped graphene quantum dot according to claim 2, which is characterized in that described in step 3)
Dialysis is to be filtered the complete solution of electropolymerization with the water system filtering head of 220nm, is then 3500Da's with molecular cut off
Bag filter is dialysed, and extra ion and unreacted Sucralose are removed, and dialysis time is 3 days, changed every 3 hours and once goes
Ionized water.
5. the purposes of chlorine doped graphene quantum dot according to claim 1 or 2, which is characterized in that the chlorine adulterates stone
Black alkene quantum dot has the ability for removing free radical, with the ability generated free radicals, the chlorine doped graphene amount when illumination
Son is applied to intracellular anti-oxidant, dye protection and visible light shines sterilization field.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112262854A (en) * | 2020-12-04 | 2021-01-26 | 陕西科技大学 | Cl-modified GQD/APGQAS/acidified attapulgite nano composite antibacterial agent and preparation method thereof |
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| CN112262854A (en) * | 2020-12-04 | 2021-01-26 | 陕西科技大学 | Cl-modified GQD/APGQAS/acidified attapulgite nano composite antibacterial agent and preparation method thereof |
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