CN109607512A - It is a kind of to pass through the pyrolysis standby carbon quantum dot of system with molecular sieve for preparing and its in the application of hydrogen peroxide context of detection - Google Patents
It is a kind of to pass through the pyrolysis standby carbon quantum dot of system with molecular sieve for preparing and its in the application of hydrogen peroxide context of detection Download PDFInfo
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Abstract
It is a kind of by the pyrolysis standby carbon quantum dot of system with molecular sieve for preparing and its in the application of hydrogen peroxide context of detection, belong to c-based nanomaterial technical field.The present invention by molecular sieve space confinement act on, by hydrothermal synthesis and post-processing obtain with ultraviolet excitation, size smaller and uniform (about 2.5nm), the carbon quantum dot material with good stability and photoluminescent property and its as fluorescence probe hydrogen peroxide context of detection application.Its main preparation process are as follows: using silicon source, magnesium source, phosphoric acid and organic formwork agent as raw material, molecular sieve crystal product is prepared using hydrothermal synthesis, by the operations purification such as being pyrolyzed, chromatographing to obtain water-soluble carbon dots product；The blue-fluorescence (transmitting peak position is about 420nm) that excitation does not depend on is presented in prepared carbon dots, and Old plant can be realized to hydrogen peroxide, and quenching constant and detection limit are respectively 7.3 × 103M‑1With 3.16 μM.
Description
Technical field
The invention belongs to c-based nanomaterial technical fields, and in particular to a kind of space confinement effect using molecular sieve,
The carbon amounts with ultraviolet excitation that hydrothermal synthesis, fumed pyrogenic, etching processing, TLC separation through over-molecular sieve obtain
Son point material and its as fluorescence probe hydrogen peroxide context of detection application.
Background technique
In recent years, hydrogen peroxide as cancer, Alzheimer disease, atherosclerosis, Parkinson's disease, myocardial infarction,
The important pathology medium of the neurodegenerative diseases such as diabetes, receives more and more attention in biochemistry and environmental area.
But the concentration of hydrogen peroxide is usually lower in biological fluids, it is difficult to track.Therefore, it establishes a kind of efficient, easy, sensitive, selective
The method of detection hydrogen peroxide is of great significance.
So far, common hydrogen peroxide detection method has colorimetric method, electrochemistry, fluorescence method, chemoluminescence method etc.
A variety of determination methods.In these methods, with its analysis, simple, quick, high sensitivity, sample damage are small, pass through for fluorescence method
The advantages that Ji, is increasingly by the attention of researchers and concern.In fluorescent technique, selecting suitable fluorescence probe is one
Mostly important step.In current report, people have used miscellaneous fluorescence probe to carry out to peroxidating
The detection of hydrogen, including metal organic framework (mental organic frameworks, MOFs), quantum dot, Nano silver grain,
Organic colorimeter, rare-earth luminescent material film are all used for the detection of hydrogen peroxide.
Carbon quantum dot (abbreviation CDs) is a kind of novel Illuminant nanometer carbon material, and size is generally less than 10nm.With biography
The semiconductor-quantum-point of system is compared, and carbon nano dot has excellent in optical properties, is easy preparation synthesis, water-soluble good, low toxicity, ring
The advantages that guarantor, causes the great research interest of people.These advantages make CDs in bio-imaging, medical diagnosis, photoelectricity and biography
The fields such as sensor have a wide range of applications.In terms of sensor or probe, CDs can be widely used for detecting various inorganic and organic matter
Kind, such as metal ion (such as Hg2+, Fe3+, Cu2+, Be2+, Ag+, K+, Zn2+, Al3+Deng), hypochlorous acid, glucose, dopamine, urine
Acid, ssDNA, melamine etc..
Compared with other hydrogen peroxide fluorescence probes, carbon quantum dot innately has good biocompatibility, low toxicity, stability
The advantages that high, thus there is very big application potential.In this patent, we are made from molecular sieve by means such as pyrolysis separation
For a kind of carbon quantum dot material of the highly sensitive response hydrogen peroxide of energy, the material settling out is nontoxic, and high sensitivity, is
A kind of fluorescence probe material of great application potential.
Summary of the invention
It is examined the purpose of the present invention is to provide a kind of carbon quantum dot standby by pyrolysis system with molecular sieve for preparing and its in hydrogen peroxide
Survey the application of aspect.The present invention is carrier by means of having the molecular sieve of regular nano-pore, passes through calcining and separating treatment, preparation
A kind of carbon quantum dot of blue emission, the carbon quantum dot have good response to hydrogen peroxide.Present invention process is simple, can weigh
Renaturation is good, and detection stability is high, reproducible, is a kind of ideal novel detection material.
The present invention utilizes the hydrothermal synthesis of molecular sieve, by calcining the molecular sieve containing organic formwork agent, then further carves
Erosion processing separation, prepares a kind of carbon quantum dot material of the blue luminescence generated by light of ultraviolet excitation, and the stability of material is excellent,
There is good dissolubility in water and in ethyl alcohol, and has sensitive fluorescence response to the hydrogen peroxide in environment, thus can
For the hydrogen peroxide in probe in detecting solution.
A kind of carbon quantum standby by pyrolysis system with molecular sieve for preparing of the present invention, is prepared by following steps:
(1) hydrothermal synthesis of molecular sieve: silicon source (boehmite), magnesium source (four acetate hydrate magnesium) are successively dissolved in water-soluble
In agent, phosphoric acid (H is then added3PO4, mass fraction 85%) and organic formwork agent (n-formyl sarcolysine phenylpiperidines), it persistently stirs to get solidifying
Glue, the molar ratio of each effective ingredient is 1.0Al in initial reactant2O3: 1.0~1.2MgO:2.2P2O5: 5.0 N-methyl piperazines
Pyridine: 350~400H2O；Gel is transferred in the stainless steel cauldron of polytetrafluoroethyllining lining, in quiet in 170~190 DEG C of baking ovens
Only heat 2~4 days；Reaction kettle is taken out, natural cooling obtains the molecular sieve with regular nano-pore；
(2) preparation and separation of carbon quantum dot CD-1 solution: 400~500 after the molecular sieve grinding that step (1) is obtained
It is calcined 3~5 hours under the conditions of DEG C, heating rate is 3~5 DEG C/min, is taken out after its cooling completely；Thereto be added 1~
3mL concentration is the sodium hydroxide solution of 2~3mol/L, ultrasonic dissolution；Then ethyl alcohol is added, is centrifugated；Centrifugation is collected to produce
The solution of object, and indissoluble object is filtered out with 0.22 micron of filter, the ethanol solution of carbon quantum dot is obtained, by obtained carbon quantum dot
Ethanol solution further separates and is enriched with by thin-layer chromatography to arrive carbon quantum dot CD-1 solution；
(3) detection of the carbon quantum dot CD-1 to hydrogen peroxide: the carbon quantum dot CD-1 solution and water body that step (2) is obtained
Then the hydrogenperoxide steam generator of a certain amount of volume (1 μ L) is added to be added in fluorescence cuvette after the dilution proportion of 1:4~8 in product
(the volumetric usage ratio of the carbon quantum dot CD-1 solution after hydrogenperoxide steam generator and dilution is 1:300~3000, and hydrogen peroxide is molten
The concentration of liquid is 0.1mol/L), then with the variation of the measurement solution fluorescence intensity of ultraviolet light irradiation 3~after five minutes；Then add every time
Enter the hydrogenperoxide steam generator (volume of the carbon quantum dot CD-1 solution after hydrogenperoxide steam generator and dilution of a certain amount of volume (1 μ L)
Usage ratio is 1:300~3000), then with the variation of the measurement solution fluorescence intensity of ultraviolet light irradiation 3~after five minutes；Through excessive
After secondary operation, standard curve of the solution fluorescence intensity than-concentration of hydrogen peroxide is established, for determining concentration of hydrogen peroxide
Amount detection.
The method have the characteristics that being carrier by the molecular sieve with regular nano-pore, acted on using its space confinement,
By simply calcine with TLC separation processing, prepare a kind of size it is smaller and uniform, have good stability and light
The carbon quantum dot material of photoluminescence property.Prepared carbon quantum dot partial size is about 2.5nm, because it is with more unsaturated carbon
Key, to there is apparent UV absorption at 300nm.And optimal luminous peak position is about 420nm, is a kind of ultraviolet region excitation
Carbon quantum dot, this has very big difference with common blue light excitation carbon quantum dot, and maximum excitation wavelength is about 250nm.
Because the higher carbon degree of unsaturation of the carbon quantum dot material, can be aoxidized, therefore peroxidating in aqueous solution by hydrogen peroxide
Hydrogen has apparent Fluorescence quenching effect to it, and quenching constant and detection limit are respectively 7.3 × 103M-1With 3.16 μM, can be with
The realization of hydrogen peroxide present in solution is responded rapidly to.And sample solution stability is good, can be visited with long-term preservation in biology
Needle has biggish application potential in terms of environment measuring.The present invention synthesizes a kind of environmentally friendly, stabilization, and has to hydrogen peroxide good
The carbon dots of good detection effect can be realized the sensitive and quick response to hydrogen peroxide.
Detailed description of the invention
Fig. 1: (experiment) (is calcined) afterwards before the hetero atom aluminum phosphate CHA type molecular sieve containing magnesium to synthesize in embodiment is calcined
And the XRD diagram of simulation (simulation) product；The XRD of analog product is the result being fitted according to standard illusion structure.
Fig. 2: for the UV-visible absorption spectrum of carbon quantum dot CD-1 obtained in embodiment；
Fig. 3: for the fluorescence excitation-emission matrix spectrogram for obtaining carbon quantum dot CD-1 in embodiment；
Fig. 4: for the high resolution transmission electron microscopy piece for obtaining carbon quantum dot CD-1 in embodiment；
Fig. 5: to obtain carbon quantum dot CD-1 in embodiment to the fluorescent quenching lab diagram of hydrogenperoxide steam generator.
As shown in Figure 1, experiment measures the powder X-ray diffractogram of solid sample CHA molecular sieve and the XRD spectrum of simulation
The diffraction peak of figure is almost the same, and the synthesized compound of this explanation is pure phase, and the spectrogram peak position of the sample of 450 DEG C of calcinings is basic
It is consistent, only intensity decreases, and illustrates that CHA skeleton is still kept, and only crystallization degree has after fumed pyrogenic
Declined, there is the presence of the organic formwork agent of carbonization in duct.
As shown in Fig. 2, there is a strong absworption peak, this attribution and unsaturated carbon core at 300nm in carbon quantum dot CD-1
The absorption of π-π * transition.
As shown in figure 3, carbon quantum dot CD-1 is excited in 250nm wavelength or so, transmitting optical range probably 400nm extremely
450nm, the best peak position wavelength for emitting light are 425nm.
As shown in figure 4, the average grain diameter of carbon quantum dot CD-1 is about 2.5nm.
As shown in figure 5, a figure is carbon quantum dot CD-1 and the quenching fluorescence spectrum of hydrogenperoxide steam generator, ordinate are each
Measured fluorescence intensity after addition hydrogen peroxide, abscissa are the wavelength of emission spectrum；B figure is not have UV illumination feelings
Under condition, the reference fluorescent spectrum of the hydrogenperoxide steam generator of same volume is added, ordinate is is surveyed after hydrogen peroxide is added every time
The fluorescence intensity obtained, abscissa are the wavelength of emission spectrum；C figure is to irradiate same time in the UV lamp, and peroxide is not added
Change the reference fluorescent spectrogram of hydrogen solution, ordinate is fluorescence intensity measured under different time, and abscissa is emission spectrum
Wavelength；D figure is the silent figure (Stern-Volmer Plot) in Stern-Wall of hydrogen peroxide detection, which quenched to substance
The embodiment of respond.Ordinate is fluorescence intensity ratio after initial fluorescent intensity and quenching, and abscissa is the hydrogen peroxide of addition
Concentration, all excitation wavelengths are all 280nm.
Specific embodiment
Below by embodiment, the present invention will be further described, and embodiments of the present invention are not limited thereto, cannot
It is interpreted as limiting the scope of the invention.
Embodiment 1:
By the hydrothermal synthesis with CHA type topological structure molecular sieve and separation is post-processed, is synthesized a kind of with ultraviolet light
Excitation, and have the carbon quantum dot of fluorescence response to hydrogenperoxide steam generator.
0.332g boehmite is dissolved in 14mL water, continues to sequentially add 0.438g magnesium acetate under magnetic agitation,
The n-formyl sarcolysine phenylpiperidines of 0.6mL phosphoric acid (mass fraction 85%) and 1.2mL continue stirring and obtain gel in 1 hour.Gel is transferred to poly-
Reaction kettle is placed in 180 DEG C of baking ovens by the stainless steel cauldron of tetrafluoroethene liner, is added under the spontaneous pressure of reaction kettle
Thermal response 3 days, after crystallization is complete, reaction kettle natural cooling is taken out, product is by washing drying to obtain MgAPO molecular sieve；
After the molecular sieve of preparation is carefully ground, the mesh number after grinding is 60 mesh.Calcining 4 is small in 450 degree of Muffle furnace
When, it is taken out after its cooling completely, gained is pale yellow powder shape solid.Calcining sample prepared by 1.0g is taken, 2.2mL is added
Sodium hydroxide solution (2.5mol/L), sufficiently ultrasound 20 points of kinds to accelerate and make it completely dissolved.Then add again into system
Enter the ethyl alcohol of 15mL, 15 points of kinds are finally centrifuged with 10000 revs/min of speed in centrifuge, makes solid insoluble and solution point
From.Solution after being centrifuged is collected, and filters out indissoluble object with 0.22 micron of filter, obtains the ethanol solution of carbon quantum dot, then use acetic acid
Ethyl ester: methanol volume ratio=11:1 is solvent, by TLC separation, be enriched with the highly polar product of separating for several times to get
To carbon quantum dot CD-1；
Quartz colorimetric utensil is added in the carbon quantum dot solution (carbon quantum dot: water volume ratio=1:6) for taking 3mL to dilute
In, measure and record its fluorescence intensity.Then the concentration that 1 μ L is added is the hydrogenperoxide steam generator of 0.1mol/L, after being added
With ultraviolet light irradiation 3 minutes, the fluorescence intensity of solution was measured again, it can be observed that with the addition fluorescence of hydrogenperoxide steam generator
Intensity has apparent reduction；Then the concentration for adding 1 μ L is the hydrogenperoxide steam generator of 0.1mol/L, with purple after being added
Outer light irradiation 3 minutes measures the fluorescence intensity of solution again；Repeatedly test (14 times altogether, the hydrogen peroxide being added every time
The volume of solution is 1 μ L, and the concentration for the hydrogenperoxide steam generator being added is 0.1mol/L) until its fluorescence intensity reaches minimum
Until.In order to exclude influence of the ultraviolet lighting to carbon dots solution intensity, the quenching experiments of same illumination time are similarly implemented.It will
The carbon dots solution of same volume is added in fluorescence cuvette, then in the case where no hydrogenperoxide steam generator is added, ultraviolet
The identical time is irradiated under lamp, then the variation of its fluorescence intensity is observed in measurement.Experiment shows prepared carbon quantum dot CD-1
There are good detection effect, fluorescence intensity ratio (initial fluorescent intensity and fluorescence intensity ratio after quenching)-dense to hydrogen peroxide
Line (also known as Stern-Volmer Plot, the silent figure in Stern-Wall) of writing music can be very good by linear equation y=0.073x+
0.682 (y is fluorescence intensity ratio, and x is hydrogenperoxide steam generator concentration, linear regression coefficient value R2It is reachable 0.9981) to intend
It closes；(quenching constant Ksv is the ratio of bimolecular quenching rate constant and unimolecule decay rate constant, value to its quenching constant
For the slope of fitting a straight line) and detection limit respectively 7.3 × 103M-1With 3.16 μM, so as to realize to concentration of hydrogen peroxide
Quantitative detection.
Claims (5)
1. a kind of carbon quantum standby by pyrolysis system with molecular sieve for preparing, is prepared by following steps:
(1) hydrothermal synthesis of molecular sieve: silicon source, magnesium source are successively dissolved in aqueous solvent, and phosphoric acid and organic formwork agent is then added,
Gel is persistently stirred to get, the molar ratio of each effective ingredient is 1.0Al in initial reactant2O3: 1.0~1.2MgO:
2.2P2O5: 5.0 n-formyl sarcolysine phenylpiperidines: 350~400H2O；Gel is transferred in the stainless steel cauldron of polytetrafluoroethyllining lining, in
Static heating 2~4 days in 170~190 DEG C of baking ovens；Reaction kettle is taken out, natural cooling obtains the molecule with regular nano-pore
Sieve；
(2) preparation and separation of carbon quantum dot CD-1 solution: in 400~500 DEG C of items after the molecular sieve grinding that step (1) is obtained
It is calcined 3~5 hours under part, heating rate is 3~5 DEG C/min, is taken out after its cooling completely；It is dense that 1~3mL is added thereto
Degree is the sodium hydroxide solution of 2~3mol/L, ultrasonic dissolution；Then ethyl alcohol is added, is centrifugated；Collect the molten of centrifugation product
Liquid, and indissoluble object is filtered out with 0.22 micron of filter, the ethanol solution of carbon quantum dot is obtained, the ethyl alcohol of obtained carbon quantum dot is molten
Liquid further separates and is enriched with by thin-layer chromatography to arrive carbon quantum dot CD-1 solution.
2. a kind of carbon quantum standby by pyrolysis system with molecular sieve for preparing as described in claim 1, it is characterised in that: silicon source is to intend thin water
Aluminium stone, magnesium source are four acetate hydrate magnesium, and the mass fraction of phosphoric acid is 85%, and organic formwork agent is n-formyl sarcolysine phenylpiperidines.
3. a kind of carbon quantum answering in hydrogen peroxide context of detection standby by pyrolysis system with molecular sieve for preparing of any of claims 1 or 2
With.
4. a kind of carbon quantum answering in hydrogen peroxide context of detection standby by pyrolysis system with molecular sieve for preparing as claimed in claim 3
With, it is characterised in that: by carbon quantum dot CD-1 solution and water volume to be added in fluorescence cuvette after the dilution proportion of 1:4~8,
Then the hydrogenperoxide steam generator of a certain amount of volume, the volume of the carbon quantum dot CD-1 solution after hydrogenperoxide steam generator and dilution is added
Usage ratio is 1:300~3000, and the concentration of hydrogenperoxide steam generator is 0.1mol/L, then with ultraviolet light irradiation 3~survey after five minutes
Measure the variation of solution fluorescence intensity；Then the hydrogenperoxide steam generator of a certain amount of volume, hydrogenperoxide steam generator and dilution are added every time
The volumetric usage ratio of carbon quantum dot CD-1 solution afterwards is 1:300~3000, and the concentration of hydrogenperoxide steam generator is 0.1mol/L,
Again with the variation of ultraviolet light irradiation 3~measure after five minutes solution fluorescence intensity；After multi-pass operation, it is strong to establish solution fluorescence
Ratio-concentration of hydrogen peroxide standard curve is spent, for the quantitative detection to concentration of hydrogen peroxide.
5. a kind of carbon quantum answering in hydrogen peroxide context of detection standby by pyrolysis system with molecular sieve for preparing as claimed in claim 4
With, it is characterised in that: hydrogen peroxide has an apparent Fluorescence quenching effect to carbon quantum dot in aqueous solution, quenching constant and
Detection limit is respectively 7.3 × 103M-1With 3.16 μM.
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Cited By (5)
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| CN112337499A (en) * | 2020-11-20 | 2021-02-09 | 重庆大学 | Composite nano material with catalytic property, preparation method and application |
| CN112570021A (en) * | 2019-09-30 | 2021-03-30 | 中国石油化工股份有限公司 | Nano material and preparation method thereof |
| CN113493197A (en) * | 2021-07-22 | 2021-10-12 | 哈尔滨工程大学 | Preparation method of carbon dot/porous silicon dioxide nanoenzyme with peroxidase-like activity |
| CN113533283A (en) * | 2021-07-15 | 2021-10-22 | 广州珠矶科技有限公司 | Method for detecting hydrogen peroxide by using carbon quantum dots |
| CN113999674A (en) * | 2021-11-21 | 2022-02-01 | 福州市第二医院（福建省福州中西医结合医院、福州市职业病医院） | CDs synthesis method and detection of H by CDs2O2Method (2) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112570021A (en) * | 2019-09-30 | 2021-03-30 | 中国石油化工股份有限公司 | Nano material and preparation method thereof |
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| CN113533283A (en) * | 2021-07-15 | 2021-10-22 | 广州珠矶科技有限公司 | Method for detecting hydrogen peroxide by using carbon quantum dots |
| CN113493197A (en) * | 2021-07-22 | 2021-10-12 | 哈尔滨工程大学 | Preparation method of carbon dot/porous silicon dioxide nanoenzyme with peroxidase-like activity |
| CN113493197B (en) * | 2021-07-22 | 2022-06-21 | 哈尔滨工程大学 | Preparation method of carbon dot/porous silica nanoenzyme with peroxidase-like activity |
| CN113999674A (en) * | 2021-11-21 | 2022-02-01 | 福州市第二医院（福建省福州中西医结合医院、福州市职业病医院） | CDs synthesis method and detection of H by CDs2O2Method (2) |
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