CN109847799A - With highlight catalytic active C-dots/UiO-66-NH2The preparation method and applications of composite material - Google Patents
With highlight catalytic active C-dots/UiO-66-NH2The preparation method and applications of composite material Download PDFInfo
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Abstract
The invention discloses one kind to have highlight catalytic active C-dots/UiO-66-NH2The preparation method and applications of composite material, by one pot of bath oiling by C-dots and UiO-66-NH2It is successfully prepared composite material, and passes through X-ray diffraction, Raman spectrum, SEM etc. is characterized.In addition, declining solution Ketoprofen experiment, illumination 1h, composite degradation 92%, UiO-66-NH by visible light2Only degrade 75%.The degradation rate of composite material is about UiO-66-NH21.87 times.C-dots and UiO-66-NH2Interface effectively promote the transfer of electronics, reduce the recombination rate in electronics and hole.Visible absorption is enhanced, energy needed for reducing generation excitation electronics promotes the generation in light induced electron and hole, enhances photocatalytic activity, can be preferably applied for the photocatalysis treatment of organic pollutant.
Description
Technical field
The invention belongs to the technical fields that nanocomposite and environmentally conscious materials are prepared and applied, and are related to a kind of oil bath one
Footwork prepares C-dots/UiO-66-NH2The enhancing photocatalytic activity that Ketoprofen is degraded under composite material and its visible light.
Background technique
In recent years, as a new class of carbon nanomaterial, carbon dots (C-dots) have at low cost, unique electronic transfer, nothing
The advantage of poison, has been more and more widely used in photocatalysis field.Compared with traditional quantum dot, C-dots biocompatibility
Well, toxicity is low, high water solubility, is easy to functional modification and has chemical inertness.In addition, C-dots has excellent photo electric
Energy, including advantageous electron-transport and ability of preserving, luminescence generated by light (PL) and wide light absorption.It is some that there is upper conversion PL performance
C-dots the long glistening light of waves can be absorbed, then issue short wavelength light, this will further improve light utilization efficiency.It can increase in conjunction with C-dots
Strong light absorption and the separation for promoting photo-generate electron-hole pair.At present in preparation C-dots composite material, needs high temperature, forges
It burns and the conditions such as logical nitrogen controls, process is sufficiently complex, and the cumbersome approaches can also reduce the light abstraction width of material, light is urged
The performances such as change.
Metal organic framework (MOF) is a series of porous materials of novel three-dimensional with high surface area with good orderly aperture
Material.They are being adsorbed, and catalysis and gas storage application aspect have good potentiality.It is worth us to be concerned with some special MOF
Type (such as Fe-MOF, Ti (IV)-MOF, Zr-MOF, Zn-MOF).They have good catalytic performance under light illumination, this returns
Because of the preparation of the excitation electronics transfer in them.Light is caused to be urged however, MOF generates excitation electronics and the low efficiency of separation charge
It is low to change reaction efficiency.UIO-66-NH2As a kind of common Zr base MOF since its thermal stability is good, surface area is big and photocatalysis
It is functional and be widely studied.However, it nevertheless suffers from some limitations due to its poorly conductive and visible light-responded weak.It is logical
Cross MOF is formed in conjunction with other function material composite material provide overcome these limit approach.
Therefore, by one-step method, it is a kind of feasible method for improving photocatalytic activity that C-dots, which is introduced into MOF,.
Summary of the invention
For UIO-66-NH2Poorly conductive and visible light-responded weak problem, the present invention provide a kind of novel C-dots/
MOF composite material, obtained composite material photocatalyst are conducive to the transmission process of photo-generated carrier, have good visible
Light photocatalytic activity, while also there is big specific surface area.And have studied C-dots/UiO-66-NH2Composite degradation ketone
Ibuprofen performance.
In order to achieve the above purpose, present invention employs technical solutions below:
A kind of bath oiling preparation C-dots/UiO-66-NH2Composite material, wherein C-dots and UiO-66-NH2Quality
Than for 0.1:1, prepared sample is denoted as C-dots/UiO-66-NH2。
C-dots/UiO-66-NH of the present invention2The preparation method of composite material, comprising the following steps:
(1) C-dots, UiO-66-NH are ultrasonically treated in organic solvent first2, it is ultrasonically treated 30 minutes, obtains mixed liquor；
The organic solvent is ethyl alcohol or N,N-dimethylformamide；
(2) mixed liquor is transferred in oil bath, is heated to 120 DEG C under stiring and is kept for 12 hours；
(3) it after cooling, is washed for several times by the way that obtained solid is collected by centrifugation, and with fresh ethanol, obtains product；
(4) finally, product to be placed on to drying in 120 DEG C of vacuum drying oven, C-dots/UiO-66-NH can be obtained2It is multiple
Condensation material.Wherein, the load capacity of C-dots is UiO-66-NH210wt%.
The C-dots is synthesized using candle cigarette ash by AMMONIA TREATMENT, and C-dots average grain diameter is 20 nm, brilliant
Compartment is away from for 0.208nm, UiO-66-NH2Surface it is smooth, partial size be 200nm or more.If C-dots partial size is too small, UiO-
66-NH2There may be multiple carbon dots in aperture, be unfavorable for being uniformly dispersed.The partial size of the carbon dots of different preparation method preparations and glimmering
Optical property differs greatly, and the luminescence generated by light of the bigger carbon dots of partial size can red shift.
C-dots/UiO-66-NH prepared by the present invention2Composite material enhances photocatalytic activity, can be used as efficiency light and urges
Change material, for handling organic pollutant.It shows to compare UiO-66-NH in Ketoprofen light degradation2Stronger Ketoprofen drop
Solve effect.
The present invention also provides above-mentioned C-dots/UiO-66-NH2Composite material is water-soluble to Ketoprofen in light degradation field
The photodegradative performance study of liquid.
Photocatalytic activity evaluation: by 10mg catalyst and 25mL Ketoprofen (25mg/L) aqueous solution in 25mL colorimetric cylinder
Mixing.Then the mixed solution was passed through into radiation of visible light (λ >=420nm) to reach adsorption equilibrium at unglazed lower stirring 1 hour
Carry out catalysis reaction.3mL ketoprofen solution is taken within every 20 minutes, by being centrifuged the catalyst being immediately disconnected in 3mL ketoprofen solution.
Concentration using ultraviolet-uisible spectrophotometer (UV-3600, Shimadzu) monitoring Ketoprofen changes, and measurement wavelength is
258nm.Absorbance measurement is carried out to the ketoprofen solution of various concentration, draws standard curve.According to the absorbance meter detected
The concentration for calculating Ketoprofen, is denoted as Ct.The concentration of Ketoprofen is denoted as C at the end of dark reaction0。
Through detecting, C-dots/UiO-66-NH prepared by the present invention2To Ketoprofen when composite material radiation of visible light 1h
Degradation rate up to 92%.
The beneficial effects of the present invention are:
(1) present invention simply prepares C-dots/UiO-66-NH using one pot of bath oiling2Composite material, compared to other sides
Method, prepared composite material have many advantages, such as that absorption property is good, photocatalysis performance is high.And simple process without high temperature, is forged
It burns, lead to the complex conditions such as nitrogen, greatly reduce energy consumption and reaction cost, convenient for batch production.
(2)C-dots/UiO-66-NH2In composite material, C-dots dispersibility is better, can be uniformly distributed, and C-
Dots and UiO-66-NH2Between interface effectively promote the transfer of electronics, reduce the recombination rate in electronics and hole, load
After C-dots, UiO-66-NH2Maximum absorption wavelength be expanded to 534 nm from 439nm, enhance visible absorption.Its forbidden band
Width is also down to 1.83eV from 2.69eV, and energy needed for reducing generation excitation electronics promotes light induced electron and hole
It generates.
(3) C-dots and UiO-66-NH2Synergistic effect is generated after Interface composites, can be improved composite material in visible light
Under photocatalytic activity, pass through detection, C-dots/UiO-66-NH2Composite material, which illustrates, compares UiO-66-NH2It is stronger for
The photocatalytic activity of degradation Ketoprofen.Radiation of visible light 1h, the degradation rate of Ketoprofen are higher than UiO-66-NH up to 92% significantly2
(75%).The kinetic rate of degradation is UiO-66-NH21.87 times.
Detailed description of the invention:
Fig. 1 is C-dots, UiO-66-NH2And C-dots/UiO-66-NH2The XRD spectrum of composite material；
Fig. 2 is C-dots, UiO-66-NH2And C-dots/UiO-66-NH2The Raman map of composite material；
Fig. 3 is C-dots/UiO-66-NH2SEM, TEM and HRTEM image of composite material；
Fig. 4 is UiO-66-NH2And C-dots/UiO-66-NH2PL map；
Fig. 5 is UiO-66-NH2And C-dots/UiO-66-NH2UV-visDRS map；
Fig. 6 is C-dots, UiO-66-NH2And C-dots/UiO-66-NH2Visible light decline solution Ketoprofen figure；
Fig. 7 is C-dots, UiO-66-NH2And C-dots/UiO-66-NH2The dynamics figure of degradation Ketoprofen.
Specific embodiment:
The following describes the present invention in detail with reference to examples, so that those skilled in the art more fully understand this hair
It is bright, but the invention is not limited to following embodiments.
Embodiment 1:
UiO-66-NH2It is synthesized by traditional method.Specifically carry out as follows:
A, 2.17g2- amino terephthalic acid (TPA) and 3.8g zirconium chloride are added in 50mL DMF；
B, it stirs the mixture for 30 minutes；
C, appeal mixture is transferred to stainless steel polytetrafluoroethyllining lining autoclave, and holding 24 is small at 120 DEG C
When；
D, by autoclave cooled to room temperature, by the way that solid is collected by centrifugation and is first washed for several times with after DMF with methanol；
E, obtained solid is first dried at room temperature for, and further 4 hours dry in 150 DEG C of baking oven.
C-dots is synthesized by candle cigarette ash.Specifically sequentially include the following steps:
A, glass plate is placed at the top of the candle of burning to collect candle cigarette ash；
B, the cigarette ash of collection is ultrasonically treated 30 minutes in 50ml ammonium hydroxide；
C, by gained suspension from the autoclave that beaker is transferred to Teflon lining, and the hydro-thermal in 150 DEG C of baking oven
Processing 7 hours；
D, finally, with after water and ethanol washing, sediment is dry in 80 DEG C of baking oven.
C-dots/UiO-66-NH2Composite material passes through bath oiling for the C-dots and UiO-66-NH of above-mentioned synthesis2In conjunction with
And it successfully prepares, comprising the following steps:
A, C-dots (0.01g), UiO-66-NH are ultrasonically treated first in 50mL DMF2(0.1g) 30 minutes；
B, mixed liquor is transferred in oil bath and is heated to 120 DEG C under stiring, and kept for 12 hours；
C, it after cooling, is washed for several times by the way that obtained solid is collected by centrifugation, and with fresh ethanol；
D, finally, product is placed on to drying in 120 DEG C of vacuum drying oven can be obtained C-dots/UiO-66-NH2Composite wood
Material.C-dots is in UiO-66-NH2In load capacity be 10%.
By the C-dots/UiO-66-NH of above-mentioned preparation2Composite material is by X-ray diffraction (XRD), Raman spectrum (Raman
Spectra), scanning electron microscope (SEM) and transmission electron microscope (TEM) prove.
Fig. 1 is C-dots, UiO-66-NH2And C-dots/UiO-66-NH2The XRD spectrum of composite material.It is multiple in XRD spectrum
The map and UiO-66-NH of condensation material2It is similar, but the intensity at peak slightly reduces, bone when this may be due to load C-dots
The slight change of frame tactical rule.
Fig. 2 is C-dots, UiO-66-NH2And C-dots/UiO-66-NH2The Raman map of composite material.Raman map
There are two characteristic peaks in the curve of middle C-dots, is located at about 1342cm-1And 1600cm-1, distribute to D the and G band of carbon.This
Outside, two characteristic peaks of C-dots also appear in C-dots/UiO-66-NH2In sample, it means that C-dots successfully exists
UiO-66-NH2On modified.UiO-66-NH2And C-dots/UiO-66-NH2Curve show 446cm-1、
1428cm-1、1554cm-1、1669cm-1The peak at place, it was demonstrated that UiO-66-NH in compound2Presence.
Fig. 3 is C-dots/UiO-66-NH2SEM, TEM and HRTEM image of composite material；SEM, TEM image show,
For the partial size of most of C-dots between 10~20nm, part is bigger than normal.UiO-66-NH2Surface it is smooth, partial size be 200nm with
On.C-dots is supported on UiO-66-NH2Surface.A large amount of C-dots is around UiO-66-NH simultaneously2Aggregation forms a large amount of
Good interface.HRTEM image shows clearly C-dots and UiO-66-NH2Interface.The spacing of lattice of C-dots is
0.208nm。
Fig. 4 is UiO-66-NH2And C-dots/UiO-66-NH2PL map；PL map shows C-dots/UiO-66-
NH2Fluorescence intensity be significantly below UiO-66-NH2, this is because C-dots and UiO-66-NH2Between interface promote
The transfer of electronics reduces the recombination rate in electronics and hole, improves photocatalytic activity.
Fig. 5 is UiO-66-NH2And C-dots/UiO-66-NH2UV-visDRS map.According to UV-vis DRS map,
After loading C-dots, UiO-66-NH2Maximum absorption wavelength be expanded to 534nm from 439nm, enhance visible absorption.It is prohibited
Bandwidth is also down to 1.83eV from 2.69eV, and energy needed for reducing generation excitation electronics promotes light induced electron and hole
Generation.
Fig. 6 is C-dots, UiO-66-NH2And C-dots/UiO-66-NH2Visible light decline solution Ketoprofen figure.Map is aobvious
Show, it is seen that light irradiate 1h after, Ketoprofen from the degradation rate that drop rate is 10%, C-dots be 80%, UiO-66-NH2Degradation
Rate is 75%, C-dots/UiO-66-NH2Degradation rate be 92%.It compares UiO-66-NH2Present stronger Ketoprofen
Degradation effect.Thus illustrate, C-dots and UiO-66-NH2Between the interfacial structure that generates promote the degradation of Ketoprofen.
Fig. 7 is C-dots, UiO-66-NH2And C-dots/UiO-66-NH2The dynamics figure of degradation Ketoprofen.Dynamics figure
Spectrum shows further C-dots, UiO-66-NH2And C-dots/UiO-66-NH2The kinetic rate of degradation Ketoprofen.C-
dots/UiO-66-NH2Kinetic rate (0.044min-1) it is about UiO-66-NH2(0.0235min-1) 1.87 times.
Above-mentioned testing result proves, C-dots/UiO-66-NH prepared by the present invention2C-dots and UiO- in composite material
66-NH2Preferable composite construction is formd, C-dots is supported on UiO-66-NH2Surface, while around UiO-66-NH2It is poly-
Collection forms a large amount of good interfacial contacts, forms unique texture, effectively promotes the transfer of electronics, reduces electronics and sky
The recombination rate in cave improves the photocatalytic activity of composite material.And by by C-dots/UiO-66-NH2Composite material and UiO-
66-NH2The comparison of degradation Ketoprofen, composite material up to 92%, are higher than the degradation rate of Ketoprofen significantly under visible light
UiO-66-NH2(75%), and the kinetic rate of degradation is UiO-66-NH21.87 times, to further demonstrate C-
Dots and UiO-66-NH2Between there are synergistic effects.
The embodiment is a preferred embodiment of the present invention, but present invention is not limited to the embodiments described above, not
In the case where substantive content of the invention, any conspicuous improvement that those skilled in the art can make, replacement
Or modification all belongs to the scope of protection of the present invention.
Claims (8)
1. one kind has highlight catalytic active C-dots/UiO-66-NH2The preparation method of composite material, which is characterized in that by C-
Dots and UiO-66-NH2It is evenly dispersed in a solvent, C-dots/UiO-66-NH is made in oil bath one-step method2Composite material.
2. having highlight catalytic active C-dots/UiO-66-NH as described in claim 12The preparation method of composite material,
It is characterized in that, comprising the following steps:
A, it is ultrasonically treated C-dots and UiO-66-NH in organic solvent first2, obtain mixed liquor；
B, mixed liquor is transferred in oil bath, is heated to 120 DEG C under stiring, and kept for 12 hours；
C, cooling after heating reaction, by the way that solid is collected by centrifugation, and for several times with ethanol washing, obtain product；
D, finally, it is product is dry in 120 DEG C of vacuum drying oven, obtain C-dots/UiO-66-NH2Composite material.
3. having highlight catalytic active C-dots/UiO-66-NH as described in claim 12The preparation method of composite material,
It being characterized in that, the C-dots is synthesized using candle cigarette ash by AMMONIA TREATMENT, and the average grain diameter of C-dots is 20nm,
Spacing of lattice is 0.208nm.
4. having highlight catalytic active C-dots/UiO-66-NH as described in claim 12The preparation method of composite material,
It is characterized in that, in C-dots/UiO-66-NH2In nano material, C-dots and UiO-66-NH2Mass ratio be 0.1:1.
5. having photocatalytic activity C-dots/UiO-66-NH as claimed in claim 22The method of composite material preparation, it is special
Sign is that the organic solvent is ethyl alcohol or n,N-Dimethylformamide.
6. having photocatalytic activity C-dots/UiO-66-NH as described in claim 12The preparation method of composite material, it is special
Sign is that in the composite material, C-dots is in UiO-66-NH2In load capacity be 10wt%.
7. as the method according to claim 1 to 6 prepares C-dots/UiO-66-NH2The application of composite material, feature
It is, the C-dots/UiO-66-NH2Composite material has visible light photocatalysis active, as high-efficiency photocatalysis material, uses
In processing organic pollutant.
8. C-dots/UiO-66-NH as claimed in claim 72The application of composite material, which is characterized in that the composite material exists
92% is reached to the degradation rate of Ketoprofen in 1h under visible light.
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