CN109759110A - A kind of N doping porous carbon loaded titanium dioxide photocatalyst and the preparation method and application thereof - Google Patents
A kind of N doping porous carbon loaded titanium dioxide photocatalyst and the preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a kind of N doping porous carbon loaded titanium dioxide photocatalysts and the preparation method and application thereof.This method is using Organometallic framework material (MOF) in N2Lower calcining carbonization obtains the porous carbon materials GC-N of N doping, and gained GC-N is dispersed in the ethanol solution containing mineralizer, and titanium source is added by hydro-thermal method and synthesizes GC-N-TiO2Composite material.Preparation method of the present invention is simple, without the use of toxic reagent, the doping of high proportion nitrogen can be realized in the synthesis process, can not only improve the separation rate of photo-generate electron-hole, increase the photocatalytic degradation efficiency to pollutant, while also there is excellent reaction stability.Prepared photochemical catalyst can be widely applied for the fields such as air contaminant treatment, water pollution control.
Description
Technical field
The invention belongs to technical field of function materials, and in particular to a kind of N doping porous carbon carried titanium dioxide photocatalysis
Agent (GC-N-TiO2) and the preparation method and application thereof.
Background technique
With the raising of Public environmental attitude, to the control pay attention to day by day of volatile organic matter (VOCs).VOCs not only comes
It derived from industrial production, is also from interior decoration and furniture, influences that crowd is wide, and exposure duration is long；Many VOCs not only have
Very strong toxicity and carcinogenicity, or the presoma of another atmosphere pollution ozone.Indoor environment has VOCs control technology
Many restrictions, traditional industrial Treatment process can not be applied effectively, and photocatalysis oxidation technique is as a kind of ring efficiently, safe
Border friendly depollution of environment technology receives significant attention.TiO2Due to having many advantages, such as that nontoxic, inexpensive, chemical property stabilization becomes
Most common photochemical catalyst, but it haves the shortcomings that electron hole is easy that compound, quantum efficiency is low, seriously affects its application effect
Fruit.By TiO2Being dispersed in carrier surface and inhibiting electron-hole recombinations is improve its photocatalysis degradation organic contaminant efficiency one
Effective way.Wherein porous carbon materials simultaneously have the characteristics that adsorptivity and high conductivity, can be enriched with pollutant and fastly
Speed transfer light induced electron, is to improve TiO2The ideal composite modification material of photocatalytic activity.
Currently, the preparation of porous carbon materials usually requires to carry out oxidation stripping using strong oxidizers such as the concentrated sulfuric acid or potassium permanganate
From and activate graphitic carbon (such as Chinese patent 201611177958.3 and periodical Advanced Materials, 2009,21,
2233-2239), or using hydrofluoric acid or sodium hydroxide structure of transvers plate pore structure (Energy & Environmental is etched
Science, 2014,7,1212-1249), and use the polymerizable raw materials such as formaldehyde, benzenediol carbonization (such as Chinese patent
201610916398.2 with periodical Renewable and Sustainable Energy Reviews, 2017,76,212-
215).The above method all inevitably uses virulent property and high pollution substance, and preparation method is complicated, is unfavorable for being catalyzed
The production application of material.
To overcome the above disadvantages, the present invention uses the metal organic framework for containing nitrogen as presoma, by forging
Burn carbonization after with TiO2It is compound, obtain the TiO modified containing nitrogen porous carbon2Material.The material of this method preparation not only synthesizes
Method is simple, is without the use of toxic reagent, and can realize that nitrogen-doping makes material possess higher conductivity in the material
With oxygen reducing ability to promote TiO2Electron-hole pair efficiently separates, and shows excellent activity and stability, is that light is urged
Change Material Field new breakthrough.Meanwhile the present invention provides new thinking for the improvement of organic pollutant.
Summary of the invention
It is an object of the invention to overcome conventional method titanium dioxide photoproduction electron-hole recombination rate high and conventional porous
Carbon synthesizes the defects of complicated pollution is big with composite titania material, provides a kind of GC-N-TiO2Photochemical catalyst and its preparation side
Method and application.Obtained photochemical catalyst is obviously improved the activity and stability of photochemical catalytic oxidation VOCs.
The object of the invention is achieved through the following technical solutions:
A kind of GC-N-TiO2The preparation method of photochemical catalyst, by organic ligand, metal node synthesize MOF be carbonized again after with titanium
N doping porous carbon carried titanium dioxide is prepared in source the methods of hydrolytic polymerization, washing and drying and calcining in specific solvent
Catalysis material.Using nitrogenous organic backbone synthesis MOF as presoma, at high temperature with nitrogen be coordinated metal Zn
Volatilization, generates defect to forming pyridine nitrogen and pyrroles's N structure, furthermore with TiO2Nitrogen in compound process, in carbon substrate
O atom can be replaced directly to be connected with Ti, further improve the rate that light induced electron is shifted from Ti atom in carbon substrate.Institute
Light induced electron transfer rate can be improved by stating photochemical catalyst, promote the separation of electron hole, possess the stable carbon skeleton of chemical property
As substrate, thus improve photocatalytic activity and stability.
A kind of GC-N-TiO2The preparation method of photochemical catalyst, which is characterized in that synthesize gold using organic ligand, metal salt
Belong to organic backbone, in the ethanol solution containing titanium source prepared by hydrolytic polymerization, washing, drying and the method for calcining after being carbonized
Obtain the catalysis material compound with N doping porous carbon.
A kind of GC-N-TiO2The preparation method of photochemical catalyst, which comprises the following steps:
(1) preparation of MOFs: the organic ligand of 3 ~ 6 g metal salts and 4 ~ 7 g is added in the methanol of 150 ~ 300 ml, room temperature
20 ~ 24 h of lower stirring, then by solution centrifuge separation, cleaning, drying, finally obtain MOFs；The metal salt includes six hydration nitre
Sour zinc, zinc acetate or zinc sulfate；The organic ligand is 2-methylimidazole；
(2) preparation of GC-N: the MOFs of 0.1 ~ 0.3 g is added in crucible, is placed in tube furnace, in N22 ~ 4 are calcined under atmosphere
H is collected after being cooled to room temperature, can be obtained the porous carbon materials GC-N of N doping；
(3) GC-N-TiO2Preparation: the GC-N of 0.01 ~ 0.02 g is added into the dehydrated alcohol of 20 ~ 40 mL, ultrasound is mixed
It is even, 0 ~ 30 min is stirred at room temperature, is obtained solution A, is subsequently added into 2 ~ 5 mL ammonium hydroxide, then the titanium source of 1 ~ 10 mL is added to and is stirred
In the solution A mixed, 30 ~ 60 min are stirred at room temperature, solution B is obtained, mixed solution B is transferred to ptfe autoclave
In liner, then ptfe autoclave liner is put into autoclave, 9 ~ 13 h of hydro-thermal reaction, then by solution pass through from
Heart separation, cleaning, drying, obtain powder C, powder C are transferred to crucible and is placed in tube furnace, in N22 ~ 4h is calcined under atmosphere,
Last GC-N-TiO to obtain the final product2Photochemical catalyst；The titanium source includes butyl titanate, isopropyl titanate.
In the above method, in step (1), the temperature stirred at room temperature is 25 ~ 35 DEG C, and stirring rate is 15 ~ 25
r/min。
In the above method, in step (1), described 4000 ~ 6000 turns of centrifuge separation revolving speed；The washing solution is first
Alcohol；The drying temperature is 60 ~ 80 DEG C, and drying time is 6 ~ 8 h.
In the above method, step (2) the tube furnace calcination temperature be 900 ~ 1000 DEG C, heating rate be 2 ~ 5 DEG C/
min。
In the above method, step (3) temperature stirred at room temperature is 25 ~ 35 DEG C, and stirring rate is 15 ~ 25 r/
min。
In the above method, step (3) hydrothermal temperature is 120 ~ 140 DEG C；The hydro-thermal reaction pressure be 0.1 ~
0.3 MPa；Described 4000 ~ 6000 turns of centrifuge separation revolving speed；The washing solution is ethyl alcohol or deionized water；The dry temperature
Degree is 60 ~ 80 DEG C, and drying time is 6 ~ 8 h.
In the above method, step (3) the tube furnace calcination temperature be 450 ~ 600 DEG C, heating rate be 2 ~ 5 DEG C/
min。。
A kind of GC-N-TiO2Photocatalyst applications are in atmospheric volatile organic compounds degradation and field of water pollution control.
There is difference substantially in material prepared by the present invention and existing material, the present invention passes through pre-synthesis nitrogenous
Organometallic skeletal, then by N2Lower high-temperature calcination, formed have Jie's microcellular structure N doping porous carbon, then with titanium
Calcining forms the TiO of Anatase after source composite hydrolysis is dry2, N can directly be connected with Ti in this course, and then quickly pass
Light induced electron is passed, inhibits electron-hole compound.Nitrogenous carbon substrate can shift rapidly light induced electron, the nitrogen-atoms on carbon
It can also be as electron acceptor and the O for being adsorbed on surface2Reaction forms O2 -, light induced electron can be made full use of, avoid it
It is compound in carbon substrate.
Compared with prior art, the present invention has the advantage that
The present invention synthesizes N doping porous carbon by carbonization organometallic skeletal and is applied to the field photochemical catalytic oxidation VOCs for the first time.
Synthetic method of the present invention is simple, without using virulent property high pollution drug, meets the objective of Green Chemistry.
This method can be achieved at the same time the N atom to carbon substrate and to the N doping of titanium dioxide, in carbon substrate directly with
Ti atom is connected, and has higher light reaction efficiency compared with common porous material.In addition, the N atom on carbon material can
Active sites are served as, and carbon skeleton chemical property is stablized, bigger serface possesses more active sites, therefore this material is with higher
Photocatalytic activity and stability, and atmospheric cleaning, water pollution control etc. can be widely used in.
Detailed description of the invention
Fig. 1 is TiO of the present invention2、GC-N-TiO2The XRD diagram of photochemical catalyst；
Fig. 2 is the scanning electron microscope sem figure of GC-N；
Fig. 3 is the GC-N-TiO after 5 mL isopropyl titanates of addition are compound2Scanning electron microscope sem figure；
Fig. 4 is GC-N-TiO2The x-ray photoelectron spectroscopy C1s of photochemical catalyst schemes；
Fig. 5 is GC-N-TiO2The x-ray photoelectron spectroscopy N1s of photochemical catalyst schemes；
Fig. 6 is GC-N-TiO2Photochemical catalyst is to 24 h of toluene degradation concentration variation diagram；
Fig. 7 is GC-N-TiO2Photochemical catalyst is to 24 h of toluene degradation CO x Production quantity variation diagram；
Fig. 8 is GC-N-TiO2, graphene-supported TiO2、TiO2To 24 h degradation effect figure of toluene.
Specific embodiment
The present invention will be further specifically described in detail with reference to specific embodiments, but embodiments of the present invention are not
It is limited to this, for not specifically specified technological parameter, can refer to routine techniques progress.
Embodiment 1
The preparation of GC-N: 5.95 g zinc nitrate hexahydrates and 6.16 g 2-methylimidazoles are added in 300 mL methanol, room temperature
24 h of lower stirring dry 8 h in 60 DEG C of baking ovens, obtain organometallic skeletal ZIF-8 after being centrifugated and being washed with methanol.
ZIF-8 is placed in porcelain crucible, in tube furnace with the heating rate of 2 DEG C/min in N2920 DEG C are warming up under atmosphere, simultaneously
In 920 DEG C of 3 h of calcining.After being cooled to room temperature, the porous carbon materials GC-N of N doping is obtained.
GC-N-TiO2Preparation: disperse 0.01 g GC-N in the dehydrated alcohol of 40mL, after 30 min of ultrasonic disperse
Solution A is formed, 2 mL ammonium hydroxide are added, 10 min is stirred at room temperature and forms solution B, then B solution is added in 5 mL isopropyl titanates
In, 20 min are persistently stirred, mixed solution C is formed, mixed solution C is transferred in ptfe autoclave liner, then will
Liner is put into autoclave, 12 h of hydro-thermal reaction under the conditions of 140 DEG C, 0.15 Mpa, after being cooled to room temperature, by sediment
It is centrifugated and is washed with ethyl alcohol and deionized water, it is dry in 60 DEG C of baking ovens, powder D is obtained, powder D is placed in porcelain crucible
In, in tube furnace with the heating rate of 2 DEG C/min in N2It is warming up to 500 DEG C under atmosphere, while calcining 3 at 500 DEG C
H is cooled to room temperature, finally obtains GC-N-TiO2.We are successful known to the X ray diffracting spectrum (Fig. 1) of catalysis material
The TiO of Anatase is synthesized2, and crystallinity with higher.It can be seen that the GC-N-TiO of synthesis from scanning electron microscope2Light
Catalyst (Fig. 3) appearance and size is similar to GC-N(Fig. 2), illustrates TiO2It can be uniformly dispersed on GC-N.From x-ray photoelectron energy
The signal peak of C-N key and C=N key and Ti-N key is able to observe that in spectrogram (Fig. 4, Fig. 5), it was demonstrated that carbon substrate and titanium dioxide
There is the doping of nitrogen.To sum up, it was demonstrated that successfully synthesize GC-N-TiO2Photochemical catalyst.
Embodiment 2
The preparation of GC-N: 5.95 g zinc nitrate hexahydrates and 6.16 g 2-methylimidazoles are added in 300 mL methanol, room temperature
24 h of lower stirring dry 8 h in 60 DEG C of baking ovens, obtain organometallic skeletal ZIF-8 after being centrifugated and being washed with methanol.
ZIF-8 is placed in porcelain crucible, in tube furnace with the heating rate of 2 DEG C/min in N2920 DEG C are warming up under atmosphere, simultaneously
In 920 DEG C of 3 h of calcining.After being cooled to room temperature, the porous carbon materials GC-N of N doping is obtained.
GC-N-TiO2Preparation: disperse 0.01 g GC-N in the dehydrated alcohol of 40mL, after 30 min of ultrasonic disperse
Solution A is formed, 2 mL ammonium hydroxide are added, 10 min is stirred at room temperature and forms solution B, then B solution is added in 1 mL isopropyl titanate
In, 20 min are persistently stirred, mixed solution C is formed, mixed solution C is transferred in ptfe autoclave liner, then will
Liner is put into autoclave, and 12 h of hydro-thermal reaction under the conditions of 140 DEG C, 0.15 Mpa after being cooled to room temperature, will be precipitated
Object is centrifugated and is washed with ethyl alcohol and deionized water, dry in 60 DEG C of baking ovens, obtains powder D, powder D is placed in porcelain crucible
In, in tube furnace with the heating rate of 2 DEG C/min in N2It is warming up to 500 DEG C under atmosphere, while in 500 DEG C of 3 h of calcining,
It is cooled to room temperature, finally obtains GC-N-TiO2。
Embodiment 3
The preparation of GC-N: 5.95 g zinc nitrate hexahydrates and 6.16 g 2-methylimidazoles are added in 300 mL methanol, room temperature
24 h of lower stirring dry 8 h in 60 DEG C of baking ovens, obtain organometallic skeletal ZIF-8 after being centrifugated and being washed with methanol.
ZIF-8 is placed in porcelain crucible, in tube furnace with the heating rate of 2 DEG C/min in N2It is warming up to 920 DEG C under atmosphere, while
920 DEG C of 3 h of calcining.After being cooled to room temperature, the porous carbon materials GC-N of N doping is obtained.
GC-N-TiO2Preparation: disperse 0.01 g GC-N in the dehydrated alcohol of 40 mL, after 30 min of ultrasonic disperse
Solution A is formed, 2 mL ammonium hydroxide are added, 10 min is stirred at room temperature and forms solution B, then B solution is added in 10 mL isopropyl titanates
In, 20 min are persistently stirred, mixed solution C is formed, mixed solution C is transferred in ptfe autoclave liner, then will
Liner is put into autoclave, and 12 h of hydro-thermal reaction under the conditions of 140 DEG C, 0.15 Mpa after being cooled to room temperature, will be precipitated
Object is centrifugated and is washed with ethyl alcohol and deionized water, dry in 60 DEG C of baking ovens, obtains powder D, powder D is placed in porcelain crucible
In, in tube furnace with the heating rate of 2 DEG C/min in N2It is warming up to 500 DEG C under atmosphere, while calcining 3 at 500 DEG C
H is cooled to room temperature, finally obtains GC-N-TiO2。
Embodiment 4
Graphene-supported TiO2Preparation: by the commercially available anatase TiO of 2 g2It is added in 400 mL deionized waters, ultrasonic disperse 30
Solution E is formed after min, 0.02 g graphene oxide is added, and 1 H-shaped of ultrasonic disperse shifts mixed solution F at mixed solution F
It is put into autoclave into ptfe autoclave liner, then by liner, is lauched in 120 DEG C, 0.15 Mpa condition
Sediment after being cooled to room temperature, is centrifugated and is washed with deionized by 12 h of thermal response, dry in 60 DEG C of baking ovens, most
Graphene-supported TiO is obtained eventually2。
Photocatalytic activity analysis: using toluene for target contaminant, and it is living to probe into photocatalysis of the catalyst under different light sources
Property.The degradation reaction of photocatalysis toluene carries out on self-control reactor, carries out degradation toluene, light intensity 200 using full spectrum
mW/cm2；The volume of reactor is 2 mL；The dosage of catalyst is 100 mg；The initial concentration of toluene is 25 ppm；Reaction gas
The flow velocity of body is 100 mL/min；Relative humidity is 60%；Reach adsorption/desorption balance through dark adsorption reaction in 3 hours, then
It turns on light；Using the concentration value with hydrogen ion flame (FID) detector Yu the gas chromatographic detection toluene of nickel reburner, experimental result
Show the TiO compound with N doping porous carbon2Material is than pure TiO2Material and graphene-supported TiO2With excellent photocatalysis
The performance of degradation toluene.The result shows that: GC-N-TiO2Photochemical catalyst is shown than pure TiO2Higher Photocatalytic Degradation of Toluene
Performance.After 24 h illumination, GC-N-TiO2Degradation of toluene rate remain at 60% or more (Fig. 6), mineralization rate is also always maintained at
In 80%(Fig. 7), and pure TiO2In illumination only 12 h just complete deactivation, and graphene-supported TiO2It is as a child active 18
It is remarkably decreased (Fig. 8).
Above embodiments be only to illustrate technical solution of the present invention and non-critical condition limitation, this field it is general
Or else logical personnel, which should be appreciated that, can deviate in the spirit and scope of the present invention defined by claims to its details or shape
Formula makes a variety of changes it.
Claims (9)
1. a kind of GC-N-TiO2The preparation method of photochemical catalyst, which is characterized in that had using organic ligand, metal salt synthesis metal
Machine skeleton, hydrolytic polymerization, washing, drying and the method for calcining are prepared in the ethanol solution containing titanium source after being carbonized
The compound catalysis material with N doping porous carbon；Specific step is as follows:
(1) preparation of MOFs: the organic ligand of 3 ~ 6 g metal salts and 4 ~ 7 g is added in the methanol of 150 ~ 300 ml, room temperature
20 ~ 24 h of lower stirring, then by solution centrifuge separation, cleaning, drying, finally obtain MOFs；The metal salt includes six hydration nitre
Sour zinc, zinc acetate or zinc sulfate；The organic ligand is 2-methylimidazole；
(2) preparation of GC-N: the MOFs of 0.1 ~ 0.3 g is added in crucible, is placed in tube furnace, in N22 ~ 4 are calcined under atmosphere
H is collected after being cooled to room temperature, can be obtained the porous carbon materials GC-N of N doping；
(3) GC-N-TiO2Preparation: the GC-N of 0.01 ~ 0.02 g is added into the dehydrated alcohol of 20 ~ 40 mL, ultrasound mix,
0 ~ 30 min is stirred at room temperature, is obtained solution A, is subsequently added into 2 ~ 5 mL ammonium hydroxide, then the titanium source of 1 ~ 10 mL is added in stirring
Solution A in, at room temperature stir 30 ~ 60 min, obtain solution B, mixed solution B be transferred to ptfe autoclave liner
In, then ptfe autoclave liner is put into autoclave, 9 ~ 13 h of hydro-thermal reaction, then by solution through centrifugation point
From, cleaning, dry, powder C is obtained, powder C is transferred to crucible and is placed in tube furnace, in N22 ~ 4h is calcined under atmosphere, finally
Up to GC-N-TiO2Photochemical catalyst；The titanium source includes butyl titanate, isopropyl titanate.
2. GC-N-TiO according to claim 12The preparation method of photochemical catalyst, which is characterized in that described in step (1)
The temperature stirred at room temperature is 25 ~ 35 DEG C, and stirring rate is 15 ~ 25 r/min.
3. GC-N-TiO according to claim 12The preparation method of photochemical catalyst, which is characterized in that described in step (1)
It is centrifugated 4000 ~ 6000 r/min of revolving speed；The washing solution is methanol or ethyl alcohol；The drying temperature is 60 ~ 80 DEG C,
Drying time is 6 ~ 8 h.
4. GC-N-TiO according to claim 12The preparation method of photochemical catalyst, which is characterized in that described in step (2)
Tube furnace calcination temperature is 900 ~ 1000 DEG C, and heating rate is 2 ~ 5 DEG C/min.
5. GC-N-TiO according to claim 12The preparation method of photochemical catalyst, which is characterized in that described in step (3)
The temperature stirred at room temperature is 25 ~ 35 DEG C, and stirring rate is 15 ~ 25 r/min.
6. GC-N-TiO according to claim 12The preparation method of photochemical catalyst, which is characterized in that described in step (3)
Hydrothermal temperature is 120 ~ 140 DEG C；The hydro-thermal reaction pressure is 0.1 ~ 0.3 MPa；The centrifuge separation revolving speed 4000 ~
6000 r/min；The washing solution is ethyl alcohol or deionized water；The drying temperature is 60 ~ 80 DEG C, and drying time is 6 ~ 8
h。
7. GC-N-TiO according to claim 12The preparation method of photochemical catalyst, which is characterized in that described in step (3)
Tube furnace calcination temperature is 450 ~ 600 DEG C, and heating rate is 2 ~ 5 DEG C/min.
8. a kind of GC-N-TiO is prepared by any one of claim 1 ~ 7 preparation method2Photochemical catalyst.
9. a kind of GC-N-TiO according to any one of claims 82Photocatalyst applications are in atmospheric volatile organic compounds degradation and water pollution control
Field processed.
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