CN109772401A - A kind of carbocyclic ring/carbonitride/composite titania material, preparation method and application - Google Patents
A kind of carbocyclic ring/carbonitride/composite titania material, preparation method and application Download PDFInfo
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- CN109772401A CN109772401A CN201910035791.4A CN201910035791A CN109772401A CN 109772401 A CN109772401 A CN 109772401A CN 201910035791 A CN201910035791 A CN 201910035791A CN 109772401 A CN109772401 A CN 109772401A
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Abstract
A kind of carbocyclic ring/carbonitride/composite titania material, the material are combined by carbocyclic ring, carbonitride, titanium dioxide；The carbocyclic ring is fixed in the planar structure of carbonitride, and the titanium dioxide deposition contacts carbocyclic ring and carbonitride simultaneously maximum probability in nitridation carbon surface to realize the ternary heterojunction contact of sufficient carbocyclic ring, carbonitride, titanium dioxide.Preparation method includes: that melamine powder and quadracycline are added in the crucible for filling ultrapure water by (1), stirring, ultrasound；Drying, calcining, obtains the nitridation carbon complex for being fixed with the carbocyclic ring；(2) compound that step (1) synthesizes is mixed and is ground with titanium dioxide granule, calcined, obtain carbocyclic ring/carbonitride/composite titania material.The application of carbocyclic ring/carbonitride/composite titania material organic pollutant in degradation water environment.The method of the present invention simple process, low in cost, the period is short, environmental-friendly, can be adapted for industrialization large-scale production.
Description
Technical field
The invention belongs to environmental protection technical field, be related to can enhancing the carbocyclic ring of photocatalysis degradation organic contaminant performance/
Carbonitride/composite titania material preparation method and application.
Background technique
With the high speed development of economic society, water pollution problems is got worse.In recent years, Photocatalitic Technique of Semiconductor is in water
Research and application in terms of environmental improvement cause the extensive concern of people.Wherein, graphitic carbon carbonitride (g-C3N4), as one
The nonmetallic visible light-responded material of kind, inexpensive, stable structure is environmental-friendly, chemical composition and band structure regulation side
Just, in recent years its in terms of application cause extensive concern.However, g-C3N4Material is also deposited
In some stern challenges: specific surface area is small, it is compound to generate the exciton binding energy of photo-generated carrier height, photo-generate electron-hole
Seriously, low, visible light utilization ratio deficiency of quantum efficiency etc., seriously restricts it in the large-scale promotion application of photocatalysis field
(see document G.Mamba, A.K.Mishra, Applied Catalysis B:Environmental, 198 (2016) 347-
377.)。
Therefore, to pure g-C3N4It is modified and makes it have more excellent and stable photocatalysis performance and seem particularly necessary.
Common method of modifying has an element doping, combined polymerization, structure design, hetero-junctions engineering etc. (see document W.J.Ong,
L.L.Tan,Y.H.Ng,S.T.Yong,S.P.Chai,Chemical Review,116(2016)7159-7329.).Wherein, different
Matter knot strategy can effectively solve the above problem, especially ternary or multi-element heterogeneous knot.Carbon material is special because of its excellent electronics transfer
Property plays an important role in ternary heterojunction system based on by carbonitride.But carbon containing carbonitride common at present
Base ternary heterojunction construction method, be by carbon material directly and the semiconductors couplings, such as g-C such as carbonitride3N4/nanocarbon/
ZnIn2S4(F.Shi, L.Chen, M.Chen, D.Jiang, Chem.Commun.51 (2015) 17144-17147.), when
ZnIn2S4With g-C3N4When contact, it not necessarily can guarantee maximum probability while touching nanocarbon, thus it is relatively difficult to achieve sufficiently high
The ternary heterojunction interfacial contact of effect.If can sufficiently improve the interfacial contact of ternary heterojunction, it can effectively enhance composite wood
The photocatalysis performance of material and the application in environmental improvement protection.
Summary of the invention
The purpose of the present invention is to provide a kind of carbocyclic ring/carbonitride/composite titania material, preparation method and answer
With the material is able to achieve sufficiently efficient ternary heterojunction contact, overcomes aforesaid drawbacks of the existing technology.
To achieve the goals above, this invention takes the following technical solutions:
A kind of carbocyclic ring/carbonitride/composite titania material (Carbon-ring/g-C3N4/TiO2, CCNT), the material
By carbocyclic ring (Carbon-ring, C), carbonitride (g-C3N4, CN), titanium dioxide (TiO2, T) and it is combined.Wherein, the carbocyclic ring
Be fixed in the planar structure of carbonitride, the titanium dioxide is once deposited on nitridation carbon surface, can maximum probability simultaneously
Carbocyclic ring and carbonitride are contacted, to realize the ternary heterojunction contact of sufficient carbocyclic ring, carbonitride, titanium dioxide.
The carbocyclic ring/carbonitride/composite titania material preparation method, includes the following steps composition:
(1) a certain amount of melamine powder is added in the crucible for filling quadracycline solution, is filled at room temperature
Divide stirring, then ultrasound a period of time.Above-mentioned crucible is placed into an oven sufficiently drying again, then crucible is placed in Muffle furnace
It is calcined, cooled to room temperature and is fully ground the nitridation carbon complex for having inlayed the carbocyclic ring to obtain the final product after calcining
(CCN)。
(2) compound that step (1) synthesizes is uniformly mixed and is fully ground with a certain amount of titanium dioxide granule, then will
This mixture, which is placed in Muffle furnace, to be calcined, and cooled to room temperature is after calcining up to carbocyclic ring/carbonitride/titanium dioxide
Composite material (CCNT).
Wherein: the mass ratio of melamine and quadracycline is 1:0.01~1:0.09.
Ultrapure water volume is 40-60mL, mixing time 30-60min, ultrasonic time 30-60min.Oven temperature is
45-75 DEG C, drying time 12-24h, calcination procedure are as follows: 300 DEG C of heat preservations 1h, 400 DEG C of heat preservations 1h, 550 DEG C of heat preservation 4h, grinding
Time is 20-60min.The quality of compound (CCN) described in step (2) and titanium dioxide mass ratio are 1:0.5-1:2, optional
Ground, the quality and titanium dioxide mass ratio of the compound (CCN) are 1:1；, milling time 20-60min.
Carbocyclic ring/carbonitride/composite titania material is as photochemical catalyst in photocatalytic degradation water prepared by the present invention
Application in middle organic pollutant.
Carbocyclic ring/carbonitride/the composite titania material is mixed with the waste water of organic pollutant, is placed in dark surrounds
Mixed solution is then placed in visible light environment until reaching adsorption equilibrium and carries out light-catalyzed reaction by middle stirring, completes to water
The degradation of middle organic pollutant.The organic pollutant is methylene blue, and mixing time is 20-60min under the dark surrounds,
The time of the light-catalyzed reaction is 90-120min.
By adopting the above-described technical solution, the beneficial effects of the present invention are:
(1) present invention has synthesized carbocyclic ring/carbonitride/titanium dioxide tri compound catalysis material, synthetic method work for the first time
Skill condition is simple, be not necessarily to complex device, the period is short, feasibility is strong, and the material synthesized catalytic environment can have under visible light
Machine contaminant degradation has good environmental protection application prospect.
(2) pass through radiation of visible light 90min through carbocyclic ring/carbonitride/composite titania material prepared by the present invention, to Asia
The degradation rate of methyl blue can reach 98.6%, and intending level-one degradation rate constant is 0.0441min-1, compared to being prepared under the same terms
Simple graphite phase carbon nitride improve 54.13 times.
(3) present invention prepares carbocyclic ring/carbonitride/composite titania material preparation method, and it is sufficiently high to use building
The strategy of the ternary heterojunction contact of effect promotes Pair production to separate, and promotes electronics transfer, enhances visible absorption range,
The thinking of photocatalysis performance to improve catalyst can be promoted in photocatalytic environmental-protection technical field.
Detailed description of the invention
A figure is the scanning electron microscope of the heterojunction interface amplification of composite material prepared by the embodiment of the present invention 3 in Fig. 1
Figure；B figure is the X-ray energy spectrum analysis chart of composite material prepared by the embodiment of the present invention 3；C figure is 2 material prepared of comparative example
Transmission electron microscope picture；D figure is the high-resolution map of c figure material, and rectangle frame indicates the region for having nitridation carbon structure, and oval frame indicates
Has carbon structure region.
Fig. 2 is the X-ray diffractogram of 1-5 of the embodiment of the present invention, 2,4,5 material prepared of comparative example.
Fig. 3 is the FTIR spectrum figure of the embodiment of the present invention 4,2,4,5 material prepared of comparative example.
Fig. 4 is 1-5 of the embodiment of the present invention, comparative example 1-5 material prepared photocatalytic degradation methylene blue under visible light
Degradation effect figure.
Fig. 5 is 1-5 of the embodiment of the present invention, comparative example 1-5 material prepared photocatalytic degradation methylene blue under visible light
Quasi- first order kinetics degradation rate constant and TOC removal rate figure.
Specific embodiment
Below in conjunction with attached drawing, embodiment, the present invention is further illustrated.
Embodiment 1
(1) melamine powder of 10g and 0.1g quadracycline are added in the crucible for filling 50mL ultrapure water,
30min, then ultrasound 30min are sufficiently stirred at room temperature.Above-mentioned crucible is placed into 60 DEG C of baking 12h in an oven again, then by crucible
It is placed in Muffle furnace and is calcined, calcination procedure are as follows: 300 DEG C of heat preservation 1h, 400 DEG C of heat preservation 1h, 550 DEG C of heat preservation 4h, calcining terminate
It cooled to room temperature and is fully ground 30min afterwards and obtains the composite nitride carbon (1-CCN) for being fixed with the carbon.
(2) compound (0.20g) that step (1) synthesizes is uniformly mixed with titanium dioxide granule (0.20g) and is sufficiently ground
Grind 30min, then this mixture be placed in 450 DEG C of calcining 1h in Muffle furnace, after calcining cooled to room temperature up to carbocyclic ring/
Carbonitride/composite titania material (1-CCNT-50).
(3) 1-TCNT-50 of 50mg is mixed with the methylene blue solution that 50mL concentration is 10mg/L, is placed in dark surrounds
Solution is then placed in progress light-catalyzed reaction 90min, the as a result degradation of methylene blue in visible light environment by middle stirring 30min
Rate is 86.6%, and intending level-one degradation rate constant is 0.0218min-1, total organic carbon (TOC) removal rate is 42.2%.
Embodiment 2
The melamine powder of 10g and 0.3g quadracycline are added in the crucible for filling 50mL ultrapure water, other
Operation is 92.7% to the degradation rate of 10mg/L methylene blue with embodiment 1, gained composite material (3-CCNT-50), intends level-one
Degradation rate constant is 0.0286min-1, TOC removal rate is 66.9%.
Embodiment 3
The melamine powder of 10g and 0.5g quadracycline are added in the crucible for filling 50mL ultrapure water, other
Operation is 92.5% to the degradation rate of 10mg/L methylene blue with embodiment 1, gained composite material (5-CCNT-50), intends level-one
Degradation rate constant is 0.0259min-1, TOC removal rate is 66.5%.
Embodiment 4
The melamine powder of 10g and 0.7g quadracycline are added in the crucible for filling 50mL ultrapure water, other
Operation is 98.6% to the degradation rate of 10mg/L methylene blue with embodiment 1, gained composite material (7-CCNT-50), intends level-one
Degradation rate constant is 0.0441min-1, TOC removal rate is 80.3%.
Embodiment 5
The melamine powder of 10g and 0.9g quadracycline are added in the crucible for filling 50mL ultrapure water, other
Operation is 76.3% to the degradation rate of 10mg/L methylene blue with embodiment 1, gained composite material (9-CCNT-50), intends level-one
Degradation rate constant is 0.0134min-1, TOC removal rate is 54.5%.
Comparative example 1
The melamine powder of 10g is added in sky crucible, crucible is placed in Muffle furnace and is calcined, calcination procedure
Are as follows: 300 DEG C of heat preservations 1h, 400 DEG C of heat preservations 1h, 550 DEG C of heat preservation 4h cooled to room temperature and are fully ground after calcining
30min obtains graphite phase carbon nitride (CN), this graphite phase carbon nitride (0.20g) is mixed with titanium dioxide granule (0.20g)
It is even and be fully ground 30min, then this mixture is placed in 450 DEG C of calcining 1h in Muffle furnace, room is naturally cooled to after calcining
Temperature is up to composite material (CN/TiO2).By the CN/TiO of 50mg2It mixes, sets with the methylene blue solution that 50mL concentration is 10mg/L
30min is stirred in dark surrounds, and solution is then placed in progress light-catalyzed reaction 90min, the material pair in visible light environment
The degradation rate of 10mg/L methylene blue is 50.4%, and intending level-one degradation rate constant is 0.0058min-1, TOC removal rate is
27.0%.
Comparative example 2
The melamine powder of 10g and 0.7g quadracycline are added in the crucible for filling 50mL ultrapure water, in room
30min, then ultrasound 30min are sufficiently stirred under temperature.Above-mentioned crucible is placed into 60 DEG C of baking 12h in an oven again, then sets crucible
It is calcined in Muffle furnace, calcination procedure are as follows: 300 DEG C of heat preservations 1h, 400 DEG C of heat preservations 1h, 550 DEG C of heat preservation 4h, after calcining
Cooled to room temperature is simultaneously fully ground 30min, obtains the carbon nitride material (7-CCN) for being fixed with carbon, by the 7-CCN of 50mg with
The methylene blue solution that 50mL concentration is 10mg/L mixes, and is placed in dark surrounds and stirs 30min, is then placed in solution visible
Light-catalyzed reaction 90min is carried out in luminous environment, as a result the degradation rate of methylene blue is 33.7%, and quasi- level-one degradation rate constant is
0.0027min-1, TOC removal rate is 15.4%.
Comparative example 3
The titania powder of 0.40g and 0.7g quadracycline are added in the crucible for filling 50mL ultrapure water,
30min, then ultrasound 30min are sufficiently stirred at room temperature.Above-mentioned crucible is placed into 60 DEG C of baking 12h in an oven again, then by crucible
It is placed in Muffle furnace and is calcined, calcination procedure are as follows: 300 DEG C of heat preservation 1h, 400 DEG C of heat preservation 1h, 550 DEG C of heat preservation 4h, calcining terminate
Cooled to room temperature and it is fully ground 30min afterwards, obtains material C/TiO2, by the C/TiO of 50mg2It is 10mg/ with 50mL concentration
The methylene blue solution of L mixes, and is placed in dark surrounds and stirs 30min, then solution is placed in visible light environment and carries out light
Catalysis reaction 90min, as a result the degradation rate of methylene blue is 79.0%, and intending level-one degradation rate constant is 0.0143min-1, TOC
Removal rate is 38.0%.
Comparative example 4
The titania powder of 0.40g is added in sky crucible, 450 DEG C of calcining 1h in Muffle furnace is placed in, obtains material
TiO2, by the TiO of 50mg2It is mixed with the methylene blue solution that 50mL concentration is 10mg/L, is placed in dark surrounds and stirs 30min,
Solution is then placed in progress light-catalyzed reaction 90min in visible light environment, as a result the degradation rate of methylene blue is 72.3%, is intended
Level-one degradation rate constant is 0.0134min-1, TOC removal rate is 35.5%.
Comparative example 5
The melamine powder of 10g is added in sky crucible, then crucible is placed in Muffle furnace and is calcined, is calcined
Program are as follows: 300 DEG C of heat preservations 1h, 400 DEG C of heat preservations 1h, 550 DEG C of heat preservation 4h cooled to room temperature and are fully ground after calcining
30min obtains graphite phase carbon nitride material (CN), and the methylene blue solution that the CN of 50mg and 50mL concentration is 10mg/L is mixed
It closes, is placed in dark surrounds and stirs 30min, solution is then placed in progress light-catalyzed reaction 90min in visible light environment, as a result
The degradation rate of methylene blue is 18.0%, and intending level-one degradation rate constant is 0.0008min-1, TOC removal rate is 4.8%.
Material of the present invention is combined by carbocyclic ring, carbonitride, titanium dioxide, wherein the carbocyclic ring is fixed on carbonitride
Planar structure in, the titanium dioxide is once deposited on nitridation carbon surface, can maximum probability simultaneously contact carbon and carbonitride,
To realize the ternary heterojunction contact of sufficient carbocyclic ring, carbonitride, titanium dioxide.This strategy effectively promotes electronics and turns
Move, it is suppressed that photo-generate electron-hole it is compound, while the response range of visible light is enhanced, to improve photocatalysis performance.
Finally formed carbocyclic ring/carbonitride/composite titania material, under suitable process conditions, compared to original graphite-phase nitrogen
Change carbon, the rate of degradable organic pollutant improves 54.13 times.In addition, the method for the present invention simple process, low in cost, all
Phase is short, environmental-friendly, can be adapted for industrialization large-scale production.
The above-mentioned description to embodiment is that this hair can be understood and applied for the ease of those skilled in the art
It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to implementations here
Example, those skilled in the art's announcement according to the present invention, the improvement made for the present invention and modification all should be of the invention
Within protection scope.
Claims (13)
1. a kind of carbocyclic ring/carbonitride/composite titania material, it is characterised in that: the material is by carbocyclic ring, carbonitride, titanium dioxide
Titanium is combined；Wherein, the carbocyclic ring is fixed in the planar structure of carbonitride, and the titanium dioxide deposition is in carbonitride table
Face contacts carbocyclic ring and carbonitride simultaneously maximum probability to realize the ternary heterojunction of sufficient carbocyclic ring, carbonitride, titanium dioxide
Contact.
2. carbocyclic ring described in claim 1/carbonitride/composite titania material preparation method, characterized by comprising:
(1) melamine powder to match and quadracycline are added in the crucible for filling ultrapure water, are filled at room temperature
Divide stirring, then carries out ultrasound；Above-mentioned crucible is placed into an oven sufficiently drying again, then crucible is placed in Muffle furnace and is carried out
Calcining cooled to room temperature and is fully ground the nitridation carbon complex for being fixed with the carbocyclic ring to obtain the final product after calcining；
(2) compound that step (1) synthesizes is uniformly mixed and is fully ground with the titanium dioxide granule to match, then this is mixed
Conjunction object, which is placed in Muffle furnace, to be calcined, and cooled to room temperature is compound up to carbocyclic ring/carbonitride/titanium dioxide after calcining
Material.
3. carbocyclic ring/carbonitride/composite titania material preparation method according to claim 2, it is characterised in that: trimerization
The mass ratio of cyanamide and quadracycline is 1:0.01~1:0.09.
4. carbocyclic ring/carbonitride/composite titania material preparation method according to claim 2, it is characterised in that: ultrapure
Water volume is 40-60mL, mixing time 30-60min, ultrasonic time 30-60min.
5. carbocyclic ring/carbonitride/composite titania material preparation method according to claim 2, it is characterised in that: baking oven
Temperature is 45-75 DEG C, drying time 12-24h.
6. carbocyclic ring/carbonitride/composite titania material preparation method according to claim 2, it is characterised in that calcining
Program are as follows: 300 DEG C of heat preservations 1h, 400 DEG C of heat preservations 1h, 550 DEG C of heat preservation 4h.
7. carbocyclic ring/carbonitride/composite titania material preparation method according to claim 2, it is characterised in that: grinding
Time is 20-60min.
8. carbocyclic ring/carbonitride/composite titania material preparation method according to claim 2, it is characterised in that: step
(2) compound described in and titanium dioxide mass ratio are 1:0.5-1:2.
9. carbocyclic ring/carbonitride/composite titania material preparation method according to claim 2, it is characterised in that: step
(2) compound described in and titanium dioxide mass ratio are 1:1.
10. carbocyclic ring/carbonitride/composite titania material preparation method according to claim 2, it is characterised in that: horse
Not calcination temperature is 400-450 DEG C in furnace, soaking time 1-2h.
11. a kind of organic contamination in degradation water environment of carbocyclic ring/carbonitride/composite titania material described in claim 1
The application of object.
12. application according to claim 11, which comprises the following steps: by the composite material with it is organic
The waste water of pollutant mixes, and is placed in dark surrounds and stirs, until reaching adsorption equilibrium, mixed solution is then placed in visible light
Light-catalyzed reaction is carried out in environment, completes the degradation to organic pollutants.
13. application according to claim 12, which is characterized in that the organic pollutant is methylene blue, the dark
Mixing time is 20-60min under environment, and the time of the light-catalyzed reaction is 90-120min.
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