CN105289693B - A kind of Zn0.5Co0.5Fe2O4/g‑C3N4The preparation method of composite photo-catalyst - Google Patents
A kind of Zn0.5Co0.5Fe2O4/g‑C3N4The preparation method of composite photo-catalyst Download PDFInfo
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Abstract
The invention belongs to technical field of environment function material preparation, and in particular to a kind of Zn0.5Co0.5Fe2O4/g‑C3N4The preparation method of composite photo-catalyst.The present invention uses hydro-thermal method technology of preparing, first calcines melamine powder, obtains g C3N4Nanometer sheet, prepares g C3N4Nanometer sheet suspension, adds a certain amount of Fe (NO3)3·9H2O solids, Zn (NO3)2·6H2O solids, Co (NO3)2·6H2O solids, tartaric acid solid, NaOH solids, then move to solution in polytetrafluoroethylene (PTFE) in the reactor in village, 160 ~ 200 DEG C of 12 ~ 24h of reaction, wash, dry, obtain Zn0.5Co0.5Fe2O4/g‑C3N4Composite photo-catalyst.The present invention builds a composite visible light photocatalytic system;The absorption region of visible ray is enhanced by forming heterojunction structure, catalyst photocatalytic activity in visible region is enhanced.
Description
Technical field
The present invention relates to a kind of Zn0.5Co0.5Fe2O4/g-C3N4The preparation method of composite photo-catalyst, belongs to environmental functional material
Expect preparing technical field.
Background technology
Environmental pollution and energy shortage are the world today's two big subject matters urgently to be resolved hurrily.Photocatalysis is used as a kind of green
Technology carries out environmental pollution there is provided the thorough elimination potential effective approach of toxic chemical with natural solar energy source is utilized
The double action of improvement, novel photocatalyst of the exploitation with visible light activity turns into an important research topic.
The metal composite oxide of spinel structure is special due to its structure, with many performances, metallurgy, electronics,
The fields such as chemical industry all have been widely used, and can be used as magnetic material, absorbing material, sensing material, battery cathode material
With high temperature engineering material etc..In addition they or the important catalyst of a class, its energy gap is about 1.9eV, can be with
Solar energy is effectively utilized, therefore can build and prepare the new ferrite photochemical catalyst sensitive to visible ray.g-C3N4It is one
Non-metal semiconductive is planted, the more C of content, N element are constituted on the earth, the eV of band gap about 2.7, there is certain suction to visible ray
Receive, antiacid, alkali, the corrosion of light, stability are good, structure and performance are easy to regulation and control, with preferable photocatalytic.Semiconductors coupling
Modification be by low energy gap gap semiconductor with wait wide band gap semiconducter energy level be harmonious, to extend the spectrum of wide band gap semiconducter
Response range, improves a kind of effective means of solar energy utilization ratio.
Analyzed based on more than, with reference to Zn0.5Co0.5Fe2O4And g-C3N4The respective advantage of material, is prepared using hydro-thermal method
Zn0.5Co0.5Fe2O4/g-C3N4Composite photo-catalyst, can greatly improve its absorption region under visible light, extension electricity
Catalytic performance under son-hole-recombination speed, more favourable visible ray, and stability is stronger, while there is very strong magnetic, easily
In recycling.
The content of the invention
Present invention aims at having used a kind of gentle easy hydro-thermal method to prepare method, a kind of ferromagnetism is prepared for(Easily return
Receive and utilize)Efficient Zn0.5Co0.5Fe2O4/g-C3N4(Zinc ferrite cobalt/graphite type carbon nitride)Composite photo-catalyst.Structure of the present invention
Build a composite visible light photocatalytic system;The absorption region of visible ray is enhanced by forming heterojunction structure, this is enhanced
Catalyst photocatalytic activity in visible region.
Technical scheme is as follows:
A kind of Zn0.5Co0.5Fe2O4/g-C3N4The preparation method of composite photo-catalyst, is carried out according to the following steps:
(1)Weigh melamine solid and put in crucible, close the lid, and crucible band lid is put into Muffle furnace together
In, temperature-programmed reaction obtains g-C3N4Nanometer sheet;
(2)Take step(1)In g-C3N4Nanometer sheet sample is ground, and weighs g-C3N4Nanometer sheet ultrasonic disperse is in deionization
In water, g-C is made3N4Nanometer sheet suspension;
(3)Weigh Fe (NO3)3·9H2O solids, Zn (NO3)2·6H2O solids and Co (NO3)2·6H2O solids are added to
Dissolving forms mixed solution in ionized water, with step(2)Middle suspension is well mixed, and increases magnetic agitation rotating speed, continues to stir
It is set fully to react;It is slowly added to L (+) tartaric acid solid thereto again, is slowly added to after finishing, continuing stirring makes its abundant
Reaction;It is slowly added to NaOH solids thereto again, increases magnetic agitation rotating speed, continuing stirring makes it fully react, and stirs;
Mixed liquor is transferred to after being reacted in reactor and obtains solid product, washed with brand-new deionized water and ethanol, be dried in vacuo, obtain
To Zn0.5Co0.5Fe2O4/g-C3N4Composite photo-catalyst.
Step(1)In, the Muffle furnace temperature-programmed reaction condition is 2 ~ 6 DEG C of min-1Rate program is warming up to 550 ~
600 DEG C of 4 ~ 6h of reaction;
Step(2)In, the g-C3N4The concentration of nanometer sheet suspension is 0.06-0.1g/mL.
Step(3)In, Fe (NO in the mixed solution3)3·9H2O, Zn (NO3)2·6H2O, Co (NO3)2·6H2O, L
(+) tartaric acid, the mass ratio of NaOH solids is 4.04 ~ 8.08g:0.74~1.48g:0.75~1.49g:1.92~3.84g:2.2~
4.4g;Wherein, Fe (NO in mixed solution3)3·9H2O substance withdrawl syndrome is 0.1-0.2g/mL.
Step(3)In, the time that L (+) the tartaric acid solid, NaOH solids are slowly added to is 1min ~ 10min;Often
Adding a kind of reaction raw materials continuation stirring makes its sufficient reaction time be 10min ~ 60min.
It is 160 ~ 200 DEG C of 12 ~ 24h of reaction that the mixed liquor, which is transferred to the condition of reactor,.
Wherein step(3)Deionized water and ethanol respectively washing three times, the vacuum drying are dried at less than 100 DEG C.
The technological merit of the present invention:
(1)Composite photo-catalyst crystallization purity obtained by hydro-thermal method employed in the present invention is high, without it is numerous and diverse one by one
Each monomer is prepared to be combined again, and reaction condition is gentle in preparation process, is not required to prepare composite catalyst by high-temperature calcination,
Effectively avoid zinc ferrite crystal type in pyroprocess to change and cause magnetic to weaken, so as to cause to reclaim difficult;
(2)Composite photo-catalyst performance prepared by the present invention is better than the general composite catalyzing prepared by material of zinc ferrite
Agent.With narrow-band semiconductor material Zn0.5Co0.5Fe2O4Pass through hydro-thermal method simple and easy to apply and broadband material g-C3N4Compound preparation can
See photochemical catalyst, be not only visible light catalyst and possess ferromagnetism, be conducive to recycling, reduce cost, environmental protection;And
Due to Zn0.5Co0.5Fe2O4With g-C3N4Level of energy matching is fine, and electro transfer and free radical can be promoted to generate after being combined,
Photochemical catalyst is improved to absorb and photocatalytic activity and g-C in visible region3N4Stability.
Brief description of the drawings
The technology of the present invention is further described with reference to the accompanying drawings and examples.
The g-C of Fig. 1 present invention3N4 , Zn0.5Co0.5Fe2O4And Zn0.5Co0.5Fe2O4/g-C3N4Composite photo-catalyst XRD
Figure.
The Zn of Fig. 2 present invention0.5Co0.5Fe2O4(a)And Zn0.5Co0.5Fe2O4/g-C3N4(b)Composite photo-catalyst TEM schemes.
The g-C of Fig. 3 present invention3N4 , Zn0.5Co0.5Fe2O4And Zn0.5Co0.5Fe2O4/g-C3N4Composite photo-catalyst is ultraviolet
Diffuse spectrogram.
The g-C of Fig. 4 present invention3N4 , Zn0.5Co0.5Fe2O4And Zn0.5Co0.5Fe2O4/g-C3N4Composite photo-catalyst light drops
Solve design sketch.
The g-C of Fig. 5 present invention3N4 , Zn0.5Co0.5Fe2O4And Zn0.5Co0.5Fe2O4/g-C3N4Composite photo-catalyst is reclaimed
Light degradation design sketch.
Embodiment
With reference to specific implementation example, the present invention will be further described.
A kind of Zn0.5Co0.5Fe2O4/g-C3N4The preparation method of composite photo-catalyst, is carried out according to the following steps:
(1)Weigh melamine solid and put in crucible, close the lid, and crucible band lid is put into Muffle furnace together
In, temperature-programmed reaction obtains g-C3N4Nanometer sheet;
(2)Take step(1)In g-C3N4Nanometer sheet sample is ground, and weighs g-C3N4Nanometer sheet ultrasonic disperse is in deionization
In water, g-C is made3N4Nanometer sheet suspension;
(3)Weigh Fe (NO3)3·9H2O solids, Zn (NO3)2·6H2O solids and Co (NO3)2·6H2O solids are added to
Dissolved in ionized water, with step(2)Middle suspension is well mixed, and increases magnetic agitation rotating speed, continues to react;It is slow thereto again
L (+) tartaric acid solid is added, is slowly added to after finishing, continuing stirring makes it fully react;It is slowly added to NaOH thereto again
Solid, increases magnetic agitation rotating speed, and continuing stirring makes it fully react, and stirs;Mixed liquor is transferred in reactor instead
Should after obtain solid product, washed with deionized water and ethanol, vacuum drying obtain Zn0.5Co0.5Fe2O4/g-C3N4Complex light is urged
Agent.
Photocatalysis performance is evaluated:Carried out in light-catalyzed reaction instrument, Zn prepared by the above method0.5Co0.5Fe2O4/g-
C3N4Composite photo-catalyst is used in the antibiotic photocatalytic degradation in water, and carries out recycling to the catalyst after catalysis.
Embodiment 1:
(1)Weigh melamine solid 10.0g and put in 50mL crucibles, close the lid, and crucible band lid is put together
Enter in Muffle furnace, Muffle furnace temperature-programmed reaction condition is 5 DEG C of min-1Rate program is warming up to 550 DEG C, and keeping temperature is constant
React 4h;Natural cooling obtains g-C3N4Nanometer sheet;
(2)Take step(1)In g-C3N4Nanometer sheet sample is ground, and weighs g-C3N4Nanometer sheet 1.84g, ultrasonic disperse,
In 20mL deionized waters, g-C is made3N4Nanometer sheet suspension;
(3)Weigh Fe (NO3)3·9H2O solid 4.04g, Zn (NO3)2·6H2O solid 0.74g and Co (NO3)2·6H2O consolidates
Body 0.75g, which is added in 40mL deionized waters, to be dissolved, with step(2)Middle suspension is well mixed, and increases magnetic agitation rotating speed, after
Continuous reaction 10min;It is slowly added to L (+) tartaric acid solid 1.92g thereto again, is slowly added to after finishing, continuing stirring makes it
Fully reaction;It is slowly added to NaOH solid 4.4g thereto again, increases magnetic agitation rotating speed, continuing stirring makes it fully react
30min, stirs;Mixed liquor is transferred to after reacting 24h in 180 DEG C of reactors and obtains solid product, with deionized water and
Ethanol is respectively washed three times, and 60 DEG C of vacuum is dried to obtain sample, and grinding obtains powdered Zn0.5Co0.5Fe2O4/g-C3N4Complex light is urged
Agent.
The XRD of obtained sample is as shown in figure 1, as can be seen from the figure Zn0.5Co0.5Fe2O4The θ of characteristic diffraction peak 2=
30.3 °, 35.5 °, 37.1 °, 43.2 °, 53.6 °, 57.3 °, 62.8 ° and g-C3N4θ=13.0 ° of characteristic diffraction peak 2,27.3 °,
Zn0.5Co0.5Fe2O4/g-C3N4Zn can be seen in composite photo-catalyst XRD spectrum simultaneously0.5Co0.5Fe2O4And g-C3N4Feature
Diffraction maximum.
The TEM of obtained sample is schemed as shown in Fig. 2 g-C3N4For flaky substance, such as Fig. 2 (a) is shown
Zn0.5Co0.5Fe2O4TEM figures, it can be seen that for the particulate of spheroid or cube, the Zn as shown in Fig. 2 (a)0.5Co0.5Fe2O4/g-
C3N4Composite photo-catalyst TEM collection of illustrative plates, it can be seen that have the particle growth of spheroid or cube in laminated structure, furtherly
Bright Zn0.5Co0.5Fe2O4And g-C3N4It is combined successfully.
The UV Diffuse Reflectance Spectroscopy of obtained sample is as shown in figure 3, as can be seen from the figure g-C3N4Nanometer sheet is 300nm-
There are preferable absorption, Zn between 480nm0.5Co0.5Fe2O4There are stronger absorption, Zn in whole region0.5Co0.5Fe2O4/
g-C3N4Composite photo-catalyst has preferable absorption in whole region, especially in visible region(420nm-700nm)Inhale
Receive stronger, therefore Zn0.5Co0.5Fe2O4/g-C3N4Composite photo-catalyst can preferably degrade rhodamine under visible light illumination
B dyestuffs.
Embodiment 2:
(1)Weigh melamine solid 6.0g and put in 50mL crucibles, close the lid, and crucible band lid is put into together
In Muffle furnace, Muffle furnace temperature-programmed reaction condition is 5 DEG C of min-1Rate program is warming up to 550 DEG C, and keeping temperature is constant anti-
Answer 4h;Natural cooling obtains g-C3N4Nanometer sheet;
(2)Take step(1)In g-C3N4Nanometer sheet sample is ground, and weighs g-C3N4Nanometer sheet 1.84g, ultrasonic disperse,
In 20mL deionized waters, g-C is made3N4Nanometer sheet suspension;
(3)Weigh Fe (NO3)3·9H2O solid 4.04g, Zn (NO3)2·6H2O solid 0.74g and Co (NO3)2·6H2O consolidates
Body 0.75g, which is added in 40mL deionized waters, to be dissolved, with step(2)Middle suspension is well mixed, and increases magnetic agitation rotating speed, after
Continuous reaction 10min;It is slowly added to L (+) tartaric acid solid 1.92g thereto again, is slowly added to after finishing, continuing stirring makes it
Fully reaction;It is slowly added to NaOH solid 4.4g thereto again, increases magnetic agitation rotating speed, continuing stirring makes it fully react
30min, stirs;Mixed liquor is transferred to after reacting 24h in 180 DEG C of reactors and obtains solid product, with deionized water and
Ethanol is respectively washed three times, and 60 DEG C of vacuum is dried to obtain sample, and grinding obtains powdered Zn0.5Co0.5Fe2O4/g-C3N4Complex light is urged
Agent.
Embodiment 3:
(1)Weigh melamine solid 10.0g and put in 50mL crucibles, close the lid, and crucible band lid is put together
Enter in Muffle furnace, Muffle furnace temperature-programmed reaction condition is 5 DEG C of min-1Rate program is warming up to 550 DEG C, and keeping temperature is constant
React 4h;Natural cooling obtains g-C3N4Nanometer sheet;
(2)Take step(1)In g-C3N4Nanometer sheet sample is ground, and weighs g-C3N4Nanometer sheet 0.92g, ultrasonic disperse,
In 20mL deionized waters, g-C is made3N4Nanometer sheet suspension;
(3)Weigh Fe (NO3)3·9H2O solid 4.04g, Zn (NO3)2·6H2O solid 0.74g and Co (NO3)2·6H2O consolidates
Body 0.75g, which is added in 40mL deionized waters, to be dissolved, with step(2)Middle suspension is well mixed, and increases magnetic agitation rotating speed, after
Continuous reaction 10min;It is slowly added to L (+) tartaric acid solid 1.92g thereto again, is slowly added to after finishing, continuing stirring makes it
Fully reaction;It is slowly added to NaOH solid 4.4g thereto again, increases magnetic agitation rotating speed, continuing stirring makes it fully react
30min, stirs;Mixed liquor is transferred to after reacting 24h in 180 DEG C of reactors and obtains solid product, with deionized water and
Ethanol is respectively washed three times, and 60 DEG C of vacuum is dried to obtain sample, and grinding obtains powdered Zn0.5Co0.5Fe2O4/g-C3N4Complex light is urged
Agent.
Embodiment 4
Weigh obtained g-C during 0.02g implements 13N4Nanometer sheet, Zn0.5Co0.5Fe2O4、Zn0.5Co0.5Fe2O4/g-C3N4It is multiple
Closing light catalyst carries out degradation experiment using light-catalyzed reaction instrument, observes what different catalysts were degraded to rhdamine B with this
Catalytic action, the light degradation design sketch of the rhodamine B degradation dyestuff of Fig. 4 addition different catalysts, as can be seen from the figure sieve
More stable, substantially unchanged, prepared Zn under illumination in red bright B dyestuffs blank test0.5Co0.5Fe2O4Rhodamine B degradation contaminates
The degradation rate of material only has 9.6%, g-C3N4 The degradation rate of rhodamine B degradation dyestuff has 68.8%, and Zn0.5Co0.5Fe2O4/g-
C3N4The degradation rate of composite photo-catalyst is up to 90.2%, so that the photocatalysis effect of the composite catalyst of explanation is best.
Embodiment 5:
The Zn that will be thrown in light degradation in embodiment 40.5Co0.5Fe2O4、Zn0.5Co0.5Fe2O4/g-C3N4Composite photocatalyst
Agent is reclaimed, and is washed with deionized respectively after drying, and the Zn of 0.02g recovery is weighed respectively0.5Co0.5Fe2O4、
Zn0.5Co0.5Fe2O4/g-C3N4Composite photo-catalyst carries out degradation experiment using light-catalyzed reaction instrument, and above-mentioned experiment is reclaimed again
In catalyst do second of recovery experiment, once analogize five times altogether, keep other conditions it is constant, its result as shown in figure 5,
It can be seen that Zn0.5Co0.5Fe2O4Catalyst reclaims the 1st, 3,5 times when, catalysis degradation modulus are respectively 9%, 8.2%, 8%,
And the Zn prepared0.5Co0.5Fe2O4/g-C3N4Composite photo-catalyst reclaims the 1st, 3,5 times when, catalysis degradation modulus are respectively 90%,
88.2%th, 87.8%, so that illustrate its stability preferably, meanwhile, under visible light illumination, catalyst photocatalytic activity ratio
Zn0.5Co0.5Fe2O4It is higher.
Claims (5)
1. a kind of Zn0.5Co0.5Fe2O4/g-C3N4The preparation method of composite photo-catalyst, it is characterised in that comprise the following steps:
(1)Weigh melamine solid and put in crucible, close the lid, and crucible band lid is put into Muffle furnace together, journey
Sequence temperature reaction obtains g-C3N4Nanometer sheet;
(2)Take step(1)In g-C3N4Nanometer sheet sample is ground, and weighs g-C3N4Nanometer sheet ultrasonic disperse in deionized water,
G-C is made3N4Nanometer sheet suspension;
(3)Weigh Fe (NO3)3·9H2O solids, Zn (NO3)2·6H2O solids and Co (NO3)2·6H2O solids are added to deionization
Dissolving forms mixed solution in water, with step(2)Middle suspension is well mixed, and increases magnetic agitation rotating speed, and continuing stirring makes it
Fully reaction;It is slowly added to L (+) tartaric acid solid thereto again, is slowly added to after finishing, continuing stirring makes it fully anti-
Should;It is slowly added to NaOH solids thereto again, increases magnetic agitation rotating speed, continuing stirring makes it fully react, and stirs;Will
Mixed liquor is transferred in reactor and obtains solid product after reaction, is washed with brand-new deionized water and ethanol, is dried in vacuo, obtains
Zn0.5Co0.5Fe2O4/g-C3N4Composite photo-catalyst;
Fe (NO in the mixed solution3)3·9H2O, Zn (NO3)2·6H2O, Co (NO3)2·6H2O, L (+) tartaric acid, NaOH is solid
The mass ratio of body is 4.04 ~ 8.08g:0.74~1.48g:0.75~1.49g:1.92~3.84g:2.2~4.4g;Wherein, mix molten
Fe (NO in liquid3)3·9H2O concentration is 0.1-0.2g/mL.
2. preparation method as claimed in claim 1, it is characterised in that step(1)In, the Muffle furnace temperature-programmed reaction bar
Part is 2 ~ 6 DEG C of min-1Rate program is warming up to 550 ~ 600 DEG C of 4 ~ 6h of reaction.
3. preparation method as claimed in claim 1, it is characterised in that step(2)In, the g-C3N4Nanometer sheet suspension
Concentration is 0.06-0.1g/mL.
4. preparation method as claimed in claim 1, it is characterised in that step(3)In, L (+) the tartaric acid solid, NaOH
The time that solid is slowly added to is 1min ~ 10min;Often adding a kind of reaction raw materials continuation stirring makes its sufficient reaction time equal
For 10min ~ 60min;It is 160 ~ 200 DEG C of 12 ~ 24h of reaction that the mixed liquor, which is transferred to the condition of reactor,.
5. preparation method as claimed in claim 1, it is characterised in that step(3)In, the deionized water and ethanol are respectively washed
Three times, the vacuum drying is dried at less than 100 DEG C.
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