CN103263942A - Preparation method and application of cobalt-loaded mesoporous graphite-phase carbon nitride visible-light-induced catalyst - Google Patents
Preparation method and application of cobalt-loaded mesoporous graphite-phase carbon nitride visible-light-induced catalyst Download PDFInfo
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- CN103263942A CN103263942A CN2013102203627A CN201310220362A CN103263942A CN 103263942 A CN103263942 A CN 103263942A CN 2013102203627 A CN2013102203627 A CN 2013102203627A CN 201310220362 A CN201310220362 A CN 201310220362A CN 103263942 A CN103263942 A CN 103263942A
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Abstract
The invention discloses a preparation method of cobalt-loaded mesoporous graphite-phase carbon nitride (Co/mpg-C3N4) and an application of cobalt-loaded mesoporous graphite-phase carbon nitride (Co/mpg-C3N4) in visible-light-induced catalytic degradation of methylene blue. The catalyst is prepared by steeping a cobalt precursor and roasting at high temperature. The preparation method comprises the following steps of: (1) roasting at high temperature by using silica solution (Ludox, HS-40, 12nm, 40wt%SiO2) as a template and cyanamide as a carbon source and a nitrogen source, and removing the template to prepare mesoporous graphite-phase carbon nitride (mpg-C3N4); and (2) steeping the precursor solution of cobalt into mpg-C3N4, carrying out secondary high-temperature roasting in a muffle furnace to prepare the load-type catalyst Co/mpg-C3N4. By using the cobalt-carried mesoporous graphite-phase carbon nitride as the visible-light-induced catalyst, the result shows that the effect of the cobalt-carried mesoporous graphite-phase carbon nitride used for the visible-light-induced catalytic degradation of methylene blue is good, and the visible-light-induced catalytic degradation rate is obviously improved in comparison with the mesoporous graphite-phase carbon nitride (mpg-C3N4) without cobalt.
Description
Technical field
The invention belongs to the visible light catalytic field, particularly preparation and the application in the visible light photocatalytic degradation methylene blue thereof of a kind of year mesoporous graphite phase carbon nitride of cobalt visible light catalyst.
Background technology
The 21 century two big challenges that face of human kind sustainable development are exactly environmental problem and energy problem.Solar energy has cheapness, cleaning, advantage such as renewable, and therefore, efficient quick ground utilizes, transforms and storage solar energy is the target that people make great efforts.The conductor photocatalysis technology just with the chemical conversion of solar energy be stored as core, eliminate toxic organic pollutant by the solar energy photocatalytic degraded, for we provide the living space of an environmental protection, so the visible light catalytic technology will become one of important means of reply challenge.For utilizing solar energy better, it is very necessary that preparation has a visible light-responded novel photocatalysis material.
Graphite phase carbon nitride (g-C
3N
4) be active material in recent years, its energy gap is 2.7 eV, visible region have absorption (
λ Max=590nm); The g-C that pi-conjugated plane accumulation mode forms
3N
4(pH=0 ~ 14) have very high stability and nontoxic in the aqueous solution, and these characteristics make it become a kind of novel visible light catalyst.Yet, g-C
3N
4Little, the quantum efficiency of specific area lowly cause the efficient of its photocatalytic degradation pollutant not high.People use multiple means to strengthen g-C
3N
4Photocatalytic activity, for example, preparation has the g-C of bigger serface meso-hole structure
3N
4(be designated as mpg-C
3N
4), meso-hole structure is conducive to g-C
3N
4Catalyst is to organic pollutant adsorption, thus the degradation rate to pollutant of enhancing catalyst.Yet the large-specific surface area nano pore structure is to g-C
3N
4The raising of photocatalytic activity is limited.Carried metal in the conventional method can further improve photocatalytic activity, document " Chemical Science for example, 2012,3:2170-2174. " reported that employing infusion process, photoreduction met hod prepare the mesoporous graphite phase carbon nitride of a kind of carried noble metal, be used for the photo catalytic reduction p-nitrophenyl, obtained good catalytic effect.The catalyst that this research institute makes has higher photocatalytic activity, but carried noble metal expense height has limited its application in actual industrial.
Summary of the invention
The object of the present invention is to provide a kind of year mesoporous graphite phase carbon nitride of cobalt (Co/mpg-C
3N
4) preparation method and in the application of visible light photocatalytic degradation methylene blue.
The technical solution that realizes the object of the invention is:
A kind of year mesoporous graphite phase carbon nitride of cobalt visible light catalyst got by the following steps preparation:
(1) Ludox HS-40 is mixed with cyanamide, high-temperature roasting in Muffle furnace after the vacuum drying, products therefrom with 4mol/L ammonium hydrogen fluoride solution washing go Ludox, deionized water be washed till neutrality, dry mpg-C
3N
4
(2) with the cobalt nitrate hexahydrate solution impregnation in mpg-C
3N
4In, constantly stir until the solution evaporate to dryness down at 50 ℃ ~ 80 ℃, in Muffle furnace, carry out after baking and make Co/mpg-C
3N
4
Wherein, Ludox HS-40 specifications parameter is Ludox, HS-40,12nm(silica particle diameter),
40wt%SiO
2(contain 40% SiO in the solution
2);
Ludox HS-40 and cyanamide mass ratio are 1:0.32 ~ 0.8 in the step (1), its vacuum drying temperature
Spend 40 ℃ ~ 70 ℃;
Sintering temperature is 550 ℃ ~ 600 ℃ in the step (1), and programming rate is 2 ℃/min, roasting time
4h~6h；
The after baking temperature is 200 ℃ ~ 500 ℃ in the step (2), 2 ℃/min of programming rate, roasting time
Be 2h ~ 6h.
The Co/mpg-C that obtains in the step (2)
3N
4The quality of middle Co accounts for Co/mpg-C
3N
4Gross mass
1%~10%；
The mesoporous graphite phase carbon nitride of cobalt visible light catalyst was used for the visible light photocatalytic degradation methylene blue in a kind of year, may further comprise the steps:
With methylene blue solution and Co/mpg-C
3N
4Mix in photo catalysis reactor, solution temperature is controlled at 15 ℃ ~ 30 ℃, and the initial mass concentration of methylene blue is 25mg/L ~ 80mg/L, after stirring 30min ~ 60min, the irradiation of 500W xenon lamp behind the reaction 180min, is measured the concentration of methylene blue after the sampling centrifugation.
Beneficial effect of the present invention is: (1) metallic cobalt is cheap and easy to get, compares than supported precious metal catalyst by the catalyst of the metallic cobalt preparation cheap and easy to get of infusion process load on mesoporous carbonitride, and its cost reduces greatly.(2) carry the visible light photocatalytic degradation methylene blue result that the mesoporous graphite phase carbon nitride of cobalt is used for methylene blue and show that the mesoporous graphite phase carbon nitride that this catalyst activity is not carried cobalt obviously strengthens.(3) carry the mesoporous graphite phase carbon nitride of cobalt stability in light-catalyzed reaction solution (pH=0 ~ 14) high, nontoxic, do not produce secondary pollution and recycling rate of waterused height.(4) the present invention has visible light-responded novel photocatalysis material for exploitation and has reference value preferably, provides effective solution for organic pollutant degradation.
Description of drawings
Fig. 1 is resulting 3%Co/mpg-C in the embodiment of the invention 1 and the Comparative Examples 1
3N
4And mpg-C
3N
4Catalyst is to methylene blue visible light catalytic clearance comparison diagram;
Fig. 2 is gained 1%Co/mpg-C in the embodiment of the invention 5,6,7
3N
4, 3%Co/mpg-C
3N
4, 1%Co/mpg-C
3N
4Catalyst is respectively to the clearance figure of methylene blue visible light catalytic;
Fig. 3 is that the after baking temperature of gained in the embodiment of the invention 8,9,10 is respectively 200 ℃, 300 ℃, 500 ℃ 3%Co/mpg-C
3N
4Catalyst is to the clearance figure of the visible light catalytic of methylene blue.
The specific embodiment
A kind of year mesoporous graphite phase carbon nitride of cobalt visible light catalyst got by the following steps preparation:
(1) Ludox HS-40 is mixed with cyanamide, high-temperature roasting in Muffle furnace after the vacuum drying, products therefrom with 4mol/L ammonium hydrogen fluoride solution washing go Ludox, deionized water be washed till neutrality, dry mpg-C
3N
4
(2) with the cobalt nitrate hexahydrate solution impregnation in mpg-C
3N
4In, constantly stir until the solution evaporate to dryness down at 50 ℃ ~ 80 ℃, in Muffle furnace, carry out after baking and make Co/mpg-C
3N
4
Wherein, Ludox HS-40 specifications parameter is Ludox, HS-40,12nm(silica particle diameter),
40wt%SiO
2(contain 40% SiO in the solution
2);
Ludox HS-40 and cyanamide mass ratio are 1:0.32 ~ 0.8 in the step (1), its vacuum drying temperature
Spend 40 ℃ ~ 70 ℃;
Sintering temperature is 550 ℃ ~ 600 ℃ in the step (1), and programming rate is 2 ℃/min, roasting time
4h~6h；
The after baking temperature is 200 ℃ ~ 500 ℃ in the step (2), 2 ℃/min of programming rate, roasting time
Be 2h ~ 6h.
The Co/mpg-C that obtains in the step (2)
3N
4The quality of middle Co accounts for Co/mpg-C
3N
4Gross mass
1%~10%；
The mesoporous graphite phase carbon nitride of cobalt visible light catalyst was used for the visible light photocatalytic degradation methylene blue in a kind of year, may further comprise the steps:
With methylene blue solution and Co/mpg-C
3N
4Mix in photo catalysis reactor, solution temperature is controlled at 15 ℃ ~ 30 ℃, and the initial mass concentration of methylene blue is 25mg/L ~ 80mg/L, after stirring 30min ~ 60min, the irradiation of 500W xenon lamp behind the reaction 180min, is measured the concentration of methylene blue after the sampling centrifugation.
Embodiment 1:
(1) be 1:0.32(Ludox 15.625g with cyanamide by mass ratio with Ludox HS-40) mix, after vacuum drying under 40 ℃ of conditions, in Muffle furnace, carry out 550 ℃ of high-temperature roasting 4h, 2 ℃/min of heating rate, products therefrom is removed Ludox with the washing of 4mol/L ammonium hydrogen fluoride solution, centrifugal washing, dry mpg-C
3N
4
(2) with the cobalt nitrate hexahydrate solution impregnation of 0.222g in the mpg-C of 1.455g
3N
4In, under 80 ℃ of conditions, constantly stir until the solution evaporate to dryness, 300 ℃ of after baking 2h in Muffle furnace, 2 ℃/min of heating rate obtains 3%Co/mpg-C
3N
4
(3) with the 3%Co/mpg-C that obtains
3N
4Catalyst mixes in photo catalysis reactor with methylene blue solution, the initial concentration of methylene blue is 80mg/L, the addition of catalyst is 0.4g/L, solution temperature control is at 15 ℃, after stirring 30min, the irradiation of 500W xenon lamp, reaction 180min, measure methylene blue concentration after the sampling centrifugation, the clearance of methylene blue is that 53%(sees Fig. 1).
Comparative Examples 1:
In embodiment 1, only adopt the preparation method of step (1) to make mpg-C
3N
4, with gained mpg-C
3N
4As catalyst, be used for the visible light photocatalytic degradation methylene blue.Under the photocatalytic reaction conditions identical with embodiment 1 step (3), behind the illumination 180min, the clearance of methylene blue is that 28.73%(sees Fig. 1).As seen,
Mpg-C
3N
4And 3%Co/mpg-C
3N
4Compare mpg-C
3N
4Visible light catalysis activity far below 3%Co/mpg-C
3N
4
Embodiment 2:
(1) be that 1:0.8 (Ludox 6.25g) mix with cyanamide by mass ratio with Ludox HS-40, after vacuum drying under 70 ℃ of conditions, in Muffle furnace, carry out 600 ℃ of high-temperature roasting 6h, 2 ℃/min of heating rate, products therefrom is removed Ludox with the washing of 4mol/L ammonium hydrogen fluoride solution, centrifugal washing, dry mpg-C
3N
4
(2) with the cobalt nitrate hexahydrate solution impregnation of 0.222g in the mpg-C of 1.455g
3N
4In, under 50 ℃ of conditions, constantly stir until the solution evaporate to dryness, 300 ℃ of after baking 2h in Muffle furnace, 2 ℃/min of heating rate obtains 3%Co/mpg-C
3N
4
What (3) will obtain mixes in photo catalysis reactor with methylene blue solution, and the initial concentration of methylene blue is 25mg/L, catalyst 3%Co/ mpg-C
3N
4Addition be 0.4g/L, solution temperature is controlled at 15 ℃, stir 30min after, the irradiation of 500W xenon lamp, reaction 180min measures methylene blue concentration after the sampling centrifugation, the clearance of methylene blue is 58.64%.
Embodiment 3:
In embodiment 1, other conditions are constant, and changing the middle Ludox HS-40 of embodiment 1 step (1) and cyanamide mass ratio is 1:0.4(Ludox 12.5g), with gained 3%Co/mpg-C
3N
4Be catalyst, its visible light catalytic reaction condition is identical with embodiment 2.Behind the light-catalyzed reaction 180min, the clearance of methylene blue is 80.28%.
Embodiment 4:
Selecting embodiment 1 preparation Ludox HS-40 and cyanamide mass ratio for use is 1:0.32(Ludox 15.625g) 3%Co/mpg-C
3N
4Be catalyst, its visible light catalytic reaction condition is identical with embodiment 2.(see figure 2) behind the light-catalyzed reaction 180min, the clearance of methylene blue are 91.65%.
Embodiment 5:
In embodiment 1, other conditions are constant, with cobalt nitrate hexahydrate and mpg-C
3N
4Amount change 0.074g and 1.485g respectively into, with gained 1%Co/mpg-C
3N
4(Co accounts for Co/mpg-C
3N
4 Gross mass 1%) be catalyst, its visible light catalytic reaction condition is identical with embodiment 2.(see figure 2) behind the light-catalyzed reaction 180min, the clearance of methylene blue are 70.49%.
Embodiment 6:
Select embodiment 1 preparation gained 3%Co/mpg-C for use
3N
4(Co accounts for Co/mpg-C
3N
4 Gross mass 3%) be catalyst, its visible light catalytic reaction condition is identical with embodiment 2.(see figure 2) behind the light-catalyzed reaction 180min, the clearance of methylene blue are 91.65%.
Embodiment 7:
In embodiment 1, other conditions are constant, with cobalt nitrate hexahydrate and mpg-C
3N
4Amount change 0.7904g and 1.44g respectively into, with gained 1%Co/mpg-C
3N
4(Co accounts for Co/mpg-C
3N
4Gross mass 10%) be catalyst, its visible light catalytic reaction condition is identical with embodiment 2.(see figure 2) behind the light-catalyzed reaction 180min, the clearance of methylene blue are 63.53%.
Embodiment 8:
In embodiment 1, other conditions are constant, and changing and carrying out the after baking temperature in embodiment 1 step (2) is 200 ℃, is 200 ℃ 3%Co/mpg-C with sintering temperature
3N
4Be catalyst, its visible light catalytic reaction condition is identical with embodiment 2.(see figure 3) behind the light-catalyzed reaction 180min, the clearance of methylene blue are 87.98%.
Embodiment 9:
The after baking temperature of carrying out of selecting that embodiment 1 prepares for use is 300 ℃ 3% Co/ mpg-C
3N
4Be catalyst, its visible light catalytic reaction condition is identical with embodiment 2.(see figure 3) behind the light-catalyzed reaction 180min, the clearance of methylene blue are 91.65%.
Embodiment 10:
In embodiment 1, other conditions are constant, and changing and carrying out the after baking temperature in embodiment 1 step (2) is 500 ℃, is 500 ℃ 3%Co/mpg-C with sintering temperature
3N
4Catalyst, its visible light catalytic reaction condition is identical with embodiment 2.Behind the light-catalyzed reaction 180min, the clearance (see figure 3) of methylene blue is 45.24%.
Claims (9)
1. one kind carries the mesoporous graphite phase carbon nitride of cobalt visible light catalyst, it is characterized in that being got by the following steps preparation:
(1) Ludox HS-40 is mixed with cyanamide, high-temperature roasting in Muffle furnace after the vacuum drying, products therefrom with 4mol/L ammonium hydrogen fluoride solution washing go Ludox, deionized water be washed till neutrality, dry mpg-C
3N
4
(2) with the cobalt nitrate hexahydrate solution impregnation in mpg-C
3N
4In, constantly stir until the solution evaporate to dryness down at 50 ℃ ~ 80 ℃, in Muffle furnace, carry out after baking and make Co/mpg-C
3N
4
2. the according to claim 1 year mesoporous graphite phase carbon nitride of cobalt visible light catalyst is characterized in that the middle Ludox HS-40 of step (1) and cyanamide mass ratio are 1:0.32 ~ 0.8, and the vacuum drying temperature is 40 ℃ ~ 70 ℃.
3. the according to claim 1 year mesoporous graphite phase carbon nitride of cobalt visible light catalyst is characterized in that sintering temperature is 550 ℃ ~ 600 ℃ in the step (1), and programming rate is 2 ℃/min, roasting time 4h ~ 6h.
4. the according to claim 1 year mesoporous graphite phase carbon nitride of cobalt visible light catalyst is characterized in that the after baking temperature is 200 ℃ ~ 500 ℃ in the step (2), 2 ℃/min of programming rate, and roasting time is 2h ~ 6h.
5. the according to claim 1 year mesoporous graphite phase carbon nitride of cobalt visible light catalyst is characterized in that the Co/mpg-C that obtains in the step (2)
3N
4The quality of middle Co accounts for Co/mpg-C
3N
41% ~ 10% of gross mass.
6. preparation method of carrying the mesoporous graphite phase carbon nitride of cobalt visible light catalyst is characterized in that described method may further comprise the steps:
(1) Ludox HS-40 is mixed with cyanamide, high-temperature roasting in Muffle furnace after the vacuum drying, products therefrom is removed Ludox with the washing of 4mol/L ammonium hydrogen fluoride solution, deionized water is washed till neutrality, dry mpg-C
3N
4
(2) with the cobalt nitrate hexahydrate solution impregnation in mpg-C
3N
4In, constantly stir until the solution evaporate to dryness down at 50 ℃ ~ 80 ℃, in Muffle furnace, carry out after baking and make Co/mpg-C
3N
4
7. the preparation method of the according to claim 6 year mesoporous graphite phase carbon nitride of cobalt visible light catalyst is characterized in that, Ludox HS-40 and cyanamide mass ratio are 1:0.32 ~ 0.8 in the step (1), and the vacuum drying temperature is 40 ℃ ~ 70 ℃; Sintering temperature is 550 ℃ ~ 600 ℃, and programming rate is 2 ℃/min, roasting time 4h ~ 6h.
8. the preparation method of the according to claim 6 year mesoporous graphite phase carbon nitride of cobalt visible light catalyst is characterized in that, the after baking temperature is 200 ℃ ~ 500 ℃ in the step (2), 2 ℃/min of programming rate, and roasting time is 2h ~ 6h; The Co/mpg-C that obtains
3N
4The quality of middle Co accounts for Co/mpg-C
3N
41% ~ 10% of gross mass.
9. application of carrying the mesoporous class graphite of cobalt phase carbon nitride visible light catalyst is characterized in that the described year mesoporous graphite phase carbon nitride of cobalt of claim 1 visible light catalyst is used for the visible light photocatalytic degradation methylene blue, may further comprise the steps:
With methylene blue solution and Co/mpg-C
3N
4Mix in photo catalysis reactor, solution temperature is controlled at 15 ℃ ~ 30 ℃, and the initial mass concentration of methylene blue is 25mg/L ~ 80mg/L, after stirring 30min ~ 60min, the irradiation of 500W xenon lamp behind the reaction 180min, is measured the concentration of methylene blue after the sampling centrifugation.
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