CN103301867A - Inorganic ion doped carbon nitride photocatalyst and preparation method thereof - Google Patents

Inorganic ion doped carbon nitride photocatalyst and preparation method thereof Download PDF

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CN103301867A
CN103301867A CN2013102569506A CN201310256950A CN103301867A CN 103301867 A CN103301867 A CN 103301867A CN 2013102569506 A CN2013102569506 A CN 2013102569506A CN 201310256950 A CN201310256950 A CN 201310256950A CN 103301867 A CN103301867 A CN 103301867A
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photochemical catalyst
preparation
carbonitride photochemical
carbonitride
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CN103301867B (en
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董帆
李秋燕
王震宇
孙艳娟
赵再望
傅敏
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Chongqing Transsut Technology Co ltd
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Chongqing Technology and Business University
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Abstract

The invention provides an inorganic ion doped carbon nitride photocatalyst and a preparation method thereof. The inorganic ion doped carbon nitride photocatalyst has a molecular formula shown in a formula (I). The preparation method comprises the following steps of: sufficiently mixing carbon and nitrogen sources and inorganic salt in a water solution, then drying and calcining to obtain the inorganic ion doped carbon nitride photocatalyst which has the molecular formula shown in the formula (I). According to the photocatalyst, inorganic ions enter a crystal lattice or an interlayer of C3N4, and visible-light catalytic activity of the C3N4 photocatalyst provided by the invention is greatly enhanced through the doping of the inorganic ions. Experiments indicate that the visible-light catalytic activity of the inorganic ion doped C3N4 photocatalyst with a two-dimensional structure is 1.5-3 times higher than that of a photocatalyst without C3N4 doped. Besides, the preparation method provided by the invention is moderate in condition, easy to operate and favorable to large-scale production.

Description

Carbonitride photochemical catalyst that a kind of inorganic ions mixes and preparation method thereof
Technical field
The present invention relates to light-catalysed technical field, relate in particular to carbonitride photochemical catalyst of a kind of inorganic ions doping and preparation method thereof.
Background technology
Current, the mankind face environmental pollution and energy shortage two big basic problems, how effectively to utilize continuable cleaning solar energy to solve environmental problem and energy problem more and more is subjected to global concern and attention.In recent years, along with the development of photocatalysis technology, realize that by solar energy photocatalysis technology is to have shown huge application potential aspect the chemical energy field in environmental pollution purification and conversion of solar energy.
What play an important role in photocatalytic process is catalysis material.Because the photochemical catalyst of visible light optical drive can directly utilize sunshine or people's irradiation, and has shown huge application potential in environmental protection, material science and conversion of solar energy field.Therefore the parent that the photochemical catalyst that has a visible light activity more and more is subjected to the researcher looks at.In the past few decades, scientists endeavours to have with research and development the photochemical catalyst of visible light activity always, such as inorganic visible light catalyst Fe 2O 3, (BiO) 2CO 3, MoS 2, SrTiO 3And WO 3/ BiOCl, organic visible light catalyst g-C 3N 4, simple substance photochemical catalyst Si, P, S and Se.Class Graphene carbonitride (g-C particularly 3N 4), be first kind of organic photochemical catalyst finding up to now, it have suitable energy gap (about 2.7eV), high heat endurance and chemical stability, nontoxic, bio-compatibility, with low cost, be easy to advantages such as chemical modification, be subjected to researcher's extensive concern.
In the research to the semiconductor type photochemical catalyst, class Graphene carbonitride semi-conducting material has unique electronic structure, good light absorpting ability and higher photocatalysis performance, the research and development more widely that it obtains.But, because the easy recombination rate in lower, the light induced electron hole of carbonitride specific area is high and have shortcoming such as a large amount of faults of construction, make carbonitride active not ideal enough under visible light, limited the large-scale application of carbonitride.Therefore, be necessary to develop the modification that effective method is used for carbonitride, with its photocatalysis performance of further raising.
Summary of the invention
The object of the present invention is to provide carbonitride photochemical catalyst of a kind of inorganic ions doping and preparation method thereof, the carbonitride photochemical catalyst that described inorganic ion mixes can strengthen visible absorption, improve the separative efficiency of light induced electron, have higher visible light catalysis activity.
The invention provides the carbonitride photochemical catalyst that a kind of inorganic ions mixes, have the molecular formula shown in the formula (I):
[X] m[C 3N 4] (1-m) （I）；
Wherein, m is 1%～40%.
Preferably, described m is 2%～20%.
Preferred X is KCl, KBr, KI, NH 4Cl, NH 4Br, NH 4I, KNO 3, K 2SO 4, K 2CO 3, KH 2PO 4, CaCl 2, MgCl 2, BaCl 2, (NH 4) 2SO 4, NH 4NO 3, (NH 4) 2CO 3
Preferred carbonitride raw material is single cyanogen ammonia, dicyan diamino, melamine, cyanuric acid, thiocarbamide or urea.
The invention provides inorganic ions doping carbonitride photochemical catalyst and preparation method thereof, may further comprise the steps:
Carbon nitrogen source and inorganic salts are fully mixed the back oven dry in the aqueous solution, calcine, the carbonitride photochemical catalyst that the inorganic ions of the molecular formula shown in (I) that obtains having formula mixes:
[X] m[C 3N 4] (1-m) （I）；
Wherein, m is 1%～40%.
Preferably, described carbon nitrogen source is single cyanogen ammonia, dicyan diamino, melamine, cyanuric acid, thiocarbamide or urea.
Preferably, described inorganic salts are KCl, KBr, KI, NH 4Cl, NH 4Br, NH 4I, KNO 3, K 2SO 4, K 2CO 3, KH 2PO 4, CaCl 2, MgCl 2, BaCl 2, (NH 4) 2SO 4, NH 4NO 3Or (NH 4) 2CO 3
Preferably, the mass ratio of described carbon nitrogen source and described inorganic salts is 1:(0.01～0.4).
Preferably, the mass ratio of described carbon nitrogen source and described inorganic salts is 1:(0.02～0.2).
Preferably, described bake out temperature is 40～70 ℃.
Preferably, described calcining heat is 400～650 ℃.
Preferably, described calcination time is 0.5～10h.
The invention provides carbonitride photochemical catalyst of a kind of inorganic ions doping and preparation method thereof, the carbonitride photochemical catalyst that inorganic ions provided by the invention mixes has the molecular formula shown in the formula (I): [X] m[C 3N 4] (1-m)(I); Wherein, m is 1%～40%.The present invention is raw material with carbon nitrogen source and inorganic salts, and both are fully mixed the back oven dry in the aqueous solution, calcines, the carbonitride photochemical catalyst that the inorganic ions of the molecular formula shown in (I) that obtains having formula mixes.In preparation process, described inorganic salts all are dissociated into ion under aqueous conditions, presoma is in the carbonitride process in high temperature polymerization, the in-situ doped structure that enters into carbonitride of inorganic ions, the carbonitride photochemical catalyst that the inorganic ions of the molecular formula shown in (I) that obtains having formula mixes.The inorganic ions and the C that mix 3N 4Form chemical bond, changed C 3N 4Forbidden band structure.C 3N 4Mixing of inorganic ions makes the energy gap of inorganic ions doping carbonitride photochemical catalyst provided by the invention be decreased to 2.2eV～2.6eV in the structure, promote catalyst to the absorption of visible light, the separative efficiency in light induced electron and hole is enhanced simultaneously, so the carbonitride photochemical catalyst that inorganic ions mixes has higher visible light catalysis activity.Experimental result shows, the carbonitride photochemical catalyst that inorganic ions provided by the invention mixes is under visible light radiation, clearance to NO is 30%～50%, has improved greatly under the condition of visible light the removal of NO, is conducive to its application in environment and energy field.
In addition, method provided by the invention does not need to use template, can obtain the carbonitride photochemical catalyst that inorganic ions mixes under the condition of gentleness, and equipment is simple to operation, can be used for large-scale production.
Description of drawings
Fig. 1 is the UV-visDRS collection of illustrative plates of the carbonitride photochemical catalyst that mixes of the potassium chloride of the embodiment of the invention 1 preparation;
Fig. 2 is the PL collection of illustrative plates of the carbonitride photochemical catalyst that mixes of the potassium chloride of the embodiment of the invention 1 preparation;
Fig. 3 is the SEM photo of the carbonitride photochemical catalyst that mixes of the KBr of the embodiment of the invention 2 preparation;
Fig. 4 is the UV-visDRS collection of illustrative plates of the carbonitride photochemical catalyst that mixes of the KI of the embodiment of the invention 3 preparation;
Fig. 5 is the XRD collection of illustrative plates of the carbonitride photochemical catalyst that mixes of the ammonium chloride of the embodiment of the invention 4 preparation;
Fig. 6 is the XRD collection of illustrative plates of the carbonitride photochemical catalyst that mixes of the ammonium bromide of the embodiment of the invention 5 preparation;
Fig. 7 is the NO clearance figure of the carbonitride photochemical catalyst that mixes of the ammonium iodide of the embodiment of the invention 6 preparation;
Fig. 8 is the TEM photo of the carbonitride photochemical catalyst that mixes of the potassium nitrate of the embodiment of the invention 7 preparation;
Fig. 9 be the carbonitride photochemical catalyst that mixes of the potassium nitrate of the embodiment of the invention 7 preparation can spectrogram;
Figure 10 is the TEM photo of the carbonitride photochemical catalyst that mixes of the potassium sulfate of the embodiment of the invention 8 preparation;
Figure 11 be the carbonitride photochemical catalyst that mixes of the potassium sulfate of the embodiment of the invention 8 preparation can spectrogram;
Figure 12 is the XRD collection of illustrative plates of the carbonitride photochemical catalyst that mixes of the potash of the embodiment of the invention 9 preparation;
Figure 13 is the UV-vis DRS collection of illustrative plates of the carbonitride photochemical catalyst that mixes of the potassium dihydrogen phosphate of the embodiment of the invention 10 preparation;
Figure 14 is the SEM photo of the carbonitride photochemical catalyst that mixes of the barium chloride of the embodiment of the invention 11 preparation;
Figure 15 is the UV-vis DRS collection of illustrative plates of the carbonitride photochemical catalyst that mixes of the calcium chloride of the embodiment of the invention 12 preparation;
Figure 16 is the NO clearance figure of the carbonitride photochemical catalyst that mixes of the magnesium chloride of the embodiment of the invention 13 preparation;
Figure 17 is the NO clearance figure of the carbonitride photochemical catalyst that mixes of the ammonium sulfate of the embodiment of the invention 14 preparation;
Figure 18 is the NO clearance figure of the carbonitride photochemical catalyst that mixes of the ammonium nitrate of the embodiment of the invention 15 preparation;
Figure 19 is the PL collection of illustrative plates of the carbonitride photochemical catalyst that mixes of the ammonium nitrate of the embodiment of the invention 15 preparation;
Figure 20 is the NO clearance figure of the carbonitride photochemical catalyst that mixes of the ammonium carbonate of the embodiment of the invention 16 preparation.
The specific embodiment
The invention provides carbonitride photochemical catalyst of a kind of inorganic ions doping and preparation method thereof, have the molecular formula shown in the formula (I):
[X] m[C 3N 4] (1-m) （I）；
Wherein, m is 1%～40%.
In inorganic ions doping carbonitride photochemical catalyst provided by the invention, inorganic ions enters into described C 3N 4In the structure, the inorganic ions doping carbonitride photochemical catalyst of the molecular formula shown in (I) that obtains having formula, wherein m is 1%～40%, is preferably 2%～20%, more preferably 5%～15%.
The carbonitride photochemical catalyst that inorganic ions provided by the invention mixes is because C 3N 4The existence of inorganic ions makes its energy gap be decreased to 2.2eV～2.6eV in the structure, and visible absorption strengthens, and the separative efficiency in light induced electron and hole is improved simultaneously, so the carbonitride that inorganic ions mixes shows higher visible light catalysis activity.Experimental result shows, inorganic ions doping carbonitride photochemical catalyst provided by the invention is under visible light radiation, clearance to NO is 30%～50%, improved greatly under the condition of visible light the removal efficient of NO, illustrated that inorganic ions doping carbonitride photochemical catalyst provided by the invention has higher visible light catalysis activity.
The invention provides a kind of preparation method of carbonitride photochemical catalyst of inorganic ions doping, may further comprise the steps:
Carbon nitrogen source and inorganic salts are fully mixed the back oven dry in the aqueous solution, calcine, the carbonitride photochemical catalyst that the inorganic ions of the molecular formula shown in (I) that obtains having formula mixes:
[X] m[C 3N 4] (1-m) （I）；
Wherein, m is 1%～40%, is preferably 2%～20%, more preferably 5%～15%;
Described carbon nitrogen source is preferably single cyanogen ammonia, dicyanodiamine, melamine, cyanuric acid, thiocarbamide or urea for the raw material of preparation carbonitride;
Described inorganic salts be potassium chloride, KBr, KI, ammonium chloride, ammonium bromide, ammonium iodide, potassium nitrate, potassium sulfate, potash, potassium dihydrogen phosphate, calcium chloride, magnesium chloride, barium chloride, ammonium sulfate, ammonium nitrate or carbonic acid by.
The present invention is at first soluble in water with carbon nitrogen source and inorganic salts, and the mixed solution that obtains is dried at low temperatures; Described carbon nitrogen source is preferably single cyanogen ammonia, dicyanodiamine, melamine, cyanuric acid, thiocarbamide or urea.Described inorganic salts be preferably potassium chloride, KBr, KI, ammonium chloride, ammonium bromide, ammonium iodide, potassium nitrate, potassium sulfate, potash, potassium dihydrogen phosphate, calcium chloride, magnesium chloride, barium chloride, ammonium sulfate, ammonium nitrate or carbonic acid by; Described water is preferably deionized water; The mass ratio of described carbonitride and described inorganic salts is preferably 1:(0.01～0.4), 1:(0.02～0.2 more preferably).The present invention preferably at first prepares inorganic salt solution, adds carbon nitrogen source then in the aqueous solution of described inorganic salts, and the temperature that obtains the described oven dry of oven dry behind the mixed solution is preferably 40～70 ℃.
The present invention with oven dry under the described mixed solution low temperature after, again mixture is carried out roasting, the carbonitride photochemical catalyst that the inorganic ions of the molecular formula shown in (I) that obtains having formula mixes.In the present invention, described inorganic salts all are dissociated into ion in the aqueous solution; Simultaneously, in the process of described roasting reaction, described inorganic ions enters into the carbonitride layer structure, thus the carbonitride photochemical catalyst that the inorganic ions of the molecular formula shown in (I) that obtains having formula mixes.In inorganic ions doping carbonitride photochemical catalyst provided by the invention, inorganic ions enters into the layer structure of carbonitride, thereby make the energy gap of the inorganic ions doping carbonitride photochemical catalyst that obtains be decreased to 2.2eV～2.6eV, its absorption spectrum is widened to visible region from the ultraviolet spectra district, therefore can absorb visible light.In the present invention, the temperature of described roasting reaction is preferably 400 ℃～650 ℃, more preferably 480 ℃～600 ℃; The time of described roasting reaction is preferably 0.5 hour～and 10 hours, more preferably 1 hour～5 hours.
After the roasting reaction was finished, the present invention preferably with the reaction system cooling, obtained product.The present invention adopts the technical scheme of cooling well known to those skilled in the art to get final product to the parameter of described cooling.
After obtaining product, the present invention preferably mills described product, obtains powder-product.The present invention does not have special restriction to described parameter of milling, and adopts technical scheme of milling well known to those skilled in the art to get final product.
Behind the inorganic ions doping carbonitride photochemical catalyst of the molecular formula shown in (I) that obtains having formula, the present invention characterizes and performance test the carbonitride photochemical catalyst that the inorganic ions that obtains mixes, and detailed process and result are as follows:
The present invention carries out X-ray diffraction (XRD) analysis to the carbonitride photochemical catalyst that the inorganic ions that obtains mixes, and the result shows that the thing of inorganic ions doping carbonitride photochemical catalyst provided by the invention is C mutually 3N 4
The present invention carries out UV, visible light diffuse reflection (UV-vis DRS) to the inorganic ions doping carbonitride photochemical catalyst that obtains and analyzes, the result shows, broadband, forbidden band with inorganic ions doping carbonitride photochemical catalyst of molecular formula shown in the formula (I) provided by the invention is 2.2eV～2.6eV, thereby make its absorption spectrum generation red shift, so it can absorb more visible light.
The present invention carries out ESEM (SEM) analysis to the carbonitride photochemical catalyst that the inorganic ions that obtains mixes, and the result shows that the carbonitride photochemical catalyst that inorganic ions provided by the invention mixes has the nanometer sheet structure of stratiform.
The present invention throws Electronic Speculum (TEM) analysis to the inorganic ions doping carbonitride photochemical catalyst that obtains, and the result shows that the carbonitride photochemical catalyst that inorganic ions provided by the invention mixes has the nanometer sheet structure of stratiform.
The present invention tests the catalytic performance of the carbonitride photochemical catalyst that the inorganic ions that obtains mixes, and detailed process and result are as follows:
Be preferably 40%～80% in relative humidity, oxygen content is under 15%～25% the condition, preferably 0.1g～0.5g inorganic ions doping provided by the invention carbonitride photochemical catalyst is placed the NO Continuous Flow, the initial concentration of described NO is preferably 500ppb～650ppb, the gas flow of described NO Continuous Flow is preferably 2.4L/min～4.0L/mim, adopt the halogen tungsten lamp of 100W, and the edge filter filtering ultraviolet light with 420nm, make the described edge filter of visible light transmissive, thereby make visible light shine described inorganic ions doping carbonitride photochemical catalyst, obtain it to the clearance of NO.Experimental result shows, inorganic ions doping carbonitride photochemical catalyst provided by the invention is under visible light radiation, clearance to NO is 30%～50%, this illustrates that inorganic ions doping carbonitride photochemical catalyst provided by the invention has higher visible light catalysis activity, and higher than the visible light catalysis activity of independent carbonitride photochemical catalyst.
The invention provides a kind of inorganic ions doping carbonitride photochemical catalyst and preparation method thereof, inorganic ions doping carbonitride photochemical catalyst provided by the invention has the molecular formula shown in the formula (I): [X] m[C 3N 4] (1-m)(I); Wherein, m is 1%～40%.The present invention is raw material with raw material and the inorganic salts of preparation carbonitride, it is mixed the back in the aqueous solution dry under the low temperature, carry out the roasting reaction at last, the inorganic ions doping carbonitride photochemical catalyst of the molecular formula shown in (I) that obtains having formula is in the aqueous solution, described inorganic ion all dissociates and is combined with the raw molecule of preparation carbonitride, obtains inorganic ions doping carbonitride photochemical catalyst under high-temperature roasting; Simultaneously, described inorganic ions enters into the carbonitride layer structure, has obtained having the inorganic ions doping carbonitride photochemical catalyst of molecular formula shown in the formula (I).Inorganic ions doping carbonitride photochemical catalyst provided by the invention is at C 3N 4Mixed inorganic ions in the layer structure, made its energy gap be decreased to 2.2eV～2.6eV, red shift from taking place in its absorption spectrum, and therefore, inorganic ions doping carbonitride photochemical catalyst provided by the invention can absorb more visible light.Experimental result shows, inorganic ions doping carbonitride photochemical catalyst provided by the invention can be realized the removal to NO under visible light radiation, and its clearance to NO is 30%～50%, improved greatly under visible light the removal of NO, this illustrates that inorganic ions doping carbonitride photochemical catalyst provided by the invention has higher visible light catalysis activity.
In addition, the two-dimensional structure that the carbonitride photochemical catalyst that the form of inorganic ions doping carbonitride photochemical catalyst provided by the invention is mixed for the inorganic ions with molecular formula shown in the formula (I) has stratiform, the two-dimensional structure of stratiform is conducive to separating of photogenerated charge and transmission with inorganic ions, improved catalytic efficiency, improved the utilization rate to light source, therefore, the carbonitride photochemical catalyst of inorganic ions doping provided by the invention has higher photocatalysis performance.
In order to further specify the present invention, carbonitride photochemical catalyst that inorganic ions provided by the invention is mixed below in conjunction with embodiment and preparation method thereof is described in detail, but they can not be interpreted as the restriction to protection domain of the present invention.
Embodiment 1
, and add the single cyanogen ammonia of 4g in the Klorvess Liquid and fully stir and evenly mix 0.126g potassium chloride dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 2h under 550 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the potassium chloride doping carbonitride photochemical catalyst of present embodiment preparation is [KCl] 0.03[C 3N 4] 0.97
The present invention carries out UV-vis DRS with the potassium chloride doping carbonitride photochemical catalyst that obtains and analyzes, and the result as shown in Figure 1.The result shows that the energy gap of the potassium chloride doping carbonitride photochemical catalyst of present embodiment preparation is 2.52eV, visible light is had significantly absorb; The present invention carries out PL with the potassium chloride doping carbonitride photochemical catalyst that obtains and analyzes, the result as shown in Figure 2, the result shows that the pure carbonitride photochemical catalyst of PL strength ratio of the potassium chloride doping carbonitride photochemical catalyst of present embodiment preparation obviously reduces, and light induced electron and separating of hole are enhanced.
The present invention is used for removal to NO with the potassium chloride doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g potassium chloride doping carbonitride photochemical catalyst that embodiment 1 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone potassium chloride doping carbonitride photochemical catalyst, the clearance that obtains NO is 31.3%, the result is as shown in table 1, the catalytic performance result of the potassium chloride doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the potassium chloride doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 2
, and add 4g dicyan diamino in the potassium bromide solution and fully stir and evenly mix 0.089g KBr dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 3h under 500 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the KBr doping carbonitride photochemical catalyst of present embodiment preparation is [KBr] 0.05[C 3N 4] 0.95
The present invention carries out sem analysis with the KBr doping carbonitride photochemical catalyst that obtains, and the result as shown in Figure 3.As seen from Figure 3, the KBr doping carbonitride photochemical catalyst that present embodiment obtains is the nanometer sheet structure of two-dimensional layer, and the doping of KBr does not damage the structure of carbonitride.
The present invention is used for removal to NO with the KBr doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g KBr doping carbonitride photochemical catalyst that embodiment 2 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone KBr doping carbonitride photochemical catalyst, the clearance that obtains NO is 38.5%, the result is as shown in table 1, the catalytic performance result of the KBr doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the KBr doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 3
, and add the 4g melamine in the liquor kalii iodide and fully stir and evenly mix 0.078g KI dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 4h under 520 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the KI doping carbonitride photochemical catalyst of present embodiment preparation is [KI] 0.07[C 3N 4] 0.93The present invention carries out UV-vis DRS with the KI doping carbonitride photochemical catalyst that obtains and analyzes, and the result as shown in Figure 4.The result shows that the energy gap of the KI doping carbonitride photochemical catalyst of present embodiment preparation is 2.47eV, visible light is had significantly absorb.
The present invention is used for removal to NO with the KI doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g KI doping carbonitride photochemical catalyst that embodiment 3 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone KI doping carbonitride photochemical catalyst, the clearance that obtains NO is 39.7%, the result is as shown in table 1, the catalytic performance result of the KI doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the KI doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 4
, and add the 4g cyanuric acid in the ammonium chloride solution and fully stir and evenly mix the 0.054g chloride leach with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 3h under 560 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The present invention carries out XRD analysis with the ammonium chloride doping carbonitride photochemical catalyst that obtains, the result as shown in Figure 5, Fig. 5 is the XRD collection of illustrative plates of the ammonium chloride doping carbonitride photochemical catalyst of the embodiment of the invention 4 preparations, as seen from Figure 5, the thing of the ammonium chloride doping carbonitride photochemical catalyst that obtains of present embodiment is C mutually 3N 4The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [NH 4Cl] 0.03[C 3N 4] 0.97
The present invention is used for removal to NO with the ammonium chloride doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g ammonium chloride doping carbonitride photochemical catalyst that embodiment 4 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone ammonium chloride doping carbonitride photochemical catalyst, the clearance that obtains NO is 38.4%, the result is as shown in table 1, the catalytic performance result of the ammonium chloride doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the ammonium chloride doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 5
, and add the 10g thiocarbamide in the ammonium bromide solution and fully stir and evenly mix 0.074g ammonium bromide dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 2h under 580 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [NH 4Br] 0.1[C 3N 4] 0.9
The present invention carries out XRD analysis with the ammonium bromide doping carbonitride photochemical catalyst that obtains, the result as shown in Figure 6, Fig. 6 is the XRD collection of illustrative plates of the ammonium bromide doping carbonitride photochemical catalyst of the embodiment of the invention 5 preparations, as seen from Figure 6, the thing of the ammonium chloride doping carbonitride photochemical catalyst that obtains of present embodiment is C mutually 3N 4
The present invention is used for removal to NO with the ammonium bromide doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g ammonium bromide doping carbonitride photochemical catalyst that embodiment 5 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone ammonium bromide doping carbonitride photochemical catalyst, the clearance that obtains NO is 39.1%, the result is as shown in table 1, the catalytic performance result of the ammonium bromide doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the ammonium bromide doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 6
, and add 10g urea in the ammonium iodide solution and fully stir and evenly mix 0.069g ammonium iodide dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 3h under 600 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [NH 4I] 0.15[C 3N 4] 0.85
The present invention carries out the removal of NO with the ammonium iodide doping carbonitride photochemical catalyst that obtains, the result as shown in Figure 7, as seen from Figure 7, the clearance to NO of the ammonium iodide doping carbonitride photochemical catalyst that present embodiment obtains is 48.7%, than unadulterated carbonitride the removal of NO is had bigger enhancing.
The present invention is used for removal to NO with the ammonium iodide doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g ammonium iodide doping carbonitride photochemical catalyst that embodiment 6 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone ammonium iodide doping carbonitride photochemical catalyst, the clearance that obtains NO is 48.7%, the result is as shown in table 1, the catalytic performance result of the ammonium iodide doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the ammonium iodide doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 7
, and add the 10g thiocarbamide in the potassium nitrate solution and fully stir and evenly mix 0.159g potassium nitrate dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 4h under 500 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that the present invention is obtained carries out SEM face scanning analysis, and the result contain potassium, oxygen, carbon and nitrogen element in the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes, and the catalyst doped chemical is evenly distributed as seen from Figure 19.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [KNO 3] 0.02[C 3N 4] 0.98
The present invention carries out tem analysis with the potassium nitrate doping carbonitride photochemical catalyst that obtains, the result as shown in Figure 8, as seen from Figure 8, the potassium nitrate doping carbonitride photochemical catalyst that present embodiment obtains is that two-dimensional nano is laminar structured, and potassium nitrate doping carbonitride does not damage the body construction of carbonitride.
The present invention is used for removal to NO with the potassium nitrate doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g potassium nitrate doping carbonitride photochemical catalyst that embodiment 7 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone potassium nitrate doping carbonitride photochemical catalyst, the clearance that obtains NO is 44.6%, the result is as shown in table 1, the catalytic performance result of the potassium nitrate doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the potassium nitrate doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Fig. 9 be the carbonitride photochemical catalyst that mixes of the potassium nitrate of the embodiment of the invention 7 preparation can spectrogram.
Embodiment 8
, and add 10g urea in the potassium sulfate solution and fully stir and evenly mix 0.158g potassium sulfate dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 2h under 500 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that the present invention is obtained carries out SEM face scanning analysis, and the result contain potassium, oxygen, sulphur, carbon and nitrogen element in the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes, and doped chemical is evenly distributed as seen from Figure 20.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [K 2SO 4] 0.07[C 3N 4] 0.93
The present invention carries out tem analysis with the potassium sulfate doping carbonitride photochemical catalyst that obtains, the result as shown in figure 10, as seen from Figure 10, the potassium sulfate doping carbonitride photochemical catalyst that present embodiment obtains is that two-dimensional nano is laminar structured, and potassium sulfate doping carbonitride does not damage the body construction of carbonitride.
The present invention is used for removal to NO with the potassium sulfate doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g potassium sulfate doping carbonitride photochemical catalyst that embodiment 8 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone potassium sulfate doping carbonitride photochemical catalyst, the clearance that obtains NO is 43.2%, the result is as shown in table 1, the catalytic performance result of the potassium sulfate doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the potassium sulfate doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Figure 11 be the carbonitride photochemical catalyst that mixes of the potassium sulfate of the embodiment of the invention 8 preparation can spectrogram.
Embodiment 9
, and add the single cyanogen ammonia of 4g in the solution of potassium carbonate and fully stir and evenly mix 0.213g potash dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 3h under 480 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [K 2CO 3] 0.05[C 3N 4] 0.95
The present invention carries out XRD analysis with the potash doping carbonitride photochemical catalyst that obtains, the result as shown in figure 12, Figure 12 is the XRD collection of illustrative plates of the potash doping carbonitride photochemical catalyst of the embodiment of the invention 9 preparations, as seen from Figure 12, the thing of the potash doping carbonitride photochemical catalyst that obtains of present embodiment is C mutually 3N 4
The present invention is used for removal to NO with the potash doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g potash doping carbonitride photochemical catalyst that embodiment 9 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone potash doping carbonitride photochemical catalyst, the clearance that obtains NO is 40.5%, the result is as shown in table 1, the catalytic performance result of the potash doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the potash doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 10
, and add 4g dicyan diamino in the potassium dihydrogen phosphate and fully stir and evenly mix 0.126g potassium dihydrogen phosphate dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 2h under 520 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [KH 2PO 4] 0.12[C 3N 4] 0.88
The present invention carries out UV-vis DRS with the potassium dihydrogen phosphate doping carbonitride photochemical catalyst that obtains and analyzes, the result as shown in figure 13, Figure 13 be the UV-vis DRS collection of illustrative plates of carbonitride photochemical catalyst of the potassium dihydrogen phosphate doping of the embodiment of the invention 10 preparations; The result shows that the energy gap of the potassium dihydrogen phosphate doping carbonitride photochemical catalyst of present embodiment preparation is 2.50eV, visible light is had significantly absorb.
The present invention is used for removal to NO with the potassium dihydrogen phosphate doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g potash doping carbonitride photochemical catalyst that embodiment 10 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone potassium dihydrogen phosphate doping carbonitride photochemical catalyst, the clearance that obtains NO is 38.7%, the result is as shown in table 1, the catalytic performance result of the potassium dihydrogen phosphate doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the potassium dihydrogen phosphate doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 11
, and add the 4g melamine in the barium chloride solution and fully stir and evenly mix 0.124g barium chloride dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 2h under 570 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [BaCl 2] 0.13[C 3N 4] 0.87
The present invention carries out sem analysis with the barium chloride doping carbonitride photochemical catalyst that obtains, the result as shown in figure 14, Figure 14 is the SEM photo of the carbonitride photochemical catalyst that mixes of the barium chloride of the embodiment of the invention 11 preparation; As seen from Figure 14, the barium chloride doping carbonitride photochemical catalyst that present embodiment obtains has stratiform two-dimensional nano chip architecture, and barium chloride doping carbonitride does not damage the structure of carbonitride.
The present invention is used for removal to NO with the barium chloride doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g barium chloride doping carbonitride photochemical catalyst that embodiment 11 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone barium chloride doping carbonitride photochemical catalyst, the clearance that obtains NO is 38.3%, the result is as shown in table 1, the catalytic performance result of the barium chloride doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the barium chloride doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 12
, and add the 4g cyanuric acid in the calcium chloride solution and fully stir and evenly mix 0.075g calcium chloride dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 3h under 500 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [CaCl 2] 0.06[C 3N 4] 0.94
The present invention carries out UV-vis DRS with the calcium chloride doping carbonitride photochemical catalyst that obtains and analyzes, the result as shown in figure 15, the result shows that the energy gap of the calcium chloride doping carbonitride photochemical catalyst of present embodiment preparation is 2.57eV, visible light is had significantly absorb.
The present invention is used for removal to NO with the calcium chloride doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g calcium chloride doping carbonitride photochemical catalyst that embodiment 12 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone calcium chloride doping carbonitride photochemical catalyst, the clearance that obtains NO is 37.6%, the result is as shown in table 1, the catalytic performance result of the calcium chloride doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the barium chloride doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 13
, and add the 10g thiocarbamide in the magnesium chloride solution and fully stir and evenly mix 0.103g magnesium chloride dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 3h under 570 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [MgCl 2] 0.08[C 3N 4] 0.92
The present invention carries out the removal of NO with the magnesium chloride doping carbonitride photochemical catalyst that obtains, the result as shown in figure 16, as seen from Figure 16, the clearance to NO of the ammonium iodide doping carbonitride photochemical catalyst that present embodiment obtains is 40.8%, than unadulterated carbonitride the removal of NO is had bigger enhancing.
The present invention is used for removal to NO with the magnesium chloride doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g magnesium chloride doping carbonitride photochemical catalyst that embodiment 13 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone magnesium chloride doping carbonitride photochemical catalyst, the clearance that obtains NO is 40.8%, the result is as shown in table 1, the catalytic performance result of the magnesium chloride doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the magnesium chloride doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 14
, and add 10g urea in the ammonium sulfate and fully stir and evenly mix 0.081g ammonium sulfate dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 4h under 470 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [(NH 4) 2SO 4] 0.15[C 3N 4] 0.85
The present invention carries out the removal of NO with the ammonium sulfate doping carbonitride photochemical catalyst that obtains, the result as shown in figure 17, as seen from Figure 17, the clearance to NO of the ammonium sulfate doping carbonitride photochemical catalyst that present embodiment obtains is 44.1%, than unadulterated carbonitride the removal of NO is had bigger enhancing.
The present invention is used for removal to NO with the ammonium sulfate doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g ammonium sulfate doping carbonitride photochemical catalyst that embodiment 14 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone ammonium sulfate doping carbonitride photochemical catalyst, the clearance that obtains NO is 44.1%, the result is as shown in table 1, the catalytic performance result of the ammonium sulfate doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the ammonium sulfate doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 15
, and add the single cyanogen ammonia of 4g in the ammonium nitrate solution and fully stir and evenly mix 0.061g ammonium nitrate dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 4h under 600 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [NH 4NO 3] 0.09[C 3N 4] 0.91
The present invention carries out the removal of NO with the ammonium nitrate doping carbonitride photochemical catalyst that obtains, the result as shown in figure 18, as seen from Figure 18, the clearance to NO of the ammonium nitrate doping carbonitride photochemical catalyst that present embodiment obtains is 46.9%, than unadulterated carbonitride the removal of NO is had bigger enhancing.
The present invention is used for removal to NO with the ammonium nitrate doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g ammonium nitrate doping carbonitride photochemical catalyst that embodiment 15 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone ammonium nitrate doping carbonitride photochemical catalyst, the clearance that obtains NO is 46.9%, the result is as shown in table 1, the catalytic performance result of the ammonium nitrate doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the ammonium nitrate doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Embodiment 16
, and add 4g dicyan diamino in the sal volatile and fully stir and evenly mix 0.074g ammonium carbonate dissolving with deionized water.With the mixture of gained after oven dry under 60 ℃ of conditions, heat treatment 3h under 550 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The photochemical catalyst that obtains is carried out XRD and XPS analysis, and the result shows.The molecular formula of the carbonitride photochemical catalyst that the inorganic ions of present embodiment preparation mixes is [(NH 4) 2CO 3] 0.05[C 3N 4] 0.95
The present invention carries out PL with the ammonium nitrate doping carbonitride photochemical catalyst that obtains and analyzes, the result as shown in figure 19, the result shows that the pure carbonitride photochemical catalyst of PL strength ratio of the ammonium nitrate doping carbonitride photochemical catalyst of present embodiment preparation obviously reduces, and light induced electron and separating of hole are enhanced; The present invention carries out the removal of NO with the ammonium carbonate doping carbonitride photochemical catalyst that obtains, the result as shown in figure 20, as seen from Figure 20, the clearance to NO of the ammonium carbonate doping carbonitride photochemical catalyst that present embodiment obtains is 38.6%, than unadulterated carbonitride the removal of NO is had bigger enhancing.
The present invention is used for removal to NO with the ammonium carbonate doping carbonitride photochemical catalyst that obtains, detailed process is as follows: be 60% in relative humidity, oxygen content is under 21% the condition, the 0.2g ammonium carbonate doping carbonitride photochemical catalyst that embodiment 16 is obtained places the NO Continuous Flow, the initial concentration of NO is 650ppb, gas flow is 2.4L/min, adopt the halogen tungsten lamp of 100W, and adopt the edge filter filtering ultraviolet light of 420nm, visible light transmissive is shone ammonium carbonate doping carbonitride photochemical catalyst, the clearance that obtains NO is 38.6%, the result is as shown in table 1, the catalytic performance result of the ammonium carbonate doping carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the ammonium carbonate doping carbonitride photochemical catalyst of present embodiment preparation has higher removal to NO under visible light radiation, illustrate that it has higher visible light catalysis activity.
Comparative example 1
With deionized water the single cyanogen ammonia of 4g is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 2h under 550 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The carbonitride photochemical catalyst that the comparative example that obtains is prepared carries out the PL analysis, the result as shown in Figure 2, the result shows that the pure carbonitride photochemical catalyst of PL strength ratio of the potassium chloride doping carbonitride photochemical catalyst of present embodiment preparation obviously reduces, and light induced electron and separating of hole are enhanced.
The potassium chloride doping carbonitride photochemical catalyst that provides according to embodiment 1 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 20.5% to the clearance of NO.
Comparative example 2
With deionized water 4g dicyan diamino is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 3h under 500 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The KBr doping carbonitride photochemical catalyst that provides according to embodiment 2 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 25.3% to the clearance of NO.
Comparative example 3
With deionized water the 4g melamine is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 4h under 520 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The KI doping carbonitride photochemical catalyst that provides according to embodiment 3 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 27.8% to the clearance of NO.
Comparative example 4
With deionized water the 4g cyanuric acid is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 3h under 560 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The ammonium chloride doping carbonitride photochemical catalyst that provides according to embodiment 4 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 26.1% to the clearance of NO.
Comparative example 5
With deionized water the 10g thiocarbamide is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 2h under 580 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The ammonium bromide doping carbonitride photochemical catalyst that provides according to embodiment 5 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 26.8% to the clearance of NO.
Comparative example 6
With deionized water 10g urea is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 3h under 600 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The ammonium iodide doping carbonitride photochemical catalyst that provides according to embodiment 6 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 36.2% to the clearance of NO.
Comparative example 7
With deionized water the 10g thiocarbamide is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 4h under 600 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The potassium nitrate doping carbonitride photochemical catalyst that provides according to embodiment 7 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 33.5% to the clearance of NO.
Comparative example 8
With deionized water 10g urea is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 2h under 600 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The potassium sulfate doping carbonitride photochemical catalyst that provides according to embodiment 8 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 31.7% to the clearance of NO.
Comparative example 9
With deionized water the single cyanogen ammonia of 4g is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 3h under 480 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The potash doping carbonitride photochemical catalyst that provides according to embodiment 9 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 28.6% to the clearance of NO.
Comparative example 10
With deionized water 4g dicyan diamino is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 2h under 520 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The potassium dihydrogen phosphate doping carbonitride photochemical catalyst that provides according to embodiment 10 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 26.5% to the clearance of NO.
Comparative example 11
With deionized water the 4g melamine is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 3h under 570 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The barium chloride doping carbonitride photochemical catalyst that provides according to embodiment 11 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 27.2% to the clearance of NO.
Comparative example 12
With deionized water the 4g cyanuric acid is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 2h under 500 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The calcium chloride doping carbonitride photochemical catalyst that provides according to embodiment 12 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 25.4% to the clearance of NO.
Comparative example 13
With deionized water the 10g thiocarbamide is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 3h under 570 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The magnesium chloride doping carbonitride photochemical catalyst that provides according to embodiment 13 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 29.6% to the clearance of NO.
Comparative example 14
With deionized water 10g urea is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 4h under 480 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The ammonium sulfate doping carbonitride photochemical catalyst that provides according to embodiment 14 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 32.9% to the clearance of NO.
Comparative example 15
With deionized water the single cyanogen ammonia of 4g is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 4h under 600 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The ammonium nitrate doping carbonitride photochemical catalyst that provides according to embodiment 15 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 34.7% to the clearance of NO.
Comparative example 16
With deionized water 4g dicyan diamino is dissolved the back after oven dry under 60 ℃ of conditions, heat treatment 3h under 550 ℃ of conditions.After treating that temperature is cooled to room temperature, product is milled into powder with standby.
The carbonitride photochemical catalyst that the comparative example that obtains is prepared carries out the PL analysis, the result as shown in figure 17, the result shows that the pure carbonitride photochemical catalyst of PL strength ratio of the potassium chloride doping carbonitride photochemical catalyst of present embodiment preparation obviously reduces, and light induced electron and separating of hole are enhanced.
The ammonium carbonate doping carbonitride photochemical catalyst that provides according to embodiment 16 is to the removal method of NO, the catalytic performance of the carbonitride photochemical catalyst that this comparative example is obtained detects, the result is as shown in table 1, the catalytic performance result of the carbonitride photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example, as can be seen from Table 1, the carbonitride photochemical catalyst of this comparative example preparation is relatively poor to the catalytic activity of visible light, under visible light radiation, only is 27.7% to the clearance of NO.
The catalytic performance result of the carbonitride series photocatalyst that table 1 embodiment of the invention and comparative example obtain
Numbering NO clearance (%)
Embodiment 1 31.3
Comparative example 1 20.5
Embodiment 2 38.5
Comparative example 2 25.3
Embodiment 3 39.7
Comparative example 3 27.8
Embodiment 4 38.4
Comparative example 4 26.1
Embodiment 5 39.1
Comparative example 5 26.8
Embodiment 6 48.7
Comparative example 6 36.2
Embodiment 7 44.6
Comparative example 7 33.5
Embodiment 8 43.2
Comparative example 8 31.7
Embodiment 9 40.5
Comparative example 9 28.6
Embodiment 10 38.7
Comparative example 10 26.5
Embodiment 11 38.3
Comparative example 11 27.2
Embodiment 12 37.6
Comparative example 12 25.4
Embodiment 13 40.8
Comparative example 13 29.6
Embodiment 14 44.1
Comparative example 14 32.9
Embodiment 15 46.9
Comparative example 15 34.7
Embodiment 16 38.6
Comparative example 16 27.7
As can be seen from Table 1, inorganic ions doping carbonitride photochemical catalyst provided by the invention has higher visible light catalysis activity.
As seen from the above embodiment, inorganic ions doping carbonitride photochemical catalyst provided by the invention has the molecular formula shown in the formula (I): [X] m[C 3N 4] (1-m)(I); Wherein, m is 1%～50%.The present invention with single cyanogen ammonia, dicyan diamino, melamine, cyanuric acid, thiocarbamide or urea as the preparation carbonitride raw material, with potassium chloride, KBr, KI, ammonium chloride, ammonium bromide, ammonium iodide, potassium nitrate, potassium sulfate, potash, potassium dihydrogen phosphate, calcium chloride, magnesium chloride, barium chloride, ammonium sulfate, ammonium nitrate or ammonium carbonate as inorganic salt raw material.The preparation raw material of carbonitride and inorganic salt raw material are fully mixed the back under 60 ℃ of conditions, dry in the aqueous solution, heat treatment under hot conditions again, the inorganic ions doping carbonitride photochemical catalyst of the molecular formula shown in (I) that obtains having formula.C provided by the invention 3N 4In the photochemical catalyst, inorganic ions enters into C 3N 4Lattice in or in the interbed, the doping of inorganic ions exists makes C provided by the invention 3N 4Photochemical catalyst has higher visible light catalysis activity.Experiment shows, the inorganic ions doping C with two-dimensional structure provided by the invention 3N 4The visible light catalysis activity of photochemical catalyst is the C that do not mix 3N 41.5～3 times of photochemical catalyst.In addition, preparation method's mild condition provided by the invention, simple to operate, be beneficial to its large-scale production.
The above only is preferred embodiment of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (10)

1. the carbonitride photochemical catalyst that mixes of an inorganic ions has the molecular formula shown in the formula (I):
[X] m[C 3N 4] (1-m) （I）；
Wherein, m is 1%～40%;
X is KCl, KBr, KI, NH 4Cl, NH 4Br, NH 4I, KNO 3, K 2SO 4, K 2CO 3, KH 2PO 4, CaCl 2, MgCl 2, BaCl 2, (NH 4) 2SO 4, NH 4NO 3Or (NH 4) 2CO 3
2. the carbonitride photochemical catalyst that mixes according to the described inorganic ions of claim 1 is characterized in that described m is 2%～20%.
3. the preparation method of the carbonitride photochemical catalyst that mixes of an inorganic ions may further comprise the steps:
Carbon nitrogen source and inorganic salts are fully mixed the back oven dry in the aqueous solution, calcine, the carbonitride photochemical catalyst that the inorganic ions of the molecular formula shown in (I) that obtains having formula mixes:
[X] m[C 3N 4] (1-m) （I）；
Wherein, m is 1%～20%.
4. preparation method according to claim 3 is characterized in that, described carbon nitrogen source is single cyanogen ammonia, dicyanodiamine, melamine, cyanuric acid, thiocarbamide or urea.
5. preparation method according to claim 3 is characterized in that, described inorganic salts are KCl, KBr, KI, NH 4Cl, NH 4Br, NH 4I, KNO 3, K 2SO 4, K 2CO 3, KH 2PO 4, CaCl 2, MgCl 2, BaCl 2, (NH 4) 2SO 4, NH 4NO 3Or (NH 4) 2CO 3
6. preparation method according to claim 3 is characterized in that, the mass ratio of described carbon nitrogen source and described inorganic salts is 1:(0.01～0.4).
7. preparation method according to claim 6 is characterized in that, the mass ratio of described carbon nitrogen source and described inorganic salts is 1:(0.02～0.2).
8. preparation method according to claim 3 is characterized in that, described bake out temperature is 40～70 ℃.
9. preparation method according to claim 8 is characterized in that, described calcining heat is 400～650 ℃.
10. preparation method according to claim 3 is characterized in that, described calcination time is 0.5～10h.
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