CN109999879A - A kind of lamellar graphite phase carbon nitride photochemical catalyst and preparation method thereof of selenium auxiliary - Google Patents
A kind of lamellar graphite phase carbon nitride photochemical catalyst and preparation method thereof of selenium auxiliary Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 26
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 22
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 18
- 239000010439 graphite Substances 0.000 title claims abstract description 18
- 239000003054 catalyst Substances 0.000 title claims abstract description 17
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 12
- 239000011669 selenium Substances 0.000 title claims abstract description 12
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004202 carbamide Substances 0.000 claims abstract description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 239000000919 ceramic Substances 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 238000007146 photocatalysis Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000011941 photocatalyst Substances 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 description 14
- 230000015556 catabolic process Effects 0.000 description 12
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 11
- 229940043267 rhodamine b Drugs 0.000 description 9
- 239000010410 layer Substances 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000003344 environmental pollutant Substances 0.000 description 6
- 231100000719 pollutant Toxicity 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000003823 mortar mixing Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
A kind of lamellar graphite phase carbon nitride photochemical catalyst and preparation method thereof of selenium auxiliary, belongs to photocatalyst material preparation technical field.It is by nitrogenous precursor (dicyandiamide first, melamine, or mixtures thereof urea) with elemental selenium dispersion in ethanol, selenium is 5~15% relative to the mass percent of nitrogenous precursor, is sufficiently stirred to be placed in baking oven at room temperature and dries and removes solvent, it grinds and is transferred in ceramic crucible, it is placed in Muffle furnace and heats, be heated to 550~650 DEG C and keep the temperature 2~5 hours, after Muffle furnace is cooled to room temperature, product is fully ground, graphite phase carbon nitride powder can be obtained.This method preparation process is simple, equipment investment is small, it is with short production cycle, it is low in cost, yield is high, and obtained photochemical catalyst has in terms of photocatalysis effect and is obviously improved, furthermore, carbonitride has very high thermal stability and solvent stability, therefore is expected to realize the target of large-scale industry preparation and application.
Description
Technical field
The invention belongs to photocatalyst material preparation technical fields, and in particular to a kind of lamellar graphite phase carbon nitride of selenium auxiliary
Photochemical catalyst and preparation method thereof.
Background technique
With development in science and technology and social progress, energy crisis with environmental pollution is getting worse.Sun optical drive is urged
This inexhaustible energy of solar energy can be efficiently used by changing reaction, mainly include following several types: light
It is catalyzed contaminant degradation, photodissociation aquatic products hydrogen/production oxygen, the conversion of photocatalysis carbon dioxide, photocatalysis sterilization and organic reaction.Cause
This, light-catalyzed reaction is for solving the problems, such as that energy and environment have very big potentiality and application value.In past 40 years,
Light-catalyzed reaction is quickly grown as a kind of green technology.Conventional semiconductors such as titanium dioxide (TiO2) it is widely used in light
Catalytic field, but due to its greater band gap (3.2eV), ultraviolet light wave band can only be absorbed, and ultraviolet light is only accounted for and is shined upon
The 3% of the sunlight of earth surface, therefore, preparing high-efficient visible-light photocatalyst can effectively improve utilization to sunlight
Rate.
No nitride metal carbon material is important a member in carbon material family, in different types of carbon nitride material, stone
Black phase carbon nitride (g-C3N4) due to physical and chemical stability with higher, it prepares raw material and inexpensively enriches, preparation process is simple,
Its band gap is about 2.7eV, and there is visible light-responded ability to be therefore applied in photocatalysis field.However, visible light-responded
The disadvantages of poor, specific surface area is small, and photo-generated carrier recombination rate is fast cause the photocatalysis effect of graphite phase carbon nitride material compared with
Difference limits its large-scale application.
Therefore, preparation has the graphite phase carbon nitride photochemical catalyst of high efficiency photocatalysis effect, improves visible light utilization efficiency, increases
Add specific surface area, improve light induced electron/hole separative efficiency, is current carbon nitride material research to improve photocatalysis efficiency
The emphasis and Hot Contents in field.
Summary of the invention
The present invention is to carry out pyrolytic reaction using elemental selenium and nitrogenous precursor dicyandiamide etc., to prepare high-efficiency silicon nitride carbon
Photochemical catalyst.Nitrogenous small molecule melamine, urea other than dicyandiamide has also been attempted in we, same that elemental selenium is used to assist
Method, also available high-efficiency silicon nitride carbon photochemical catalyst.We have selected the temperature of suitable raw material proportioning and pyrolytic reaction
To prepare series of silicon nitride carbon product.
This have the advantage that: graphite phase carbon nitride catalysis material preparation process is simple, and equipment investment is small, production
Period is short, low in cost, and yield is high, and obtained photochemical catalyst has in terms of photocatalysis effect and is obviously improved, in addition, nitrogen
Changing carbon has very high thermal stability and solvent stability, therefore is expected to realize the target of large-scale industry preparation and application.
Of the invention comprises the concrete steps that:
1) 10g nitrogenous precursor (or mixtures thereof dicyandiamide, melamine, urea) and 0.5~1.5g elemental selenium are weighed,
It is dispersed in 50mL ethyl alcohol, room temperature magnetic agitation is uniformly mixed it;
2) by step 1) product, heat drying removes solvent at 50~80 DEG C, by obtained desciccate in agate mortar
Middle grinding;
3) product after step 2) grinding is transferred in ceramic crucible, is heated to 550~650 DEG C of (heating speed in Muffle furnace
Degree is 10~20 DEG C/min), soaking time is 2~5 hours, naturally cools to room temperature after reaction;Reaction product is taken out,
It is fully ground in the agate mortar again, to obtain the stratiform stone of the selenium auxiliary of yellow or light brown of the present invention
Black phase carbon nitride photochemical catalyst.
Detailed description of the invention
Fig. 1: scanning electron microscope (SEM) figure of carbonitride sample CN-10-650 in embodiment 1;
Fig. 2: transmission electron microscope (TEM) figure of carbonitride sample CN-10-650 in embodiment 1 has and is similar to graphene
Stratiform appearance structure, there is apparent difference with the block structure of body phase carbon nitride material.Due to the addition of selenium, presoma exists
During pyrolysis, the hydrogen bond in the Van der Waals force and layer of part interlayer is destroyed, and effectively removes unstable region, thus shape
Layered structure;
Fig. 3: X-ray diffraction (XRD) map of carbonitride sample CN-10-650 in embodiment 1, it is apparent with 2
Diffraction maximum, corresponds to the graphite of 3-s- triazine ring (100) structure and the accumulation of interlayer aromatic rings in layer by respectively 13.2 ° and 27.5 °
Carbon (002) crystal face, it was demonstrated that the formation of the basic structure of graphite phase carbon nitride.;
Fig. 4: uv drs (DRS) figure of carbonitride sample CN-10-650 in embodiment 1 has and typically partly leads
Body absorption characteristic, and there is visible light absorption capacity;
Fig. 5: the Tauc plot curve of carbonitride sample CN-10-650, band gap magnitude 2.66eV in embodiment 1;
Fig. 6: the fluorescence spectra of carbonitride sample CN-10-650 in embodiment 1, a length of 350 nanometers of optimum excitation wave, most
Good launch wavelength is 524 nanometers.And under the excitation of portable ultraviolet lamp (365 nanometers), product CN-10-650 is sent out with fluorescence
Penetrate property;
Fig. 7: the shape of three exponential dampings is presented in the fluorescence decay spectrogram of carbonitride sample CN-10-650 in embodiment 1
Formula, excitation wavelength are 360 nanometers, and the mean fluorecence service life is 18.17ns;
Fig. 8: the transient photocurrents response curve of carbonitride sample CN-10-650 in embodiment 1 (is received λ > 420 in illumination
Rice) under conditions of, current density increases;And when there is no light, current density is then reduced rapidly, it was demonstrated that CN-10-650 has excellent
Different photoelectric respone property;
Fig. 9: the UV-visible spectrum of photocatalytic degradation rhodamine B in embodiment 1, with the increase of light application time, absorption value
It gradually becomes smaller, after illumination in 30 minutes (λ > 420 nanometer), the rhodamine B more than 99% is degraded;
Figure 10: thermogravimetric analysis (TGA) curve of dicyandiamide, elemental selenium and its mixture, products therefrom yield in embodiment 1
Up to 31%, it was demonstrated that this method yield is higher and is expected to be applied in large-scale industrial production;
Figure 11: the scanning electron microscope (SEM) photograph of carbonitride sample CN-10-550 in embodiment 2, with porous laminated structure;
Figure 12: the transmission electron microscope picture of carbonitride sample CN-10-550 in embodiment 2, with porous laminated structure;
Figure 13: the X ray diffracting spectrum of carbonitride sample CN-10-550 in embodiment 2 has 2 apparent diffraction
Peak, corresponds to the graphitic carbon of 3-s- triazine ring (100) structure and the accumulation of interlayer aromatic rings in layer by respectively 13.2 ° and 27.5 °
(002) crystal face, it was demonstrated that the formation of the basic structure of graphite phase carbon nitride;
Figure 14: the transmission electron microscope picture of carbonitride sample CN-5-650 in embodiment 3, with layer structure;
Figure 15: the transmission electron microscope picture of carbonitride sample CN-15-650 in embodiment 4, with layer structure;
Figure 16: the transmission electron microscope picture of carbonitride sample CNM-10-550 in embodiment 5, with porous laminated structure;
Figure 17: the transmission electron microscope picture of carbonitride sample CNDU-10-650 in embodiment 6, with layer structure and size
Reduced.
Specific embodiment
Embodiment 1
Weigh 10g dicyandiamide solid (Shanghai Aladdin biochemical technology limited liability company) and 1g selenium powder (Shanghai Mike woods
Biochemical technology Co., Ltd) in 100mL beaker, 50mL ethyl alcohol is added and magneton is added, it is small that 1 is stirred on magnetic stirring apparatus
When.Then suspension is put into drying in 60 DEG C of baking ovens, after sufficiently drying, mixture grinding is made it sufficiently with agate mortar
Mixing.Gained presoma solid is transferred in 50mL ceramic crucible, is placed in Muffle furnace and is heated to 650 DEG C, heating rate is
15 DEG C/min, soaking time is 3 hours.After Muffle furnace cooled to room temperature, product is taken out, and abundant with agate mortar
Grinding is denoted as CN-10-650 to get graphite phase carbon nitride nanometer layer product is arrived.
Resulting graphite phase carbon nitride photochemical catalyst is used for photocatalytic pollutant degradation rhodamine B, the use of photochemical catalyst
Amount is 40mg, and the volume of rhodamine B solution is 100mL, and initial concentration is 10ppm, and light source is 300w xenon lamp (λ > 420 nanometer),
Degradation process meets first order reaction rate equation dynamics:
ln(Ct/C0)=- kt
Wherein C0It is the initial concentration of substrate, CtThe concentration of substrate, passes through uv-visible absorption spectra when being light application time t
Instrument can measure substrate Rhodamine B absorption spectrum, and replace its concentration with the ratio between 554 nanometers of its maximum absorption wavelength absorbance value
The ratio between, and then available degradation reaction rate constants k, numerical value can be used as measure rate of photocatalytic oxidation speed according to
According to.CN-10-650 is 13.63h for the rate of photocatalytic oxidation constant of rhodamine B-1。
Embodiment 2
Carbonitride preparation method and light degradation experiment parameter are as described in Example 1;
Wherein, selenium powder quality is 1g, and heating temperature is 550 DEG C, and products therefrom is denoted as CN-10-550.It is for pollutant
The degradation rate constant of rhodamine B is 2.40h-1。
Embodiment 3
Carbonitride preparation method and light degradation experiment parameter are as described in Example 1;
Wherein, selenium powder quality is 0.5g, and products therefrom is denoted as CN-5-650.Its degradation speed for pollutant rhodamine B
Rate constant is 10.40h-1。
Embodiment 4
Carbonitride preparation method and light degradation experiment parameter are as described in Example 1;
Wherein, selenium powder quality is 1.5g, and products therefrom is denoted as CN-15-650.Its degradation speed for pollutant rhodamine B
Rate constant is 9.13h-1。
Embodiment 5
Carbonitride preparation method and light degradation experiment parameter are as described in Example 1;
Wherein, nitrogenous precursor is melamine solid (Shanghai Aladdin biochemical technology limited liability company), quality
For 10g, heating temperature is 550 DEG C, and products therefrom is denoted as CNM-10-550.It is normal for the degradation rate of pollutant rhodamine B
Number is 3.31h-1。
Embodiment 6
Carbonitride preparation method and light degradation experiment parameter are as described in Example 1;
Wherein, nitrogenous precursor is 5g dicyandiamide and 5g urea (Beijing Chemical Plant) mixture, and product is denoted as CNDU-10-
650.It is 20.27h for the degradation rate constant of pollutant rhodamine B-1。
Claims (4)
1. a kind of preparation method of the lamellar graphite phase carbon nitride photochemical catalyst of selenium auxiliary, its step are as follows:
1) 10g nitrogenous precursor and 0.5~1.5g elemental selenium are weighed, is dispersed in 50mL ethyl alcohol, room temperature magnetic agitation keeps it mixed
It closes uniform;
2) by step 1) product, heat drying removes solvent at 50~80 DEG C, and obtained desciccate is ground in the agate mortar
Mill;
3) product after step 2) grinding is transferred in ceramic crucible, is heated to 550~650 DEG C in Muffle furnace, soaking time 2
~5 hours, room temperature was naturally cooled to after reaction;Reaction product is taken out, then is fully ground in the agate mortar, from
And obtain the lamellar graphite phase carbon nitride photochemical catalyst of selenium auxiliary.
2. a kind of preparation method of the lamellar graphite phase carbon nitride photochemical catalyst of selenium auxiliary as described in claim 1, feature
Be: nitrogenous precursor is or mixtures thereof dicyandiamide, melamine, urea.
3. a kind of preparation method of the lamellar graphite phase carbon nitride photochemical catalyst of selenium auxiliary as described in claim 1, feature
Be: the heating rate heated in Muffle stove heating is 10~20 DEG C/min.
4. a kind of lamellar graphite phase carbon nitride photochemical catalyst of selenium auxiliary, it is characterised in that: be by claims 1 to 3 any one
Method described in is prepared.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111085235A (en) * | 2019-12-27 | 2020-05-01 | 扬州大学 | Environment catalyst for visible light catalytic degradation of aldehydes and synthesis method thereof |
CN111790441A (en) * | 2020-07-03 | 2020-10-20 | 扬州大学 | Polyaniline loaded copper-iron catalyst material and preparation method and application thereof |
CN113289659A (en) * | 2021-05-25 | 2021-08-24 | 西安工程大学 | Preparation method and application of sulfonic functional group modified carbon nitride photocatalytic material |
CN115845902A (en) * | 2022-12-08 | 2023-03-28 | 上海交通大学深圳研究院 | Graphite phase carbon nitride photocatalytic material and preparation method thereof |
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CN104391062A (en) * | 2014-10-31 | 2015-03-04 | 厦门大学 | Method for preparing g-C3N4 coating on solid-phase microextraction head |
CN107398292A (en) * | 2017-05-23 | 2017-11-28 | 哈尔滨理工大学 | A kind of preparation method of selenides/graphite phase carbon nitride photocatalysis composite |
CN108226121A (en) * | 2018-01-24 | 2018-06-29 | 吉林大学 | A kind of double fluorescent emission test paper of gold nanoclusters base, preparation method and its application in Cu2+ detections |
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CN111085235A (en) * | 2019-12-27 | 2020-05-01 | 扬州大学 | Environment catalyst for visible light catalytic degradation of aldehydes and synthesis method thereof |
CN111085235B (en) * | 2019-12-27 | 2022-10-14 | 扬州大学 | Environment catalyst for visible light catalytic degradation of aldehydes and synthesis method thereof |
CN111790441A (en) * | 2020-07-03 | 2020-10-20 | 扬州大学 | Polyaniline loaded copper-iron catalyst material and preparation method and application thereof |
CN111790441B (en) * | 2020-07-03 | 2022-10-25 | 扬州大学 | Polyaniline loaded copper-iron catalyst material and preparation method and application thereof |
CN113289659A (en) * | 2021-05-25 | 2021-08-24 | 西安工程大学 | Preparation method and application of sulfonic functional group modified carbon nitride photocatalytic material |
CN113289659B (en) * | 2021-05-25 | 2023-09-01 | 西安工程大学 | Preparation method and application of sulfonic functional group modified carbon nitride photocatalytic material |
CN115845902A (en) * | 2022-12-08 | 2023-03-28 | 上海交通大学深圳研究院 | Graphite phase carbon nitride photocatalytic material and preparation method thereof |
CN115845902B (en) * | 2022-12-08 | 2024-04-19 | 上海交通大学深圳研究院 | Graphite-phase carbon nitride photocatalytic material and preparation method thereof |
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