CN113769771B - Graphite-phase carbon nitride photocatalyst for sewage treatment and preparation method and application thereof - Google Patents
Graphite-phase carbon nitride photocatalyst for sewage treatment and preparation method and application thereof Download PDFInfo
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- CN113769771B CN113769771B CN202110938930.1A CN202110938930A CN113769771B CN 113769771 B CN113769771 B CN 113769771B CN 202110938930 A CN202110938930 A CN 202110938930A CN 113769771 B CN113769771 B CN 113769771B
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 148
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 96
- 239000010865 sewage Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 11
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000007787 solid Substances 0.000 claims abstract description 21
- -1 ethylenediamine tetraacetic acid modified graphite Chemical class 0.000 claims abstract description 12
- 239000012071 phase Substances 0.000 claims description 113
- 239000002243 precursor Substances 0.000 claims description 68
- 238000000034 method Methods 0.000 claims description 51
- 238000005406 washing Methods 0.000 claims description 44
- 238000001816 cooling Methods 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- 238000001914 filtration Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 20
- 239000006228 supernatant Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 14
- 239000012298 atmosphere Substances 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 13
- 239000002244 precipitate Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 11
- 239000007790 solid phase Substances 0.000 claims description 11
- 229910001220 stainless steel Inorganic materials 0.000 claims description 11
- 239000010935 stainless steel Substances 0.000 claims description 11
- 229920000877 Melamine resin Polymers 0.000 claims description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical group NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- 239000003344 environmental pollutant Substances 0.000 claims description 2
- 231100000719 pollutant Toxicity 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 8
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000969 carrier Substances 0.000 abstract description 7
- 239000003054 catalyst Substances 0.000 abstract description 6
- 229910002804 graphite Inorganic materials 0.000 abstract description 6
- 239000010439 graphite Substances 0.000 abstract description 6
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 3
- 229960001484 edetic acid Drugs 0.000 description 58
- 230000000052 comparative effect Effects 0.000 description 15
- 239000012465 retentate Substances 0.000 description 10
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000000103 photoluminescence spectrum Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000006798 recombination Effects 0.000 description 5
- 238000005215 recombination Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000001052 transient effect Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010335 hydrothermal treatment Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- HZAXFHJVJLSVMW-UHFFFAOYSA-N monoethanolamine hydrochloride Natural products NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000005303 weighing 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
-
- B01J35/39—
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
-
- 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—
-
- B01J35/40—
-
- 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
-
- 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
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a graphite phase carbon nitride photocatalyst for sewage treatment and a preparation method and application thereof, wherein the photocatalyst comprises ethylenediamine tetraacetic acid modified graphite phase carbon nitride, the morphology of the ethylenediamine tetraacetic acid modified graphite phase carbon nitride is hollow tubular or solid rod-shaped, and the diameters of the hollow tubular and the solid rod-shaped are 1-10 mu m. The graphite-phase carbon nitride photocatalyst comprises ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, can realize targeted morphology regulation and control, and improves g-C 3 N 4 The specific surface area is small, the photo-generated carriers are seriously compounded, and the like, compared with the traditional g-C 3 N 4 The activity of the graphite phase carbon nitride photocatalyst for decomposing triethanolamine under the irradiation of visible light can be improved by 11.5 times at most, and the catalyst has the characteristic of high photocatalytic degradation of organic pollutants of alcohol amines.
Description
Technical Field
The invention belongs to the technical field of organic pollution treatment, and particularly relates to a graphite-phase carbon nitride photocatalyst for sewage treatment, and a preparation method and application thereof.
Background
The ethanolamine compound is a chemical raw material with wide application, is used as a surfactant, a humidifier for textiles and cosmetics, a dispersing agent for resin and rubber, and the like, and has wide application in modern industrial production. At present, most of waste water similar to alcohol amine-containing organic pollutants adopts a biochemical treatment method and a method combining chemical pretreatment and biochemistry. The alcohol amine wastewater is used as a sacrificial agent for photocatalytic reaction, is degraded by hole reaction generated by the photocatalyst, and cooperatively generates hydrogen, so that the method is an economical and effective method for treating the alcohol amine wastewater.
Graphite-like phase carbon nitride (g-C) 3 N 4 ) Is a novel organic photocatalyst. Such kind ofThe catalyst has low cost, simple synthesis process and narrow band gap (E) g =2.70 eV, can respond to visible light), has the characteristics of strong chemical stability, easy modification and the like, and is regarded as a very promising photocatalyst. Nevertheless, there are many disadvantages that limit its photocatalytic reactivity and more widely used, such as easy recombination of photogenerated electrons and holes, small specific surface area, etc. Therefore, in order to overcome these disadvantages, researchers have proposed a series of modification schemes such as morphology control, doping modification, copolymerization modification, etc. for improving g-C 3 N 4 Is used for the photocatalytic performance of the catalyst.
In the prior modification method and process, such as Chinese patent CN105478153A, the name is CeV0 4 /Ag/g-C 3 N 4 The technical characteristics of the patent lie in that g-C 3 N 4 Powder and CeV0 4 Respectively dissolving in ethanol, ultrasonic dispersing, mixing, and adding AgNO 3 Mixing the solutions, heating for evaporation, oven drying, and grinding to obtain CeV0 4 /Ag/g-C 3 N 4 The composite photocatalyst has the advantages of simple synthesis process, low raw material requirement, lack of morphology regulation and control and limited application range. For another example, chinese patent CN109046422A, named "a lamellar graphite-like phase carbon nitride g-C 3 N 4 Material and preparation method thereof, g-C prepared by the patent 3 N 4 The preparation method has the advantages of lamellar structure, simple flow, wide raw material sources, easy preparation of products and good repeatability, but the lack of regulation and control on the electronic structure and the limited application range.
Disclosure of Invention
The invention aims to solve the technical problems of the prior art and provides a graphite-phase carbon nitride photocatalyst for sewage treatment, and a preparation method and application thereof. The graphite-phase carbon nitride photocatalyst comprises ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, can realize targeted morphology regulation and control, and improves g-C 3 N 4 The specific surface area is small, the photo-generated carriers are seriously compounded, and the like, compared with the traditional g-C 3 N 4 Catalytic reactionThe activity of the graphite-phase carbon nitride photocatalyst for decomposing triethanolamine under the irradiation of visible light can be improved by 11.5 times at most, and the graphite-phase carbon nitride photocatalyst has the characteristic of high photocatalytic degradation of organic pollutants of alcohol amines.
In order to solve the technical problems, the invention adopts the following technical scheme: a graphite-phase carbon nitride photocatalyst for sewage treatment is characterized by comprising ethylenediamine tetraacetic acid modified graphite-phase carbon nitride.
The graphite-phase carbon nitride photocatalyst for sewage treatment is characterized in that the morphology of the ethylenediamine tetraacetic acid modified graphite-phase carbon nitride is hollow tubular or solid rod-shaped, and the diameters of the hollow tubular and the solid rod-shaped are 1-10 mu m.
In addition, the invention also provides a method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment, which is characterized in that the raw materials comprise a graphite-phase carbon nitride precursor and ethylenediamine tetraacetic acid, and the mass of the ethylenediamine tetraacetic acid is 0.2-20 times of that of the graphite-phase carbon nitride precursor.
The method is characterized in that the graphite-like carbon nitride precursor is melamine, dicyandiamide or urea.
The method is characterized by comprising the following steps:
adding deionized water into a hydrothermal kettle liner filled with a graphite-like carbon nitride precursor and ethylenediamine tetraacetic acid, and stirring to uniformly mix;
step two, placing the inner liner of the hydrothermal kettle provided with the mixed system in the step one into a stainless steel shell, sealing, and carrying out hydrothermal reaction for 1-20 h in a baking oven at 100-200 ℃;
step three, cooling the system after the hydrothermal reaction in the step two to the temperature of less than or equal to 25 ℃, centrifuging the cooled system, filtering, and washing and centrifuging the precipitate for 3 times;
step four, placing the solid phase after washing and centrifuging in a drying oven at 40-100 ℃ for drying treatment for 6-24 hours to obtain a photocatalyst precursor;
and fifthly, in the air atmosphere, heating the photocatalyst precursor in the fourth step to 500-550 ℃ at a heating rate of 2-10 ℃/min, and carrying out heat preservation roasting for 2-4 hours, and grinding to obtain the graphite-phase carbon nitride photocatalyst for sewage treatment.
The method is characterized in that in the third step, the cooling is performed in an air flow at 25 ℃ or in a water bath at 25 ℃.
The method is characterized in that the washing and centrifuging in the third step comprises washing the retentate with deionized water, centrifuging, and filtering out supernatant.
Furthermore, the invention also provides a method for catalytically treating alcohol amine-containing pollutants by using the graphite-phase carbon nitride photocatalyst for sewage treatment.
Compared with the prior art, the invention has the following advantages:
1. the graphite-phase carbon nitride photocatalyst comprises ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, can realize targeted morphology regulation and control, and improves g-C 3 N 4 The specific surface area is small, the photo-generated carriers are seriously compounded, and the like, compared with the traditional g-C 3 N 4 The activity of the graphite phase carbon nitride photocatalyst for decomposing triethanolamine under the irradiation of visible light can be improved by 11.5 times at most, and the catalyst has the characteristic of high photocatalytic degradation of organic pollutants of alcohol amines.
2. Preferably, the ethylenediamine tetraacetic acid modified graphite phase carbon nitride is hollow tubular or solid rod-shaped, has lower photon-generated carrier recombination rate and higher efficient electron transmission efficiency.
3. The method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment comprises the steps of carrying out hydrothermal treatment on raw materials including melamine, dicyandiamide or urea and other graphite-phase carbon nitride precursors and ethylenediamine tetraacetic acid, introducing chelating agent ethylenediamine tetraacetic acid in the hydrothermal treatment process, controlling the hydrothermal reaction temperature to be 100-200 ℃ for 1-20 h, cooling to be less than or equal to 25 ℃, and realizing morphology control of the photocatalyst by utilizing the chelation of ethylenediamine tetraacetic acid to prepare the photocatalyst with high photocatalytic activity.
4. The preparation method of the invention comprises the steps of heating the photocatalyst precursor in the fourth step to 500-550 ℃ at a heating rate of 2-10 ℃/min under air atmosphere, and carrying out heat preservation roasting for 2-4 h, so as to realize the regulation and control of the element proportion, the carried group, the crystallinity, the energy band position, the forbidden band width, the microcosmic morphology, the specific surface area, the pore characteristics and the like of the catalyst, realize lower photon-generated carrier recombination rate and higher efficient electron transmission efficiency.
5. Preferably, in the preparation method of the invention, the cooling is carried out in an air flow at 25 ℃ or in a water bath at 25 ℃ to prepare the modified graphite phase carbon nitride with a hollow tubular or solid rod-shaped special structure, and the modified graphite phase carbon nitride is endowed with modified performance.
The technical scheme of the invention is further described in detail below with reference to the accompanying drawings and the examples.
Drawings
FIG. 1 is a schematic flow chart of the preparation method of example 1.
Fig. 2 is an XRD spectrum of the graphite-phase carbon nitride photocatalyst of examples 1 to 2 and comparative example 1.
Fig. 3 is an SEM image of the graphite-phase carbon nitride photocatalyst of examples 1 to 2 and comparative example 1.
Fig. 4 is a TEM image of the graphite phase carbon nitride photocatalyst of example 1.
Fig. 5 is steady state and transient PL spectra of the graphite phase carbon nitride photocatalyst of example 1 and comparative example 1.
Fig. 6 is a graph showing photocurrent density curves of graphite-phase carbon nitride photocatalysts of examples 1 to 2 and comparative example 1.
Fig. 7 is a graph showing the comparison of the activities of the graphite-phase carbon nitride photocatalysts of examples 1 to 2 and comparative example 1 for decomposing triethanolamine under irradiation of visible light.
Detailed Description
Example 1
The embodiment provides a graphite-phase carbon nitride photocatalyst for sewage treatment, which comprises ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, wherein the ethylenediamine tetraacetic acid modified graphite-phase carbon nitride is hollow, and the diameter of the hollow tube is 1-10 mu m.
As shown in fig. 1, the embodiment also provides a method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment, wherein the raw materials of the method comprise a graphite-like carbon nitride precursor and ethylenediamine tetraacetic acid; the mass of the ethylenediamine tetraacetic acid is 0.2 times of that of the graphite-like phase carbon nitride precursor.
The graphite-like phase carbon nitride precursor is melamine.
The method comprises the following steps:
step one, adding 30mL of deionized water into a hydrothermal kettle liner with the volume of 100mL and filled with 5g of graphite-like carbon nitride precursor and 1g of ethylenediamine tetraacetic acid, and stirring to uniformly mix; the stirring time may be 30 minutes;
step two, placing the inner liner of the hydrothermal kettle provided with the mixed system in the step one into a stainless steel shell, sealing, and carrying out hydrothermal reaction in a 180 ℃ oven for 20 hours;
step three, cooling the system after the hydrothermal reaction in the step two to the temperature of less than or equal to 25 ℃, centrifuging the cooled system, filtering to remove supernatant, and washing and centrifuging the precipitate for 3 times; the cooling is cooling in an air stream at 25 ℃; the washing and centrifuging comprises the steps of washing the retentate with deionized water, centrifuging at a speed of 5000r/min, and filtering out supernatant;
step four, placing the solid phase obtained after washing and centrifuging in the step three in a 60 ℃ oven for drying treatment for 24 hours to obtain a photocatalyst precursor;
and fifthly, in the air atmosphere, heating the photocatalyst precursor in the fourth step to 520 ℃ at a heating rate of 5 ℃/min, preserving heat and roasting for 4 hours, and grinding to obtain the graphite-phase carbon nitride photocatalyst for sewage treatment, which is named MEH-10.
Example 2
The embodiment provides a graphite-phase carbon nitride photocatalyst for sewage treatment, which comprises ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, wherein the ethylenediamine tetraacetic acid modified graphite-phase carbon nitride is in a solid rod shape, and the diameter of the solid rod shape is 1-10 mu m.
The embodiment also provides a method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment, wherein the raw materials of the method comprise a graphite-like carbon nitride precursor and ethylenediamine tetraacetic acid; the mass of the ethylenediamine tetraacetic acid is 2 times of that of the graphite-like phase carbon nitride precursor.
The graphite-like phase carbon nitride precursor is melamine.
The method comprises the following steps:
step one, adding 30mL of deionized water into a hydrothermal kettle liner filled with 5g of graphite-like carbon nitride precursor and 10g of ethylenediamine tetraacetic acid, and stirring to uniformly mix; the stirring time may be 30 minutes;
step two, placing the inner liner of the hydrothermal kettle provided with the mixed system in the step one into a stainless steel shell, sealing, and carrying out hydrothermal reaction in a 180 ℃ oven for 20 hours;
step three, cooling the system after the hydrothermal reaction in the step two to the temperature of less than or equal to 25 ℃, centrifuging the cooled system, filtering to remove supernatant, and washing and centrifuging the precipitate for 3 times; the cooling is cooling in an air stream at 25 ℃; the washing and centrifuging comprises the steps of washing the retentate with deionized water, centrifuging at a speed of 5000r/min, and filtering out supernatant;
step four, placing the solid phase obtained after washing and centrifuging in the step three in a 60 ℃ oven for drying treatment for 24 hours to obtain a photocatalyst precursor;
and fifthly, in the air atmosphere, heating the photocatalyst precursor in the fourth step to 520 ℃ at a heating rate of 5 ℃/min, preserving heat and roasting for 4 hours, and grinding to obtain the graphite-phase carbon nitride photocatalyst for sewage treatment, which is named as MEH-100.
Example 3
The embodiment provides a graphite-phase carbon nitride photocatalyst for sewage treatment, which comprises ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, wherein the ethylenediamine tetraacetic acid modified graphite-phase carbon nitride is in a solid rod shape, and the diameter of the solid rod shape is 1-10 mu m.
The embodiment also provides a method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment, wherein the raw materials of the method comprise a graphite-like carbon nitride precursor and ethylenediamine tetraacetic acid; the mass of the ethylenediamine tetraacetic acid is 20 times of that of the graphite-like phase carbon nitride precursor.
The graphite-like phase carbon nitride precursor is melamine.
The method comprises the following steps:
step one, adding 30mL of deionized water into a hydrothermal kettle liner filled with 5g of graphite-like carbon nitride precursor and 100g of ethylenediamine tetraacetic acid, and stirring to uniformly mix; the stirring time may be 30 minutes;
step two, placing the inner liner of the hydrothermal kettle provided with the mixed system in the step one into a stainless steel shell, sealing, and performing hydrothermal reaction in a baking oven at 100 ℃ for 18 hours;
step three, cooling the system after the hydrothermal reaction in the step two to the temperature of less than or equal to 25 ℃, centrifuging the cooled system, filtering to remove supernatant, and washing and centrifuging the precipitate for 3 times; the cooling is carried out under the water bath condition of 25 ℃; the washing and centrifuging comprises the steps of washing the retentate with deionized water, centrifuging at a speed of 5000r/min, and filtering out supernatant;
step four, placing the solid phase after washing and centrifuging in the step three in a drying oven at 100 ℃ for drying treatment for 10 hours to obtain a photocatalyst precursor;
and fifthly, in the air atmosphere, heating the photocatalyst precursor in the fourth step to 500 ℃ at a heating rate of 2 ℃/min, preserving heat and roasting for 2 hours, and grinding to obtain the graphite-phase carbon nitride photocatalyst for sewage treatment.
Example 4
The embodiment provides a graphite-phase carbon nitride photocatalyst for sewage treatment, which comprises ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, wherein the ethylenediamine tetraacetic acid modified graphite-phase carbon nitride is hollow, and the diameter of the hollow tube is 1-10 mu m.
The embodiment also provides a method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment, wherein the raw materials of the method comprise a graphite-like carbon nitride precursor and ethylenediamine tetraacetic acid; the mass of the ethylenediamine tetraacetic acid is 0.2 times of that of the graphite-like phase carbon nitride precursor.
The graphite-like phase carbon nitride precursor is dicyandiamide.
The method comprises the following steps:
step one, adding 30mL of deionized water into a hydrothermal kettle liner filled with 5g of graphite-like carbon nitride precursor and 1g of ethylene diamine tetraacetic acid, and stirring to uniformly mix; the stirring time may be 30 minutes;
step two, placing the inner liner of the hydrothermal kettle provided with the mixed system in the step one into a stainless steel shell, sealing, and carrying out hydrothermal reaction in a baking oven at 100 ℃ for 20 hours;
step three, cooling the system after the hydrothermal reaction in the step two to the temperature of less than or equal to 25 ℃, centrifuging the cooled system, filtering to remove supernatant, and washing and centrifuging the precipitate for 3 times; the cooling is carried out under the water bath condition of 25 ℃; the washing and centrifuging comprises the steps of washing the retentate with deionized water, centrifuging at a speed of 5000r/min, and filtering out supernatant;
step four, placing the solid phase after washing and centrifuging in the step three in a baking oven at 40 ℃ for drying treatment for 20 hours to obtain a photocatalyst precursor;
and fifthly, in the air atmosphere, heating the photocatalyst precursor in the fourth step to 500 ℃ at a heating rate of 2 ℃/min, preserving heat and roasting for 2 hours, and grinding to obtain the graphite-phase carbon nitride photocatalyst for sewage treatment.
Example 5
The embodiment provides a graphite-phase carbon nitride photocatalyst for sewage treatment, which comprises ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, wherein the ethylenediamine tetraacetic acid modified graphite-phase carbon nitride is in a solid rod shape, and the diameter of the solid rod shape is 1-10 mu m.
The embodiment also provides a method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment, wherein the raw materials of the method comprise a graphite-like carbon nitride precursor and ethylenediamine tetraacetic acid; the mass of the ethylenediamine tetraacetic acid is 2 times of that of the graphite-like phase carbon nitride precursor.
The graphite-like phase carbon nitride precursor is dicyandiamide.
The method comprises the following steps:
step one, adding 30mL of deionized water into a hydrothermal kettle liner filled with 5g of graphite-like carbon nitride precursor and 10g of ethylenediamine tetraacetic acid, and stirring to uniformly mix; the stirring time may be 30 minutes;
step two, placing the inner liner of the hydrothermal kettle provided with the mixed system in the step one into a stainless steel shell, sealing, and carrying out hydrothermal reaction in a baking oven at 150 ℃ for 12 hours;
step three, cooling the system after the hydrothermal reaction in the step two to the temperature of less than or equal to 25 ℃, centrifuging the cooled system, filtering to remove supernatant, and washing and centrifuging the precipitate for 3 times; the cooling is carried out under the water bath condition of 25 ℃; the washing and centrifuging comprises the steps of washing the retentate with deionized water, centrifuging at a speed of 5000r/min, and filtering out supernatant;
step four, placing the solid phase after washing and centrifuging in the step three in a drying oven at 100 ℃ for drying treatment for 6 hours to obtain a photocatalyst precursor;
and fifthly, in the air atmosphere, heating the photocatalyst precursor in the fourth step to 520 ℃ at a heating rate of 5 ℃/min, preserving heat and roasting for 3 hours, and grinding to obtain the graphite-phase carbon nitride photocatalyst for sewage treatment.
Example 6
The embodiment provides a graphite-phase carbon nitride photocatalyst for sewage treatment, which comprises ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, wherein the ethylenediamine tetraacetic acid modified graphite-phase carbon nitride is in a solid rod shape, and the diameter of the solid rod shape is 1-10 mu m.
The embodiment also provides a method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment, wherein the raw materials of the method comprise a graphite-like carbon nitride precursor and ethylenediamine tetraacetic acid; the mass of the ethylenediamine tetraacetic acid is 20 times of that of the graphite-like phase carbon nitride precursor.
The graphite-like phase carbon nitride precursor is dicyandiamide.
The method comprises the following steps:
step one, adding 30mL of deionized water into a hydrothermal kettle liner filled with 5g of graphite-like carbon nitride precursor and 100g of ethylenediamine tetraacetic acid, and stirring to uniformly mix; the stirring time may be 30 minutes;
step two, placing the inner liner of the hydrothermal kettle provided with the mixed system in the step one into a stainless steel shell, sealing, and carrying out hydrothermal reaction in a baking oven at 200 ℃ for 1 h;
step three, cooling the system after the hydrothermal reaction in the step two to the temperature of less than or equal to 25 ℃, centrifuging the cooled system, filtering to remove supernatant, and washing and centrifuging the precipitate for 3 times; the cooling is carried out under the water bath condition of 25 ℃; the washing and centrifuging comprises the steps of washing the retentate with deionized water, centrifuging at a speed of 5000r/min, and filtering out supernatant;
step four, placing the solid phase obtained after washing and centrifuging in the step three in a 60 ℃ oven for drying treatment for 24 hours to obtain a photocatalyst precursor;
and fifthly, in the air atmosphere, heating the photocatalyst precursor in the fourth step to 550 ℃ at a heating rate of 10 ℃/min, preserving heat and roasting for 4 hours, and grinding to obtain the graphite-phase carbon nitride photocatalyst for sewage treatment.
Example 7
The embodiment provides a graphite-phase carbon nitride photocatalyst for sewage treatment, which comprises ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, wherein the ethylenediamine tetraacetic acid modified graphite-phase carbon nitride is hollow, and the diameter of the hollow tube is 1-10 mu m.
The hollow tube has a hollow tube diameter of 1 μm.
The embodiment also provides a method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment, wherein the raw materials of the method comprise a graphite-like carbon nitride precursor and ethylenediamine tetraacetic acid; the mass of the ethylenediamine tetraacetic acid is 10 times of that of the graphite-like phase carbon nitride precursor.
The graphite-like phase carbon nitride precursor is urea.
The method comprises the following steps:
step one, adding 30mL of deionized water into a hydrothermal kettle liner filled with 5g of graphite-like carbon nitride precursor and 50g of ethylenediamine tetraacetic acid, and stirring to uniformly mix; the stirring time may be 30 minutes;
step two, placing the inner liner of the hydrothermal kettle provided with the mixed system in the step one into a stainless steel shell, sealing, and carrying out hydrothermal reaction in a baking oven at 200 ℃ for 1 h;
step three, cooling the system after the hydrothermal reaction in the step two to the temperature of less than or equal to 25 ℃, centrifuging the cooled system, filtering to remove supernatant, and washing and centrifuging the precipitate for 3 times; the cooling is cooling in an air stream at 25 ℃; the washing and centrifuging comprises the steps of washing the retentate with deionized water, centrifuging at a speed of 5000r/min, and filtering out supernatant;
step four, placing the solid phase after washing and centrifuging in the step three in a drying oven at 100 ℃ for drying treatment for 6 hours to obtain a photocatalyst precursor;
and fifthly, in the air atmosphere, heating the photocatalyst precursor in the fourth step to 550 ℃ at a heating rate of 10 ℃/min, preserving heat, roasting for 3 hours, and grinding to obtain the graphite-phase carbon nitride photocatalyst for sewage treatment.
Example 8
The embodiment provides a graphite-phase carbon nitride photocatalyst for sewage treatment, which comprises ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, wherein the ethylenediamine tetraacetic acid modified graphite-phase carbon nitride is in a solid rod shape, and the diameter of the solid rod shape is 1-10 mu m.
The hollow tube has a hollow tube diameter of 1 μm.
The embodiment also provides a method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment, wherein the raw materials of the method comprise a graphite-like carbon nitride precursor and ethylenediamine tetraacetic acid; the mass of the ethylenediamine tetraacetic acid is 0.2 times of that of the graphite-like phase carbon nitride precursor.
The graphite-like phase carbon nitride precursor is urea.
The method comprises the following steps:
step one, adding 30mL of deionized water into a hydrothermal kettle liner filled with 5g of graphite-like carbon nitride precursor and 1g of ethylene diamine tetraacetic acid, and stirring to uniformly mix; the stirring time may be 30 minutes;
step two, placing the inner liner of the hydrothermal kettle provided with the mixed system in the step one into a stainless steel shell, sealing, and carrying out hydrothermal reaction in a baking oven at 100 ℃ for 20 hours;
step three, cooling the system after the hydrothermal reaction in the step two to the temperature of less than or equal to 25 ℃, centrifuging the cooled system, filtering to remove supernatant, and washing and centrifuging the precipitate for 3 times; the cooling is cooling in an air stream at 25 ℃; the washing and centrifuging comprises the steps of washing the retentate with deionized water, centrifuging at a speed of 5000r/min, and filtering out supernatant;
step four, placing the solid phase after washing and centrifuging in the step three in a baking oven at 40 ℃ for drying treatment for 10 hours to obtain a photocatalyst precursor;
and fifthly, in the air atmosphere, heating the photocatalyst precursor in the fourth step to 500 ℃ at a heating rate of 2 ℃/min, preserving heat and roasting for 4 hours, and grinding to obtain the graphite-phase carbon nitride photocatalyst for sewage treatment.
Example 9
The embodiment provides a graphite-phase carbon nitride photocatalyst for sewage treatment, which comprises ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, wherein the ethylenediamine tetraacetic acid modified graphite-phase carbon nitride is in a solid rod shape, and the diameter of the solid rod shape is 1-10 mu m.
The hollow tube has a hollow tube diameter of 1 μm.
The embodiment also provides a method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment, wherein the raw materials of the method comprise a graphite-like carbon nitride precursor and ethylenediamine tetraacetic acid; the mass of the ethylenediamine tetraacetic acid is 20 times of that of the graphite-like phase carbon nitride precursor.
The graphite-like phase carbon nitride precursor is urea.
The method comprises the following steps:
step one, adding 30mL of deionized water into a hydrothermal kettle liner filled with 5g of graphite-like carbon nitride precursor and 100g of ethylenediamine tetraacetic acid, and stirring to uniformly mix; the stirring time may be 30 minutes;
step two, placing the inner liner of the hydrothermal kettle provided with the mixed system in the step one into a stainless steel shell, sealing, and carrying out hydrothermal reaction in a baking oven at 150 ℃ for 10 hours;
step three, cooling the system after the hydrothermal reaction in the step two to the temperature of less than or equal to 25 ℃, centrifuging the cooled system, filtering to remove supernatant, and washing and centrifuging the precipitate for 3 times; the cooling is cooling in an air stream at 25 ℃; the washing and centrifuging comprises the steps of washing the retentate with deionized water, centrifuging at a speed of 5000r/min, and filtering out supernatant;
step four, placing the solid phase obtained after washing and centrifuging in the step three in a 60 ℃ oven for drying treatment for 24 hours to obtain a photocatalyst precursor;
and fifthly, in the air atmosphere, heating the photocatalyst precursor in the fourth step to 520 ℃ at a heating rate of 5 ℃/min, carrying out heat preservation and roasting for 2 hours, and grinding to obtain the graphite-phase carbon nitride photocatalyst for sewage treatment.
Comparative example 1
The comparative example provides a method for preparing a graphite-phase carbon nitride photocatalyst, which specifically comprises the following steps:
weighing 5g of powdered melamine, placing the powdered melamine in a 20mL crucible, capping the crucible filled with the melamine, placing the crucible in an air atmosphere, heating to 520 ℃ at a heating rate of 5 ℃/min, carrying out heat preservation reaction for 4 hours, and grinding to obtain a graphite-phase carbon nitride photocatalyst named as ME-0.
Evaluating performance;
fig. 2 is an XRD spectrum of the graphite-phase carbon nitride photocatalyst of examples 1 to 2 and comparative example 1. According to FIG. 2, the diffraction patterns of all three samples have a diffraction pattern corresponding to graphite-phase carbon nitride g-C 3 N 4 (100) The characteristic diffraction peaks of the crystal face and (002) crystal face, and the positions of the sample characteristic peaks corresponding to the examples are not obviously shifted, which shows that the addition of ethylenediamine tetraacetic acid in the hydrothermal process does not cause the final obtained g-C 3 N 4 A change in crystal structure.
Fig. 3 is an SEM image of the graphite-phase carbon nitride photocatalyst of examples 1 to 2 and comparative example 1, and fig. 4 is a TEM image of the graphite-phase carbon nitride photocatalyst of example 1. According to fig. 3, the sample in comparative example 1 shows a large block shape with a small specific surface area, and it can be seen in combination with fig. 3 and fig. 4 that the corresponding sample in example 1 has a hollow tubular structure with a diameter of about 1 μm and the wall of the hollow tubular structure has a loose porous structure, and the corresponding sample in example 2 has a loose porous solid rod-like structure with a diameter of about 10 μm.
FIG. 5 shows steady-state and transient PL spectra (photoluminescence spectra) of the graphite-phase carbon nitride photocatalyst of example 1 and comparative example 1, from the steady-state PL spectrum (a), it can be seen that the pure g-C of comparative example 1 3 N 4 The compound has a strong PL characteristic peak, the intensity of the characteristic peak of the embodiment 1 is obviously weakened, which indicates that the change of the morphology effectively inhibits the compound of the photogenerated carriers and the electronic structure is effectively regulated. From the transient PL spectrum (b), the service life of the carrier of the graphite-phase carbon nitride photocatalyst of example 1 is shortened, which indicates that electrons can be rapidly transferred to surface for recombination, modification promotes separation of photo-generated carriers, and also indicates that the electronic structure is effectively regulated.
Fig. 6 is a graph showing the photocurrent density curves of the graphite-phase carbon nitride photocatalysts of examples 1 to 2 and comparative example 1, and it can be seen that the photocurrent density of the graphite-phase carbon nitride photocatalysts according to examples is significantly improved.
Fig. 7 is a graph showing the comparison of the activities of the graphite-phase carbon nitride photocatalysts of examples 1 to 2 and comparative example 1 for decomposing triethanolamine under irradiation of visible light. The activity test process comprises the following steps: 20mg of catalyst is weighed and dispersed in 160mL of 10% triethanolamine solution, 3% wtPt of cocatalyst is added, argon is purged for 30min before illumination to remove oxygen, a 420nm cut-off filter is added in a xenon lamp, and the temperature of the whole reaction system is controlled by 35 ℃ circulating water. It can be seen that under the action of the graphite phase carbon nitride photocatalyst of examples 1-2, the activity of the photocatalytic decomposition of triethanolamine is significantly improved, wherein compared with the pure g-C of comparative example 1 3 N 4 (ME-0), the MEH-100 activity of example 2 was increased 11.5-fold, which may be due to: the morphology of the sample is changed by adding the ethylenediamine tetraacetic acid in the hydrothermal process, the generated loose porous structure has higher specific surface area, the recombination of photon-generated carriers is inhibited, the separation and the transmission of the photon-generated carriers are promoted, and finally the photocatalytic activity is improved.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any simple modification, variation and equivalent structural changes of the above embodiment according to the technical matter of the present invention still fall within the scope of the technical solution of the present invention.
Claims (4)
1. The method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment is characterized by comprising ethylenediamine tetraacetic acid modified graphite-phase carbon nitride, wherein the morphology of the ethylenediamine tetraacetic acid modified graphite-phase carbon nitride is hollow tubular or solid rod-shaped, the diameters of the hollow tubular and the solid rod-shaped are 1-10 mu m, the raw materials of the method comprise graphite-like carbon nitride precursors and ethylenediamine tetraacetic acid, and the mass of the ethylenediamine tetraacetic acid is 0.2-20 times that of the graphite-like carbon nitride precursors; the graphite-like carbon nitride precursor is melamine, dicyandiamide or urea;
the method specifically comprises the following steps:
adding deionized water into a hydrothermal kettle liner filled with a graphite-like carbon nitride precursor and ethylenediamine tetraacetic acid, and stirring to uniformly mix;
step two, placing the inner liner of the hydrothermal kettle provided with the mixed system in the step one into a stainless steel shell, sealing, and carrying out hydrothermal reaction for 1-20 h in a baking oven at 100-200 ℃;
step three, cooling the system after the hydrothermal reaction in the step two to the temperature of less than or equal to 25 ℃, centrifuging the cooled system, filtering, and washing and centrifuging the precipitate for 3 times;
step four, placing the solid phase subjected to washing and centrifugation in an oven at 40-100 ℃ for drying treatment for 6-24 hours to obtain a photocatalyst precursor;
and fifthly, in the air atmosphere, heating the photocatalyst precursor in the fourth step to 500-550 ℃ at a heating rate of 2-10 ℃/min, carrying out heat preservation and roasting for 2-4 hours, and grinding to obtain the graphite-phase carbon nitride photocatalyst for sewage treatment.
2. The method of claim 1, wherein the cooling in step three is cooling in a 25 ℃ air stream or cooling in a 25 ℃ water bath.
3. The method of claim 1, wherein the washing centrifugation in step three comprises washing the precipitate with deionized water, centrifuging, and filtering the supernatant.
4. A method for catalytically treating alcohol amine-containing pollutants by using the graphite-phase carbon nitride photocatalyst for sewage treatment prepared by the method for preparing the graphite-phase carbon nitride photocatalyst for sewage treatment according to claim 1.
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