CN110694664A - Preparation method and application of graphite-phase carbon nitride/graphene composite photocatalyst - Google Patents
Preparation method and application of graphite-phase carbon nitride/graphene composite photocatalyst Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 35
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 31
- 239000010439 graphite Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000002244 precipitate Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 5
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 11
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000013032 photocatalytic reaction Methods 0.000 claims description 7
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 4
- 229910052724 xenon Inorganic materials 0.000 claims description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 238000007605 air drying Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000002329 infrared spectrum Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 6
- 238000000862 absorption spectrum Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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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
-
- B01J35/39—
-
- 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
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- 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
Abstract
The invention discloses a preparation method and application of a graphite-phase carbon nitride/graphene composite photocatalyst, wherein the preparation method comprises the following steps: mixing graphite phase carbon nitride g-C3N4The graphene-phase carbon nitride/graphene composite photocatalyst is prepared by mixing graphite oxide GO, adding water for ultrasonic dispersion, then adding hydrazine hydrate, stirring in a water bath, cooling to room temperature, centrifuging to obtain a precipitate, drying and heating the precipitate to obtain the graphite-phase carbon nitride/graphene composite photocatalyst.
Description
Technical Field
The invention relates to the technical field of powder material preparation, and particularly relates to a preparation method and application of a graphite phase carbon nitride/graphene composite photocatalyst.
Background
Along with the development of economy, the pollution is increasingly serious, so that the life of human beings is influenced, and great burden is brought to the environment. Environmental problems become a key factor of economic development, people gradually discover that photocatalytic pollution treatment is an energy-saving, efficient and environment-friendly treatment mode in the treatment process, and treatment is remarkably advanced in recent years. Among the numerous photocatalysts, the graphite phase carbon nitride (g-C)3N4) The photocatalyst belongs to a semiconductor, has good performance, can absorb partial visible light, has strong stability and better photocatalytic performance. However, g-C3N4The distance from the top of the valence band to the bottom of the conduction band is 2.7eV, the conduction band is narrow, the conduction band is suitable for utilizing visible light, photogenerated electrons are excited by the visible light to generate transition, and the recombination of the electrons and holes is fast, so the improvement is needed.
The electrons take graphene (RGO) as a carrier and migrate from the interior of the RGO to the surface, and the RGO blocks the recombination of photogenerated electrons and holes, although the current research has made good progress, the g-C can be prepared by a plurality of different methods3N4RGO, the properties of which with respect to photocatalytic degradation are to be verified and improved, still needs further investigation. Meanwhile, related reports also have researches on different mass ratios, including g-C3N4The mass ratio of the RGO to the RGO is 200:1, 600:1, 800:1 and 5000:1, the ratio is greatly different, the two can not be ensured to be fully and uniformly compounded during preparation, and other ratios are not reported.
Disclosure of Invention
The inventor prepares g-C by taking urea as a raw material3N4Preparing graphite oxide GO by a graphite oxide method, and then adding g-C3N4Mixing with GO, and reducing with hydrazine hydrate to obtain graphite phase carbon nitride/graphene composite photocatalyst g-C3N4/RGO and its application to light of methylene blueAnd (4) catalyzing and degrading.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a graphite phase carbon nitride/graphene composite photocatalyst comprises the following steps:
s1: preparation of graphite phase carbon nitride g-C3N4And is ready for use;
s2: preparing graphite oxide GO by an oxidation method for later use;
s3: mixing graphite phase carbon nitride g-C3N4And mixing with graphite oxide GO, adding water for ultrasonic dispersion, then adding hydrazine hydrate, stirring in a water bath, cooling to room temperature, centrifuging to obtain a precipitate, drying and heating the precipitate to obtain the graphite-phase carbon nitride/graphene composite photocatalyst.
Further, in the step S1, the graphite phase carbon nitride g-C3N4The preparation method comprises the following steps:
and (3) putting the urea into a crucible, keeping the temperature of an electric furnace of the crucible at 530-560 ℃, keeping the temperature for 2-3h, and naturally cooling to room temperature.
Further, in the step S3, water is added for ultrasonic dispersion for 0.5-1.5h, 1.5-2.5mL of hydrazine hydrate is added, water bath stirring is carried out for 0.5-1.5h at the temperature of 75-85 ℃, the temperature is reduced to room temperature, centrifugation is carried out to obtain a precipitate, air blowing drying is carried out for 23-25h at the temperature of 75-85 ℃, and heating is carried out for 1-1.5h at the temperature of 540-.
Further, the graphite phase carbon nitride g-C3N4And graphite oxide GO in a mass ratio of 6.7: 1. 8: 1. 9: 1. 9.3: 1 or 9.7: 1.
further, the graphite phase carbon nitride g-C3N4And graphite oxide GO in a mass ratio of 9.7: 1.
in addition, the invention also provides application of the graphite-phase carbon nitride/graphene composite photocatalyst prepared by the preparation method in photocatalytic degradation of methylene blue.
Further, mixing the graphite-phase carbon nitride/graphene composite photocatalyst with a methylene blue solution for photocatalytic reaction to complete the treatment of antibiotics in the wastewater.
Further, 50mg of graphite-phase carbon nitride/graphene composite photocatalyst is added into 100mL of 50mg/L methylene blue solution, the light source of the photocatalytic reaction is a long-arc xenon lamp light source, and the time of the photocatalytic reaction is 4-4.5 h.
The invention has the beneficial effects that:
the prepared graphite-phase carbon nitride/graphene composite photocatalyst has excellent photocatalytic degradation performance on methylene blue, and has considerable application prospect in the field of photocatalytic degradation.
Drawings
Fig. 1 is an X-ray diffraction pattern of the photocatalysts prepared in examples one to five and comparative examples, wherein the abscissa indicates that the X-ray diffractometer scans the entire diffraction region at an angle of 2 θ.
FIG. 2 is an infrared spectrum of the photocatalyst prepared in the first to fifth examples and the comparative example and the graphene RGO, wherein the curves sequentially show the photocatalyst prepared in the comparative example, the RGO, the first example, the second example, the third example, the fourth example and the fifth example from top to bottom, the abscissa thereof represents the wave number, and the unit is cm-1。
Fig. 3 is a graph showing the photocatalytic degradation rate of the photocatalysts prepared in the first to fifth examples and the comparative example to methylene blue under the irradiation of visible light, wherein curves in the graph sequentially show the photocatalysts prepared in the first to fifth examples, the second example, the comparative example, the third example, the fourth example and the fifth example from top to bottom, the abscissa of the graph shows irradiation time in min, and the ordinate of the graph shows the degradation rate in%.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a preparation method of a graphite phase carbon nitride/graphene composite photocatalyst comprises the following steps:
s1: weighing 8g of urea, putting the urea into a crucible, keeping the temperature of the crucible at 550 ℃ for 2.5h in an electric furnace, and naturally cooling the urea to room temperature to obtain graphite-phase carbon nitride g-C3N4A pale yellow powder.
S2: preparing graphite oxide GO by an oxidation method, specifically, placing graphite powder in a three-neck flask, carrying out ice bath to 0 ℃, adding sulfuric acid and sodium nitrate, uniformly stirring, keeping the temperature at 0-12 ℃, adding potassium permanganate, heating to 30-40 ℃, stirring to form brown paste, adding water for diluting, stirring for 0.5-1H, adding 10-20mL of H2O2Reacting, filtering, washing a product with 20-50mL hydrochloric acid to remove chloride ions, centrifuging, and drying at 60-70 ℃ for 23-25h to obtain the graphite oxide GO.
S3: g to C3N4And GO according to a mass ratio of 9.7: 1, placing the mixture in a beaker, adding water, ultrasonically dispersing for 1h, then adding 2mL of hydrazine hydrate, stirring in a water bath at 80 ℃ for 1h, cooling to room temperature, centrifuging to obtain a precipitate, drying by air blowing at 80 ℃ for 24h, and heating at 550 ℃ for 1h to obtain the graphite-phase carbon nitride/graphene composite photocatalyst g-C3N4/RGO。
Graphite-phase carbon nitride/graphene composite photocatalyst g-C prepared in this example3N4The X-ray diffraction spectrum of/RGO is shown as curve f in FIG. 1, and the infrared spectrum is shown in FIG. 2.
Example two:
parts of this embodiment that are the same as those of the first embodiment are not described again, except that:
g-C3N4and GO according to a mass ratio of 9.3: 1.
graphite-phase carbon nitride/graphene composite photocatalyst g-C prepared in this example3N4The X-ray diffraction spectrum of/RGO is shown as curve e in FIG. 1, and the infrared spectrum is shown in FIG. 2.
Example three:
parts of this embodiment that are the same as those of the first embodiment are not described again, except that:
g-C3N4and GO according to the mass ratio of 9: 1.
graphite-phase carbon nitride/graphene composite photocatalyst g-C prepared in this example3N4The X-ray diffraction spectrum of/RGO is shown as curve d in FIG. 1, and the infrared spectrum is shown in FIG. 2.
Example four:
parts of this embodiment that are the same as those of the first embodiment are not described again, except that:
g-C3N4and GO is mixed according to the mass ratio of 8: 1.
graphite-phase carbon nitride/graphene composite photocatalyst g-C prepared in this example3N4The X-ray diffraction spectrum of/RGO is shown as curve c in FIG. 1, and the infrared spectrum is shown as FIG. 2.
Example five:
parts of this embodiment that are the same as those of the first embodiment are not described again, except that:
g-C3N4and GO is mixed according to the mass ratio of 6.7: 1.
graphite-phase carbon nitride/graphene composite photocatalyst g-C prepared in this example3N4The X-ray diffraction spectrum of/RGO is shown as curve b in FIG. 1, and the infrared spectrum is shown as FIG. 2.
Comparative example:
weighing 8g of urea, placing the urea in a crucible, covering the crucible with a cover, placing the urea in an electric furnace of the crucible, setting the temperature at 550 ℃, keeping the temperature for 2.5 hours, naturally cooling to room temperature to obtain light yellow powder, and obtaining the graphite-phase carbon nitride g-C3N4。
Graphite phase carbon nitride g-C prepared in this example3N4The X-ray diffraction spectrum of (1) is shown as curve a in FIG. 1, and the infrared spectrum thereof is shown as FIG. 2.
And (3) comparison test:
50mg of photocatalyst is added into 100mL of 50mg/L methylene blue solution, dark treatment is carried out for 0.5h, 5mL of liquid is taken for centrifugation, the supernatant is taken for measuring a visible absorption spectrum, and the spectral data at 0h are recorded. And after the rest solution is illuminated under visible light for 1h, taking out 5mL of liquid for centrifugation, taking supernatant, measuring a visible absorption spectrum, and recording spectral data at 1 h. Then, the visible absorption spectrum of the residual liquid is measured every 1h of multiple illumination, and the data is recorded. Wherein, the light source of the photocatalytic reaction is a long-arc xenon lamp light source.
Respectively taking the graphite-phase carbon nitride/graphene composite photocatalyst g-C prepared in the first to fifth embodiments3N4RGO, graphite phase carbon nitride g-C prepared in comparative example3N4And graphene RGO, the test results obtained by performing the above comparative test are shown in fig. 3. As can be seen from fig. 3: example one prepared graphite phase carbon nitride/graphene composite photocatalyst g-C3N4The irradiation of the long-arc xenon lamp light source for 4h by the/RGO can degrade 88% of 100mL of 50mg/L methylene blue.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A preparation method of a graphite phase carbon nitride/graphene composite photocatalyst is characterized by comprising the following steps:
s1: preparation of graphite phase carbon nitride g-C3N4And is ready for use;
s2: preparing graphite oxide GO by an oxidation method for later use;
s3: mixing graphite phase carbon nitride g-C3N4And mixing with graphite oxide GO, adding water for ultrasonic dispersion, then adding hydrazine hydrate, stirring in a water bath, cooling to room temperature, centrifuging to obtain a precipitate, drying and heating the precipitate to obtain the graphite-phase carbon nitride/graphene composite photocatalyst.
2. The method according to claim 1, wherein in step S1, the graphite-phase carbon nitride is G-C3N4The preparation method comprises the following steps:
and (3) putting the urea into a crucible, keeping the temperature of an electric furnace of the crucible at 530-560 ℃, keeping the temperature for 2-3h, and naturally cooling to room temperature.
3. The method as claimed in claim 1, wherein in step S3, water is added for ultrasonic dispersion for 0.5-1.5h, 1.5-2.5mL hydrazine hydrate is added, water bath stirring at 75-85 ℃ is carried out for 0.5-1.5h, the temperature is reduced to room temperature, centrifugation is carried out to obtain precipitate, air drying at 75-85 ℃ is carried out for 23-25h, and heating at 540 ℃ and 560 ℃ is carried out for 1-1.5 h.
4. The production method according to claim 3, wherein the graphite-phase carbon nitride g-C3N4And graphite oxide GO in a mass ratio of 6.7: 1. 8: 1. 9: 1. 9.3: 1 or 9.7: 1.
5. the method of claim 4, wherein the graphite phase carbon nitride g-C3N4And graphite oxide GO in a mass ratio of 9.7: 1.
6. the application of the graphite-phase carbon nitride/graphene composite photocatalyst prepared by the preparation method of any one of claims 1 to 5 in photocatalytic degradation of methylene blue.
7. Use according to claim 6, characterized in that it comprises the following steps: and mixing the graphite-phase carbon nitride/graphene composite photocatalyst with a methylene blue solution for photocatalytic reaction to complete the treatment of the methylene blue.
8. The use of claim 7, wherein 50mg of the graphite-phase carbon nitride/graphene composite photocatalyst is added to 100mL of 50mg/L methylene blue solution, the light source of the photocatalytic reaction is a long-arc xenon lamp light source, and the time of the photocatalytic reaction is 4-4.5 h.
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CN113731458A (en) * | 2020-05-29 | 2021-12-03 | 山东海科创新研究院有限公司 | Graphene/carbon nitride composite material and preparation method and application thereof |
CN113617351A (en) * | 2021-08-27 | 2021-11-09 | 西安理工大学 | Graphite-like phase carbon nitride/graphene oxide composite aerogel and method |
CN114988515A (en) * | 2022-04-21 | 2022-09-02 | 南京林业大学 | Method for removing Cr (VI) and g-C adopted by same 3 N 4 Composite foam/cellulose/GO |
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