CN111889123A - Carbon-doped heterojunction photocatalyst and preparation method thereof - Google Patents
Carbon-doped heterojunction photocatalyst and preparation method thereof Download PDFInfo
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- CN111889123A CN111889123A CN202010520648.7A CN202010520648A CN111889123A CN 111889123 A CN111889123 A CN 111889123A CN 202010520648 A CN202010520648 A CN 202010520648A CN 111889123 A CN111889123 A CN 111889123A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims abstract description 58
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000013081 microcrystal Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 20
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 11
- 239000004202 carbamide Substances 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 229920002678 cellulose Polymers 0.000 claims description 10
- 239000001913 cellulose Substances 0.000 claims description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 10
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- QWMFKVNJIYNWII-UHFFFAOYSA-N 5-bromo-2-(2,5-dimethylpyrrol-1-yl)pyridine Chemical compound CC1=CC=C(C)N1C1=CC=C(Br)C=N1 QWMFKVNJIYNWII-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000004310 lactic acid Substances 0.000 claims description 5
- 235000014655 lactic acid Nutrition 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002159 nanocrystal Substances 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000000707 layer-by-layer assembly Methods 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims 1
- 230000032900 absorption of visible light Effects 0.000 abstract description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 4
- 230000008859 change Effects 0.000 abstract description 3
- XMEVHPAGJVLHIG-FMZCEJRJSA-N chembl454950 Chemical compound [Cl-].C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H]([NH+](C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O XMEVHPAGJVLHIG-FMZCEJRJSA-N 0.000 abstract description 2
- 229960004989 tetracycline hydrochloride Drugs 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000000926 separation method Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 239000003403 water pollutant 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
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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
- 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
-
- 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
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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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Abstract
The invention relates to a carbon-doped heterojunction photocatalyst and a preparation method thereof. Wherein, the carbon-doped carbon nitride effectively inhibits the growth of microcrystals to block phase change and enhances the absorption of visible light; the combination of the compound with tungsten trioxide effectively improves the carrier life, excites electrons to improve the electron mobility, and compared with pure carbon nitride/tungsten trioxide, the efficiency of photocatalytic degradation of tetracycline hydrochloride is enhanced.
Description
Technical Field
The invention belongs to the field of functional polymer materials and photocatalytic pollutant degradation. In particular to a carbon-doped carbon nitride/tungsten trioxide heterojunction photocatalyst.
The invention also relates to two preparation methods of the carbon-doped heterojunction photocatalyst.
Background
The carbon nitride is used as a stable and nontoxic nonmetal semiconductor photocatalyst, has a proper forbidden band width, can absorb visible light with the wavelength of 460-698nm, and has good chemical stability and thermal stability. Carbon nitride has wide application under the irradiation of visible light, such as light-induced reduction of carbon dioxide, photocatalytic decomposition of water to generate hydrogen, photocatalytic degradation of water and air pollutants, and the like.
The pure carbon nitride photocatalyst is limited by insufficient absorption of visible light and rapid recombination of carriers, so that the photocatalytic activity is low. Element doping is used as an effective method for adjusting carbon nitride band gap and electronic structure, so that the photoresponse range is greatly widened, and the charge separation is enhanced. Compared with other metal and nonmetal dopants, the carbon doping has the advantages of rich content, no toxicity, low cost, ecological friendliness, high stability and the like. The most important of these is that the carbon element doped carbon nitride forms a carbon nitride with an atomic size comparable to that of nitrogen atoms and a small ionization energy. Thus, carbon-doped carbon nitride can enhance the absorption of visible light and improve the mobility of photo-induced charge carriers.
The oxidation and reduction reactions of the conventional heterojunction photocatalyst respectively occur in a high valence band and a low conduction band, which are beneficial to the separation of photo-generated electrons and holes, but lead to the reduction of oxidation and reduction capabilities. The Z-type heterojunction photocatalyst is prepared by combining carbon nitride with an inorganic semiconductor material, the separation efficiency of electrons and holes is improved, the high oxidation and reducibility of a photon-generated carrier is kept, light absorption is expanded, the separation of charges is promoted, and the activity and the stability of the photocatalyst are effectively improved. Thus, the activity of the carbon nitride/tungsten trioxide in photocatalytic degradation of pollutants is enhanced. The two methods are combined to simultaneously change the band gap and the electronic structure, so that the light absorption range of the photocatalyst is expanded, the carrier separation efficiency is improved, and the photocatalytic degradation efficiency of the heterojunction photocatalyst is further improved.
According to the invention, carbon-doped carbon nitride and tungsten trioxide are combined to form the heterojunction photocatalyst, the carbon-doped carbon nitride effectively inhibits the growth of microcrystals to block phase change, the band gap structure is properly improved, the absorption of visible light is enhanced, and the separation efficiency of carriers is promoted, so that the catalytic performance of the photocatalyst is improved. The electrostatic attraction is formed by utilizing the electropositivity of the surface of the carbon-doped carbon nitride and the electronegativity of the surface of the tungsten trioxide, and the carbon-doped carbon nitride tungsten trioxide heterojunction photocatalyst is prepared by utilizing the coulomb electrostatic interaction self-assembly.
Disclosure of Invention
The invention aims to provide a carbon-doped carbon nitride/tungsten trioxide heterojunction photocatalyst, which takes nano-cellulose microcrystals, urea and sodium tungstate dihydrate as raw materials of the photocatalyst, carbon nitride is subjected to carbon doping by a direct method and a hydrothermal method, and the heterojunction photocatalyst with thermal stability is prepared by an electrostatic self-assembly method.
The invention also aims to provide two preparation methods of the carbon-doped heterojunction photocatalyst. According to the method, carbon in nano-cellulose is doped in carbon nitride prepared from urea by using a hydrothermal method and a direct method, and a photocatalyst with high catalytic degradation performance is prepared by combining tungsten trioxide. Firstly, dispersing cellulose in a urea aqueous solution, and obtaining two carbon-doped carbon nitrides by a direct calcination method and a hydrothermal treatment method; then, preparing tungsten trioxide by using a sodium tungstate dihydrate hydrothermal method; and finally, mixing carbon-doped carbon nitride with a certain concentration and a tungsten trioxide aqueous solution according to a certain proportion, drying and calcining to obtain the heterojunction photocatalyst with thermal stability.
In the carbon-doped carbon nitride prepared by the two different methods, the carbon doping amount is 0.1%, the calcining temperature is 550 ℃, the heating rate is 10 ℃/min, and the heat preservation time is 2 h.
In the hydrothermal method for preparing tungsten trioxide, the reaction temperature is 180 ℃ and the reaction time is 24 hours.
In the preparation method of the heterojunction photocatalyst, the ratio of carbon-doped carbon nitride to tungsten trioxide is 5: 1; the calcination temperature of the heterojunction photocatalyst is 450 ℃, the heating rate is 5 ℃/min, and the heat preservation time is 2 h.
The invention has the advantages and characteristics that:
the invention designs and synthesizes the carbon-doped carbon nitride/tungsten trioxide photocatalyst, and utilizes the positive electricity of the surface of the carbon-doped carbon nitride and the negative electricity of the surface of the tungsten trioxide to improve the chemical stability and the thermal stability of the photocatalyst through self-assembly under the electrostatic action of coulomb.
According to the invention, as the carbon atoms come from the cellulose nanocrystals and replace sp2 hybridized nitrogen atoms in the carbon nitride, the band gap and the electronic structure are properly changed, and the absorption of visible light is enhanced.
The carbon-doped carbon nitride is combined with tungsten trioxide to form a heterojunction photocatalyst, so that the efficiency of degrading tetracycline hydrochloride by photocatalysis is effectively improved.
Detailed Description
Through intensive research, the inventor of the invention prepares carbon-doped carbon nitride by combining cellulose nanocrystals with urea and prepares a heterojunction photocatalyst by combining tungsten trioxide.
In order to clearly understand the technical contents of the present invention, the following examples are specifically used for the purpose of better understanding the contents of the present invention and are not intended to limit the scope of the present invention.
Example (b): preparation of carbon-doped carbon nitride/tungsten trioxide heterojunction photocatalyst
Direct method of carbon doping with carbon nitride: diluting 1mL of Cellulose Nanocrystalline (CNC) solution with 20mL of water, adding 20g of urea, stirring and ultrasonically dissolving completely, preparing a CNC/urea aqueous solution with the concentration of 0.1%, drying, and calcining by using a muffle furnace, wherein the heat preservation temperature is 550 ℃, the temperature rise rate is 10 ℃/min, and the heat preservation time is 2 h.
Hydrothermal method of carbon-doped carbon nitride: the CNC/urea aqueous solution with the concentration of 0.1% is firstly transferred into a polytetrafluoroethylene high-pressure reaction kettle, the reaction temperature is 150 ℃, the reaction time is 2 hours, and then the preparation is carried out by calcination.
Dispersing 1g of sodium tungstate dihydrate in 50mL of water, adding 1mL of lactic acid, stirring, changing the solution from colorless transparency to light yellow, adding 3M hydrochloric acid to adjust the pH value to 1, transferring the solution into a polytetrafluoroethylene high-pressure reaction kettle, reacting at the temperature of 180 ℃ for 24 hours to obtain blue precipitate, washing with ethanol and water for multiple times, and drying.
100mg of two nitrogen-doped carbon nitrides are respectively dispersed in 80mL of 20% lactic acid solution, 40mL0.5mg/mL of tungsten trioxide solution is dropwise added, and the mixture is washed by water, dried and then transferred to a muffle furnace to be calcined at 450 ℃.
Claims (6)
1. The carbon-doped heterojunction photocatalyst is characterized in that cellulose nanocrystals, urea and sodium tungstate dihydrate are used as main photocatalyst raw materials of the photocatalyst, carbon nitride is subjected to carbon doping by a direct method and a hydrothermal method, and an electrostatic self-assembly method is utilized to prepare the heterojunction photocatalyst with thermal stability.
2. The preparation method of the carbon-doped heterojunction photocatalyst comprises the following steps:
step 1: dispersing nano-cellulose microcrystals in a urea aqueous solution, and preparing carbon-doped carbon nitride by a direct method and a hydrothermal method, wherein the direct method comprises the steps of dispersing the nano-cellulose microcrystals in the urea aqueous solution, mixing the solution, drying and calcining to obtain the carbon-doped carbon nitride; the hydrothermal method is to disperse the nano-cellulose microcrystals in an aqueous solution of urea, firstly transfer the solution into a high-pressure reaction kettle of polytetrafluoroethylene for reaction, and then take out the solution, dry and calcine the solution to obtain another carbon-doped carbon nitride;
step 2: dispersing sodium tungstate dihydrate in water, adding a certain amount of lactic acid, adding hydrochloric acid to adjust the pH value, generating blue precipitate by using a hydrothermal method, and washing with ethanol and water for multiple times to obtain nano tungsten trioxide square crystals;
and step 3: respectively dispersing the carbon-doped carbon nitride prepared by the two methods in a lactic acid aqueous solution, mixing the lactic acid aqueous solution with the prepared tungsten trioxide aqueous solution according to a certain proportion and a certain concentration, and drying and calcining to obtain the carbon-doped carbon nitride/tungsten trioxide heterojunction photocatalyst prepared by the two different methods.
3. The carbon-doped carbon nitride/tungsten trioxide heterojunction photocatalyst prepared by two different methods as claimed in claims 1 and 2, wherein the carbon doping amount of the carbon nitride is 0.1%, the calcining temperature is 550 ℃, the temperature rise rate is 10 ℃/min, and the holding time is 2 h.
4. The carbon-doped carbon nitride/tungsten trioxide heterojunction photocatalyst prepared by two different methods as claimed in claims 1 and 2, wherein the hydrothermal reaction temperature of the sodium tungstate dihydrate for preparing tungsten trioxide is 180 ℃ and the reaction time is 24 h.
5. Carbon-doped carbon nitride/tungsten trioxide heterojunction photocatalyst prepared according to two different methods as described in claims 1 and 2, characterized in that the ratio of carbon nitride and tungsten trioxide is 5: 1.
6. The carbon-doped carbon nitride/tungsten trioxide heterojunction photocatalyst prepared by two different methods as claimed in claims 1 and 2, wherein the calcination temperature of the carbon-doped carbon nitride/tungsten trioxide heterojunction is 450 ℃, the temperature rise rate is 5 ℃/min, and the holding time is 2 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113926481A (en) * | 2021-09-29 | 2022-01-14 | 东华大学 | CNC/g-C3N4Nanocomposite material, preparation and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113926481A (en) * | 2021-09-29 | 2022-01-14 | 东华大学 | CNC/g-C3N4Nanocomposite material, preparation and application thereof |
| CN113926481B (en) * | 2021-09-29 | 2024-06-21 | 东华大学 | CNC/g-C3N4Nanocomposite, preparation and use thereof |
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Application publication date: 20201106 |