CN110252367B - Solvothermal method for preparing few-layer carbon nitride supported vanadium dioxide catalyst and desulfurization application thereof - Google Patents
Solvothermal method for preparing few-layer carbon nitride supported vanadium dioxide catalyst and desulfurization application thereof Download PDFInfo
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- 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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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G27/00—Refining of hydrocarbon oils in the absence of hydrogen, by oxidation
- C10G27/04—Refining of hydrocarbon oils in the absence of hydrogen, by oxidation with oxygen or compounds generating oxygen
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
Abstract
The invention belongs to the technical field of material preparation and catalytic reaction, relates to catalyst desulfurization, and particularly relates to a method for preparing a few-layer carbon nitride supported vanadium dioxide catalyst by a solvothermal method, which comprises the following steps: mixing and stirring vanadium dioxide and few-layer carbon nitride in dichloromethane, transferring the mixture to a reaction kettle with a polytetrafluoroethylene lining for solvothermal reaction after uniform stirring, and drying the product to obtain the few-layer carbon nitride loaded vanadium dioxide supported catalyst X-VO2/g‑C3N4(X represents the amount of vanadium dioxide supported). The supported catalyst prepared by the invention is applied to the field of catalytic oxidation desulfurization, and particularly, the dibenzothiophene sulfides in diesel oil are efficiently removed by oxidation by using oxygen in air as an oxidant. The synthesis process is simple to operate, the carbon nitride with the few-layer structure can realize effective dispersed loading of the vanadium dioxide as the active center, the conditions required by the catalytic oxidation desulfurization reaction are mild, oxygen in the air is used as an oxidant, and the catalyst has high desulfurization efficiency and excellent stability.
Description
Technical Field
The invention belongs to the technical field of material preparation and catalytic reaction, relates to catalyst desulfurization, and particularly relates to a few-layer carbon nitride supported vanadium dioxide catalyst prepared by a solvothermal method and desulfurization application thereof.
Background
SO is generated by combustion of sulfur-containing compounds in automobile fuel x This is one of the main pollutants in the atmosphere, reducing sulfur contentThe amount is helpful for the normal operation of the automobile exhaust device, and is beneficial to controlling the emission of the automobile exhaust. Therefore, the sulfur content in the vehicle fuel is an important index to be strictly controlled. Since 2017, China has supplied all-round motor gasoline and diesel oil meeting the national standard (national standard V) of the fifth stage, the standard reduces the sulfur content index limit value from 50 ppm of the fourth stage to 10 ppm, and deep desulfurization becomes an important task of the oil refining industry. At present, the oxidative desulfurization technology attracts extensive attention of researchers due to mild reaction conditions, simple operation and good removal performance of aromatic sulfides which are difficult to remove by the conventional desulfurization technology, and people are dedicated to developing a catalytic system with high activity and low cost to realize deep desulfurization of fuel oil.
Research shows that vanadium oxide is used as an active center, and Dibenzothiophene (DBT) sulfur-containing compounds and derivatives thereof can be effectively activated and oxidized under the action of an oxidant to generate sulfone substances with strong polarity, so that the aim of ultra-deep desulfurization under mild conditions is fulfilled. However, the metal oxide is easy to agglomerate in the reaction process, which leads to the problems of poor catalytic activity and difficult recovery and reutilization of the catalyst. Research reports that the proper carrier is used for loading the metal oxide, which is beneficial to the high dispersion of the active center, promotes the generation of a heterojunction structure between the metal oxide and the carrier, improves the catalytic performance, and can realize the separation and recovery of the catalyst and the repeated recycling. At the same time, a few layers of carbon nitride (g-C)3N4) As a green material, the material has the advantages of easy realization of the preparation method, stable physical and chemical properties, adjustable structure and the like, and is widely applied to the preparation research of carrier materials.
By selecting a proper loading means, the method can be designed and developed to use carbon nitride as a carrier and vanadium dioxide (VO) which is cheap, simple, green, efficient, high in desulfurization efficiency2) The supported catalyst is an active center supported catalyst, has stable structural property, mild reaction operation conditions and high desulfurization efficiency, and has excellent industrial application prospect.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing a few-layer carbon nitride supported vanadium dioxide supported catalyst by a solvothermal method.
The technical scheme is as follows:
a method for preparing a few-layer carbon nitride supported vanadium dioxide catalyst by a solvothermal method comprises the following steps: vanadium dioxide and a few layers of carbon nitride in methylene Chloride (CH)2Cl2) Mixing and stirring, transferring the mixture to a reaction kettle with a polytetrafluoroethylene lining for solvothermal reaction after uniform stirring, and drying the product to obtain the few-layer carbon nitride loaded vanadium dioxide supported catalyst X-VO2/g-C3N4(X represents the amount of vanadium dioxide supported).
In the preferred embodiment of the invention, the solid-to-liquid ratio of the vanadium dioxide, the carbon nitride with less layers and the solvent dichloromethane is 0.016-0.064 g/0.16-0.19 g/25-50 mL, preferably 0.032 g/0.18 g/30 mL.
In the preferred embodiment of the invention, the crystal form of the vanadium dioxide is a monoclinic phase, and can be sold in the market or made by self.
In the preferred embodiment of the invention, the stirring time of the mixture is 0.5-3.5 h, preferably 1 h.
In the preferred embodiment of the invention, the solvothermal reaction temperature is 80-120 ℃, the time is 12-36 h, and the heating at 100 ℃ is preferably 12 h.
In the preferred embodiment of the invention, the drying temperature of the product is 50-80 ℃, the drying time is 1-3 h, and the drying time at 50 ℃ is preferably 1 h.
The vanadium dioxide can be sold in the market or made by self, and the preparation method comprises the following steps: adding ammonium metavanadate and oxalic acid dihydrate into 30mL of deionized water, mixing, fully and uniformly stirring, and transferring the mixture into a reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction; carrying out suction filtration on the obtained product, washing the product with deionized water and absolute ethyl alcohol, and then drying the product in a vacuum drying oven to obtain blue-black powder; and calcining the bluish black powder in a programmed heating tubular furnace under the argon atmosphere, and cooling to room temperature to obtain the monoclinic-phase vanadium dioxide.
In the preferred embodiment of the invention, the solid-to-liquid ratio of the ammonium metavanadate, the oxalic acid dihydrate and the deionized water is 2 mmol: 3 mmol: 1.67 mol.
In the preferred embodiment of the invention, the stirring time of the mixture is 0.5-3.5 h.
In the preferred embodiment of the invention, the temperature of the hydrothermal reaction is 100-160 ℃ and the time is 48-72 hours.
In the preferred embodiment of the invention, the washing times of the deionized water and the absolute ethyl alcohol are 2-5 times.
In the preferred embodiment of the invention, the drying temperature of the product is 75-100 ℃ and the time is 1-3 h.
In the preferred embodiment of the invention, the calcination under the argon atmosphere refers to calcination in a temperature programmed tube furnace, wherein the calcination temperature is 500-800 ℃, the temperature rise rate is 5-10 ℃/min, and the calcination time is 1-3 h.
The few-layer carbon nitride (g-C) of the present invention3N4) The preparation method comprises the following steps: and (2) putting the urea into a crucible with a cover, calcining the urea in an air atmosphere by using a temperature-programmed muffle furnace, taking out the urea after cooling to room temperature to obtain a faint yellow blocky solid, putting the faint yellow blocky solid into a ceramic ark, calcining the faint yellow blocky solid again by using the temperature-programmed muffle furnace, and taking out the faint yellow blocky solid after cooling to room temperature to obtain white powder, namely the few-layer carbon nitride.
In the preferred embodiment of the invention, the mass of the urea is 20-30 g.
In the preferred embodiment of the invention, the calcination in the air atmosphere refers to calcination in a temperature-programmed muffle furnace, wherein the calcination temperature is 530-550 ℃, the temperature-rise rate is 2-5 ℃/min, and the calcination time is 3-5 h.
In the preferred embodiment of the invention, the step of calcining again in the air atmosphere refers to calcining in a temperature-programmed muffle furnace, wherein the calcining temperature is 500-530 ℃, the temperature-rising rate is 5-8 ℃/min, and the calcining time is 2-5 h.
The invention also aims to provide the application of the supported catalyst prepared by the method in the field of catalytic oxidative desulfurization, in particular to the efficient oxidative removal of dibenzothiophene sulfides in diesel oil by using oxygen in air as an oxidant.
The reported metal oxide catalysts generally have the problems of easy agglomeration, poor dispersibility and the like, so that a template agent is usually required to be added or a proper carrier is selected to regulate the morphological structure of the metal oxide, so that more active sites are exposed to improve the catalytic oxidation activity. Compared with the conventional method, the method prepares and synthesizes the vanadium dioxide supported catalyst supported by the carbon nitride with few layers by using the solvothermal method which is simple to operate, firstly prepares the carbon nitride with few layers by using a secondary calcination method, and the carbon nitride with the structure is beneficial to realizing high dispersion loading of an active center. The solvent heat treatment process is favorable for inducing the crystallization growth of vanadium dioxide on the carrier carbon nitride to form a vanadium dioxide-few-layer carbon nitride heterojunction structure, the loading capacity of the catalyst is controlled by adjusting the using amount of the vanadium dioxide, and the structure-activity relationship between the loading capacity and the catalytic activity of the catalyst is explored.
Performing morphology and structure analysis on the product by utilizing wide-angle X-ray powder diffraction (XRD), infrared spectrum analysis (FT-IR) and the like, configuring model oil by taking DBT as a typical sulfur-containing compound, and applying the synthesized supported vanadium dioxide material as a catalyst to the oxidation desulfurization reaction by taking oxygen in the air as an oxidant. The catalytic performance of the catalyst was evaluated by measuring the amount of DBT remaining after the reaction by Gas Chromatography (GC).
The method takes ammonium metavanadate as a raw material, and prepares monoclinic phase vanadium dioxide by combining hydrothermal treatment with hot calcination in an argon atmosphere and using the monoclinic phase vanadium dioxide as an active center. The method is characterized in that urea is used as a raw material, carbon nitride with a few-layer structure is prepared through twice thermal polycondensation in a temperature programming muffle furnace, high-dispersity loading of active center metal oxide can be achieved by combining a solvothermal method, a supported vanadium dioxide catalyst with a heterojunction structure is formed, and the electron cloud density of an active center is enhanced to improve the catalytic performance. The loading capacity of the catalyst is adjusted by adjusting the using amount of vanadium dioxide, and the optimal loading capacity is explored by combining a desulfurization activity experiment, so that the aim of deep desulfurization under a mild condition is fulfilled.
Advantageous effects
The synthesis process is simple to operate, the carbon nitride with the few-layer structure can realize effective dispersed loading of the vanadium dioxide as the active center, the conditions required by the catalytic oxidation desulfurization reaction are mild, oxygen in the air is used as an oxidant, the desulfurization efficiency of the catalyst is high, and the catalyst shows excellent stability.
Drawings
FIG. 1 Wide-angle XRD of catalyst;
FIG. 2 FT-IR of catalyst;
FIG. 3 FT-IR before and after catalyst reaction;
FIG. 4 shows the performance of different loaded catalysts in the catalytic oxidation removal of DBT.
Detailed Description
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
Example 1
The preparation method of the few-layer carbon nitride supported vanadium dioxide supported catalyst comprises the following steps:
0.016 g of monoclinic-phase vanadium dioxide and 0.19 g of a few-layer carbon nitride are added into 30mL of dichloromethane solution, the mixture is fully mixed and stirred for 2h, then the mixed solution is transferred into a reaction kettle with a polytetrafluoroethylene lining, and the reaction kettle is placed into an air-blowing drying oven for solvent heat treatment at 120 ℃ for 24 h. After the temperature is reduced to room temperature, the obtained product is placed in a drying oven at 70 ℃ for drying for 3 hours, and the few-layer carbon nitride supported vanadium dioxide supported catalyst (5% -VO) can be obtained2/g-C3N4）。
Example 2
The preparation method of the few-layer carbon nitride supported vanadium dioxide supported catalyst comprises the following steps:
0.032g of monoclinic-phase vanadium dioxide and 0.18g of few-layer carbon nitride are added into 30mL of dichloromethane solution, the mixture is fully mixed and stirred for 1h, then the mixed solution is transferred into a reaction kettle with a polytetrafluoroethylene lining, and the reaction kettle is placed into an air-blast drying oven for solvent heat treatment at 100 ℃ for 12 h. After the temperature is reduced to room temperature, the obtained product is placed in a drying oven at 50 ℃ for drying for 1h, and the few-layer carbon nitride supported vanadium dioxide supported catalyst (10% -VO) can be obtained2/g-C3N4）。
Example 3
The preparation method of the few-layer carbon nitride supported vanadium dioxide supported catalyst comprises the following steps:
0.064g of monoclinic-phase vanadium dioxide and 0.16 g of few-layer carbon nitride are added into 30mL of dichloromethane solution, the mixture is fully mixed and stirred for 3h, then the mixed solution is transferred into a reaction kettle with a polytetrafluoroethylene lining, and the reaction kettle is placed into a forced air drying oven for solvent heat treatment at the temperature of 80 ℃ for 36 h. After the temperature is reduced to room temperature, the obtained product is placed in a drying oven at 80 ℃ for drying for 2 hours, and the few-layer carbon nitride supported vanadium dioxide supported catalyst (20% -VO) can be obtained2/g-C3N4）。
From fig. 1, it can be seen that the few-layer carbon nitride supported vanadium dioxide supported catalyst is successfully prepared by the solvothermal method, and after the catalyst is supported, the characteristic peak of vanadium dioxide can be detected.
The characteristic peaks of carbon nitride can be seen in fig. 2, indicating that the structure of the carbon nitride is not destroyed after loading by solvothermal treatment.
Example 4
Oxidation desulfurization performance investigation of few-layer carbon nitride supported vanadium dioxide supported catalyst
The supported catalyst obtained in the examples 1 to 3 is applied to catalytic oxidation removal of sulfur-containing compounds in model oil, and the specific dosage is as follows: 0.01 g of supported catalyst and 100 mL/min of air flow are added into 20 mL of self-made model oil containing 200 ppm of DBT, the mixture is stirred and reacted under the condition of a constant-temperature oil bath at 120 ℃, timing is started after air is introduced, the reaction is stopped after 6h, and samples are taken at intervals of 1h and are detected by GC-MS (gas chromatography-Mass spectrometer), so that the DBT removal effect of different catalysts is obtained, and the result is shown in figure 4.
The desulfurization rate is calculated by the formula: s% = (C)0-Ct)/C0X 100. Wherein C is0(ppm) represents the initial sulphur content of the model oil, Ct(ppm) represents the sulfur content of the model oil at reaction t (min).
It can be seen from fig. 3 that the structure of the supported catalyst is maintained before and after the reaction, and a new characteristic peak is observed in the sample after the reaction, which is attributed to the S = O characteristic peak, indicating that the oxidation product of the DBT sulfone is obtained.
It can be seen from fig. 4 that under the reaction conditions, different catalysts have certain oxidation removal effects on DBT, and the supported catalyst with 10% of loading has the best catalytic performance.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (9)
1. A preparation method of a few-layer carbon nitride supported vanadium dioxide catalyst for catalytic oxidation desulfurization is characterized by comprising the following steps: mixing and stirring vanadium dioxide and a small amount of carbon nitride in dichloromethane, transferring the mixture to a reaction kettle with a polytetrafluoroethylene lining for solvothermal reaction after uniform stirring, and drying a product to obtain a small amount of carbon nitride loaded vanadium dioxide supported catalyst, wherein the crystal form of the vanadium dioxide is a monoclinic phase, and the solid-to-liquid ratio of the vanadium dioxide, the small amount of carbon nitride and the solvent dichloromethane is 0.016-0.064 g: 0.16-0.19 g: 25-50 mL; the solvothermal reaction temperature is 80-120 ℃, and the time is 12-36 h; the drying temperature of the product is 50-80 ℃, and the drying time is 1-3 h.
2. The method for preparing the few-layer carbon nitride supported vanadium dioxide catalyst for catalytic oxidative desulfurization according to claim 1, wherein: the solid-to-liquid ratio of the vanadium dioxide, the carbon nitride with less layers and the solvent dichloromethane is 0.032g to 0.18g to 30 mL.
3. The method for preparing the few-layer carbon nitride supported vanadium dioxide catalyst for catalytic oxidative desulfurization according to claim 1, wherein: the mixing and stirring time is 0.5-3.5 h.
4. The method for preparing the few-layer carbon nitride supported vanadium dioxide catalyst for catalytic oxidative desulfurization according to claim 1, wherein: the mixing and stirring time is 1 h.
5. The method for preparing the few-layer carbon nitride supported vanadium dioxide catalyst for catalytic oxidative desulfurization according to claim 1, wherein: the solvent thermal reaction is heated for 12 hours at 100 ℃.
6. The method for preparing the few-layer carbon nitride supported vanadium dioxide catalyst for catalytic oxidative desulfurization according to claim 1, wherein: the product was dried at 50 ℃ for 1 h.
7. The few-layer carbon nitride supported vanadium dioxide catalyst prepared by the method according to any one of claims 1 to 6.
8. The use of the few-layer carbon nitride supported vanadium dioxide catalyst of claim 7, wherein: it is applied to catalytic oxidation desulfurization.
9. Use according to claim 8, characterized in that: the method is applied to the efficient oxidation and removal of dibenzothiophene sulfides in diesel oil by using oxygen in the air as an oxidant.
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| CN110833867B (en) * | 2019-10-25 | 2022-03-22 | 江苏大学 | Preparation method and desulfurization application of three-dimensional porous carbon nitride supported vanadium-based ionic liquid catalyst |
| CN111151282B (en) * | 2020-01-15 | 2021-12-21 | 华南理工大学 | Nitrogen-doped graphite-like phase carbon nitride visible-light-induced photocatalyst and preparation method and application thereof |
| CN113797952B (en) * | 2020-06-17 | 2023-02-17 | 中国科学院过程工程研究所 | Catalyst for synthesizing alicyclic amine through selective hydrogenation saturation of benzene ring containing benzene ring amine compounds and preparation method thereof |
| CN112018348A (en) * | 2020-08-10 | 2020-12-01 | 五邑大学 | VO (volatile organic compound)2/MXene composite material and preparation method and application thereof |
| CN112657532B (en) * | 2021-01-06 | 2022-09-23 | 山东科技大学 | VO (volatile organic compound) 2 /g-C 3 N 4 Composite photocatalyst and preparation method and application thereof |
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