CN109759110B - Nitrogen-doped porous carbon loaded titanium dioxide photocatalyst and preparation method and application thereof - Google Patents
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Abstract
The invention discloses a nitrogen-doped porous carbon loaded titanium dioxide photocatalyst, and a preparation method and application thereof. The method utilizes an organometallic framework Material (MOF) at N2Calcining and carbonizing to obtain N-doped porous carbon material GC-N, dispersing the obtained GC-N in ethanol solution containing mineralizer, adding titanium source, and synthesizing GC-N-TiO by a hydrothermal method2A composite material. The preparation method is simple, does not need toxic reagents, can realize the doping of high-proportion nitrogen elements in the synthesis process, can improve the separation rate of photoproduction electrons and holes, increases the photocatalytic degradation efficiency of pollutants, and has excellent reaction stability. The prepared photocatalyst can be widely applied to the fields of atmospheric pollution treatment, water pollution treatment and the like.
Description
Technical Field
The invention belongs to the technical field of functional materials, and particularly relates to a nitrogen-doped porous carbon loaded titanium dioxide photocatalyst (GC-N-TiO)2) And a preparation method and application thereof.
Background
Along with the improvement of public environmental protection consciousness, the control day of Volatile Organic Compounds (VOCs)It is good for attention. VOCs not only come from industrial production, but also come from interior decoration and furniture, so that the influence on the population is wide, and the exposure time is long; many VOCs are not only highly toxic and carcinogenic, but also precursors to ozone, another atmospheric pollutant. The indoor environment has many limitations on the VOCs control technology, the traditional industrial treatment technology cannot be effectively applied, and the photocatalytic oxidation technology is widely concerned as an efficient and safe environment-friendly environmental purification technology. TiO 22The photocatalyst is the most commonly used photocatalyst due to the advantages of no toxicity, low price, stable chemical properties and the like, but has the defects of easy recombination of electron holes and low quantum efficiency, and the application effect of the photocatalyst is seriously influenced. Adding TiO into the mixture2The dispersion on the surface of the carrier and the inhibition of electron hole recombination are an effective way for improving the efficiency of photocatalytic degradation of organic pollutants. Wherein the porous carbon material has the characteristics of adsorbability and high conductivity, can enrich pollutants and rapidly transfer photogenerated electrons, and is used for improving TiO2The composite modified material with photocatalytic activity is ideal.
At present, the preparation of porous carbon Materials usually requires oxidation stripping and activation of graphite carbon by using strong oxidant such as concentrated sulfuric acid or potassium permanganate (e.g. chinese patent 201611177958.3 and journal Advanced Materials, 2009, 21, 2233-. The above methods inevitably use highly toxic and highly polluting substances, and the preparation method is complicated, which is not favorable for the production and application of catalytic materials.
In order to overcome the defects, the invention uses a metal organic framework containing nitrogen as a precursor, and the metal organic framework is carbonized by calcination and then mixed with TiO2Compounding to obtain porous carbon modified TiO containing nitrogen element2A material. The material prepared by the method not only has simple synthesis method and does not need toxic reagents, but also can realize nitrogen element doping in the material so that the material has higher conductivity and oxygen reduction capability, therebyPromoting TiO2The effective separation of the hole-electron pair shows excellent activity and stability, and is a new breakthrough in the field of photocatalytic materials. Meanwhile, the invention provides a new idea for treating organic pollutants.
Disclosure of Invention
The invention aims to overcome the defects of high photoproduction electron hole recombination rate of titanium dioxide in the traditional method, complex synthesis of the traditional porous carbon and titanium dioxide composite material, large pollution and the like, and provides a GC-N-TiO2Photocatalyst, and a preparation method and application thereof. The prepared photocatalyst obviously improves the activity and stability of the photocatalytic oxidation of VOCs.
The purpose of the invention is realized by the following technical scheme:
GC-N-TiO2The preparation method of the photocatalyst comprises the steps of synthesizing MOF by organic ligands and metal nodes, carbonizing, and carrying out hydrolytic polymerization, washing, drying and calcining with a titanium source in a specific solvent to obtain the nitrogen-doped porous carbon loaded titanium dioxide photocatalytic material. The MOF synthesized by using a nitrogen-containing organic framework is used as a precursor, metal Zn coordinated with nitrogen elements at high temperature volatilizes to generate defects so as to form pyridine nitrogen and pyrrole nitrogen structures, and the structure is further combined with TiO2In the process of compounding, nitrogen in the carbon substrate can replace an O atom to be directly connected with Ti, so that the transfer rate of photo-generated electrons from the Ti atom to the carbon substrate is further improved. The photocatalyst can improve the transfer rate of photo-generated electrons, promote the separation of electron holes, and has a carbon skeleton with stable chemical properties as a substrate, so that the photocatalytic activity and stability are improved.
GC-N-TiO2The preparation method of the photocatalyst is characterized in that an organic ligand and metal salt are used for synthesizing a metal organic framework, the metal organic framework is carbonized, and then the metal organic framework is hydrolyzed and polymerized in ethanol solution containing a titanium source, washed, dried and calcined to prepare the photocatalyst material compounded with the nitrogen-doped porous carbon.
GC-N-TiO2The preparation method of the photocatalyst is characterized by comprising the following steps:
(1) preparation of MOFs: adding 3-6 g of metal salt and 4-7 g of organic ligand into 150-300 ml of methanol, stirring at room temperature for 20-24 h, and then centrifugally separating, cleaning and drying the solution to finally obtain MOFs; the metal salt comprises zinc nitrate hexahydrate, zinc acetate or zinc sulfate; the organic ligand is 2-methylimidazole;
(2) preparation of GC-N: adding 0.1-0.3 g of MOFs into a crucible, placing the crucible in a tube furnace, and adding N2Calcining for 2-4 h in the atmosphere, cooling to room temperature, and collecting to obtain a nitrogen-doped porous carbon material GC-N;
（3）GC-N-TiO2the preparation of (1): adding 0.01-0.02 g of GC-N into 20-40 mL of absolute ethyl alcohol, ultrasonically mixing uniformly, stirring for 0-30 min at room temperature to obtain a solution A, then adding 2-5 mL of ammonia water, adding 1-10 mL of a titanium source into the stirred solution A, stirring for 30-60 min at room temperature to obtain a solution B, transferring the mixed solution B into a polytetrafluoroethylene reaction kettle liner, placing the polytetrafluoroethylene reaction kettle liner into a high-pressure reaction kettle, carrying out hydrothermal reaction for 9-13 h, carrying out centrifugal separation, cleaning and drying on the solution to obtain powder C, transferring the powder C into a crucible, placing the crucible into a tubular furnace, and placing the crucible into a N-type tubular furnace2Calcining for 2-4 h in atmosphere to obtain GC-N-TiO2A photocatalyst; the titanium source comprises butyl titanate and isopropyl titanate.
In the method, in the step (1), the stirring temperature at room temperature is 25-35 ℃, and the stirring speed is 15-25 r/min.
In the method, in the step (1), the centrifugal separation rotating speed is 4000-6000 revolutions; the washing solution is methanol; the drying temperature is 60-80 ℃, and the drying time is 6-8 h.
In the method, the calcining temperature of the tubular furnace in the step (2) is 900-1000 ℃, and the heating rate is 2-5 ℃/min.
In the method, the stirring temperature in the step (3) at room temperature is 25-35 ℃, and the stirring speed is 15-25 r/min.
In the method, the hydrothermal reaction temperature in the step (3) is 120-140 ℃; the hydrothermal reaction pressure is 0.1-0.3 MPa; the centrifugal separation rotating speed is 4000-6000 revolutions; the washing solution is ethanol or deionized water; the drying temperature is 60-80 ℃, and the drying time is 6-8 h.
In the method, the calcining temperature of the tubular furnace in the step (3) is 450-600 ℃, and the heating rate is 2-5 ℃/min. .
GC-N-TiO2The photocatalyst is applied to the fields of degradation of atmospheric volatile organic compounds and water pollution control.
The material prepared by the invention is essentially different from the existing material in that the nitrogen-containing organic metal framework is synthesized in advance and then N is added2Calcining at high temperature to form nitrogen-doped porous carbon with a mesoporous and microporous structure, then carrying out composite hydrolysis drying with a titanium source, and calcining to form anatase-phase TiO2In the process, N can be directly connected with Ti, so that photogenerated electrons are rapidly transferred, and the electron-hole recombination is inhibited. The nitrogen-containing carbon substrate can rapidly transfer photo-generated electrons, and the nitrogen atom on the carbon can also be used as an electron acceptor and O adsorbed on the surface2Reaction to form O2 -The photo-generated electrons can be fully utilized, and the recombination of the photo-generated electrons on a carbon substrate is avoided.
Compared with the prior art, the invention has the following advantages:
the invention synthesizes nitrogen-doped porous carbon by carbonizing an organic metal framework and is applied to the field of photocatalytic oxidation of VOCs for the first time.
The synthesis method is simple, does not need to use strong-toxicity and high-pollution medicines, and meets the aim of green chemistry.
The method can realize nitrogen doping of the carbon substrate and the titanium dioxide at the same time, and the N atoms on the carbon substrate are directly connected with the Ti atoms, so that the method has higher photoreaction efficiency compared with the common porous material. In addition, N atoms on the carbon material can serve as active sites, the carbon skeleton has stable chemical properties, and the large specific surface area has more active sites, so that the material has higher photocatalytic activity and stability, and can be widely applied to the aspects of air purification, water pollution treatment and the like.
Drawings
FIG. 1 shows TiO of the present invention2、GC-N-TiO2XRD pattern of photocatalyst;
FIG. 2 is a SEM image of GC-N;
FIG. 3 shows the GC-N-TiO compound after adding 5mL isopropyl titanate2Scanning electron microscope SEM picture;
FIG. 4 shows GC-N-TiO2A diagram of X-ray photoelectron spectrum C1s of the photocatalyst;
FIG. 5 shows GC-N-TiO2A diagram of an X-ray photoelectron spectrum N1s of the photocatalyst;
FIG. 6 shows GC-N-TiO2A 24-hour degradation concentration change diagram of the photocatalyst for toluene;
FIG. 7 shows GC-N-TiO2Photocatalyst for degrading CO in toluene for 24h x Generating a quantity change map;
FIG. 8 shows GC-N-TiO2And graphene-supported TiO2、TiO2And (3) a 24-hour degradation effect graph of toluene.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto, and may be carried out with reference to conventional techniques for process parameters not particularly noted.
Example 1
Preparation of GC-N: 5.95 g of zinc nitrate hexahydrate and 6.16 g of 2-methylimidazole were added to 300mL of methanol, stirred at room temperature for 24 hours, centrifuged, washed with methanol, and dried in an oven at 60 ℃ for 8 hours to obtain an organometallic framework ZIF-8. ZIF-8 is placed in a ceramic crucible, and heated in a tube furnace at a heating rate of 2 ℃/min under N2The temperature is increased to 920 ℃ under the atmosphere, and the mixture is calcined for 3h at 920 ℃. And cooling to room temperature to obtain the nitrogen-doped porous carbon material GC-N.
GC-N-TiO2The preparation of (1): dispersing 0.01 g GC-N in 40mL of absolute ethyl alcohol, performing ultrasonic dispersion for 30min to form a solution A, adding 2 mL of ammonia water, stirring at room temperature for 10 min to form a solution B, adding 5mL of isopropyl titanate into the solution B, continuously stirring for 20 min to form a mixed solution C, transferring the mixed solution C into a polytetrafluoroethylene reaction kettle lining, placing the lining into a high-pressure reaction kettle, performing hydrothermal reaction at 140 ℃ and 0.15 Mpa for 12 h, cooling to room temperature, performing centrifugal separation on precipitates, and removing the precipitates with ethanolWashing with ionized water, drying in a 60 deg.C oven to obtain powder D, placing powder D in a ceramic crucible, and heating at 2 deg.C/min in a tubular furnace at N2Heating to 500 ℃ in the atmosphere, calcining for 3h at 500 ℃, and cooling to room temperature to finally obtain GC-N-TiO2. From the X-ray diffraction pattern (figure 1) of the photocatalytic material, we can know that the TiO of anatase phase is successfully synthesized2And has higher crystallinity. The synthesized GC-N-TiO can be seen from a scanning electron microscope2The photocatalyst (FIG. 3) has a similar morphology and size to GC-N (FIG. 2), indicating that TiO2Can be uniformly dispersed on GC-N. From the X-ray photoelectron spectra (fig. 4, fig. 5), signal peaks of C-N bond and C = N bond as well as Ti-N bond can be observed, demonstrating that both carbon substrate and titanium dioxide are doped with nitrogen. In conclusion, the successful synthesis of GC-N-TiO is proved2A photocatalyst.
Example 2
Preparation of GC-N: 5.95 g of zinc nitrate hexahydrate and 6.16 g of 2-methylimidazole were added to 300mL of methanol, stirred at room temperature for 24 hours, centrifuged, washed with methanol, and dried in an oven at 60 ℃ for 8 hours to obtain an organometallic framework ZIF-8. ZIF-8 is placed in a ceramic crucible, and heated in a tube furnace at a heating rate of 2 ℃/min under N2The temperature is increased to 920 ℃ under the atmosphere, and the mixture is calcined for 3h at 920 ℃. And cooling to room temperature to obtain the nitrogen-doped porous carbon material GC-N.
GC-N-TiO2The preparation of (1): dispersing 0.01 g GC-N in 40mL of absolute ethyl alcohol, performing ultrasonic dispersion for 30min to form a solution A, adding 2 mL of ammonia water, stirring at room temperature for 10 min to form a solution B, adding 1 mL of isopropyl titanate into the solution B, continuously stirring for 20 min to form a mixed solution C, transferring the mixed solution C into a polytetrafluoroethylene reaction kettle lining, putting the lining into a high-pressure reaction kettle, performing hydrothermal reaction at 140 ℃ and 0.15 Mpa for 12 h, cooling to room temperature, performing centrifugal separation on precipitates, washing with ethanol and deionized water, drying in a 60 ℃ oven to obtain powder D, putting the powder D into a ceramic crucible, and heating in a tubular furnace at the temperature rise rate of 2 ℃/min in N2Heating to 500 ℃ in the atmosphere, calcining for 3h at 500 ℃, and cooling to room temperature to finally obtain GC-N-TiO2。
Example 3
Preparation of GC-N: 5.95 g of zinc nitrate hexahydrate and 6.16 g of 2-methylimidazole were added to 300mL of methanol, stirred at room temperature for 24 hours, centrifuged, washed with methanol, and dried in an oven at 60 ℃ for 8 hours to obtain an organometallic framework ZIF-8. ZIF-8 is placed in a ceramic crucible, and heated in a tube furnace at a heating rate of 2 ℃/min under N2The temperature is increased to 920 ℃ under the atmosphere, and the mixture is calcined for 3h at 920 ℃. And cooling to room temperature to obtain the nitrogen-doped porous carbon material GC-N.
GC-N-TiO2The preparation of (1): dispersing 0.01 g GC-N in 40mL of absolute ethyl alcohol, performing ultrasonic dispersion for 30min to form a solution A, adding 2 mL of ammonia water, stirring at room temperature for 10 min to form a solution B, adding 10mL of isopropyl titanate into the solution B, continuously stirring for 20 min to form a mixed solution C, transferring the mixed solution C into a polytetrafluoroethylene reaction kettle lining, putting the lining into a high-pressure reaction kettle, performing hydrothermal reaction at 140 ℃ and 0.15 Mpa for 12 h, cooling to room temperature, performing centrifugal separation on precipitates, washing with ethanol and deionized water, drying in a 60 ℃ oven to obtain powder D, putting the powder D into a ceramic crucible, and heating in a tubular furnace at the temperature rise rate of 2 ℃/min in N2Heating to 500 ℃ in the atmosphere, calcining for 3h at 500 ℃, and cooling to room temperature to finally obtain GC-N-TiO2。
Example 4
Graphene-supported TiO2The preparation of (1): 2g of commercially available anatase TiO2Adding the mixture into 400 mL of deionized water, performing ultrasonic dispersion for 30min to form a solution E, adding 0.02g of graphene oxide, performing ultrasonic dispersion for 1 h to form a mixed solution F, transferring the mixed solution F into a liner of a polytetrafluoroethylene reaction kettle, placing the liner into a high-pressure reaction kettle, performing hydrothermal reaction at 120 ℃ and 0.15 Mpa for 12 h, cooling to room temperature, performing centrifugal separation on a precipitate, washing with deionized water, drying in a 60 ℃ oven, and finally obtaining the graphene-loaded TiO2。
Photocatalytic activity analysis: toluene is used as a target pollutant, and the photocatalytic activity of the catalyst under different light sources is explored. Photocatalytic degradation of tolueneThe reaction is carried out on a self-made reactor, and the toluene is degraded by adopting a full spectrum, wherein the light intensity is 200 mW/cm2(ii) a The volume of the reactor is 2 mL; the dosage of the catalyst is 100 mg; the initial concentration of toluene was 25 ppm; the flow rate of the reaction gas is 100 mL/min; relative humidity is 60%; the adsorption/desorption equilibrium is reached after 3 hours of dark adsorption reaction, and then the lamp is turned on; the concentration value of toluene is detected by adopting a gas chromatography with a hydrogen ion Flame (FID) detector and a nickel converter, and experimental results show that the TiO compounded with the nitrogen-doped porous carbon is2Material ratio pure TiO2Material and graphene-loaded TiO2Has excellent performance of degrading toluene by photocatalysis. The results show that: GC-N-TiO2The photocatalyst shows purer TiO2Higher performance of degrading toluene by photocatalysis. After 24h of illumination, GC-N-TiO2The degradation rate of the toluene is still kept above 60 percent (figure 6), the mineralization rate is also kept at 80 percent (figure 7), and the pure TiO is2The inactivation is completed only 12 h under illumination, and the TiO loaded by the graphene2Activity also decreased significantly at 18 hours (figure 8).
The above examples are merely illustrative of the technical solutions of the present invention and not restrictive, and it will be understood by those of ordinary skill in the art that various changes in the details or forms thereof may be made without departing from the spirit and scope of the present invention as defined by the claims.
Claims (3)
1. GC-N-TiO2The preparation method of the photocatalyst is characterized in that an organic ligand and metal salt are used for synthesizing a metal organic framework, and the metal organic framework is carbonized and then hydrolyzed and polymerized in ethanol solution containing a titanium source, washed, dried and calcined to prepare the photocatalytic material compounded with nitrogen-doped porous carbon; the method comprises the following specific steps:
(1) preparation of MOFs: adding 3-6 g of metal salt and 4-7 g of organic ligand into 150-300 ml of methanol, stirring at room temperature for 20-24 h, and then centrifugally separating, cleaning and drying the solution to finally obtain MOFs; the metal salt comprises zinc nitrate hexahydrate, zinc acetate or zinc sulfate; the organic ligand is 2-methylimidazole;
(2) preparation of GC-N: adding 0.1-0.3 g of MOFs into a crucible, placing the crucible in a tube furnace, and adding N2Calcining for 2-4 h in the atmosphere, cooling to room temperature, and collecting to obtain a nitrogen-doped porous carbon material GC-N;
(3)GC-N-TiO2the preparation of (1): adding 0.01-0.02 g of GC-N into 20-40 mL of absolute ethyl alcohol, ultrasonically mixing uniformly, stirring for 0-30 min at room temperature to obtain a solution A, then adding 2-5 mL of ammonia water, adding 1-10 mL of a titanium source into the stirred solution A, stirring for 30-60 min at room temperature to obtain a solution B, transferring the mixed solution B into a polytetrafluoroethylene reaction kettle liner, placing the polytetrafluoroethylene reaction kettle liner into a high-pressure reaction kettle, carrying out hydrothermal reaction for 9-13 h, carrying out centrifugal separation, cleaning and drying on the solution to obtain powder C, transferring the powder C into a crucible, placing the crucible into a tubular furnace, and placing the crucible into a N-type tubular furnace2Calcining for 2-4 h in atmosphere to obtain GC-N-TiO2A photocatalyst; the titanium source comprises butyl titanate and isopropyl titanate;
in the step (1), the stirring temperature at room temperature is 25-35 ℃, and the stirring speed is 15-25 r/min;
the centrifugal separation rotating speed is 4000-6000 r/min; the cleaning solution is methanol or ethanol; the drying temperature is 60-80 ℃, and the drying time is 6-8 h;
in the step (2), the calcining temperature of the tubular furnace is 900-1000 ℃, and the heating rate is 2-5 ℃/min;
in the step (3), the stirring temperature at room temperature is 25-35 ℃, and the stirring speed is 15-25 r/min;
the hydrothermal reaction temperature is 120-140 ℃; the hydrothermal reaction pressure is 0.1-0.3 MPa; the centrifugal separation rotating speed is 4000-6000 r/min; the cleaning solution is ethanol or deionized water; the drying temperature is 60-80 ℃, and the drying time is 6-8 h;
the calcining temperature of the tubular furnace is 450-600 ℃, and the heating rate is 2-5 ℃/min.
2. GC-N-TiO compound produced by the production method according to claim 12A photocatalyst.
3. A GC-N-TiO compound as claimed in claim 22The photocatalyst is applied to the fields of degradation of atmospheric volatile organic compounds and water pollution control.
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