CN111545233A - Boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants and preparation method thereof - Google Patents
Boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants and preparation method thereof Download PDFInfo
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- 239000000809 air pollutant Substances 0.000 title claims abstract description 40
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- 230000004044 response Effects 0.000 title claims abstract description 38
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 174
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
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- 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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/007—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by irradiation
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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Abstract
The invention discloses a boron nitrogen carbon broadband response photocatalyst capable of removing air pollutants and a preparation method thereof, and belongs to the field of photocatalyst material preparation and indoor air treatment. According to the method, non-metal elements such as boron, nitrogen and carbon are used as photocatalytic components, the local structure of the boron-nitrogen carbon material is adjusted by atmosphere heat treatment, and the boron-nitrogen carbon material after heat treatment has good stability due to wide visible light response and can effectively generate active oxygen species under visible light, so that the boron-nitrogen carbon material has an excellent degradation effect on volatile organic gas pollutants, nitrogen oxides and the like in indoor air. The catalyst has stable and excellent performance, wide photoresponse range, easily obtained raw materials and simple preparation, and can be widely applied to the field of indoor air treatment and other environmental treatment.
Description
Technical Field
The invention relates to a preparation method of a photocatalyst, in particular to a preparation method of a photocatalyst capable of degrading air pollutants, which is applied to the technical fields of photocatalyst material preparation and indoor air treatment.
Background
Indoor air contains a large amount of pollutants, wherein volatile organic gas pollutants account for one of the most main pollutants, and the sources of the pollutants are wide, and the pollutants comprise indoor building decoration materials, kitchen oil smoke, daily-used disinfectants, cosmetic solvents, outdoor polluted air and the like. Volatile organic gas pollutants can harm human health and cause various diseases. At present, the relevant standards of indoor air quality in China are 'control standard of indoor environmental pollutants for civil buildings' and 'standard of indoor air quality', and clear requirements are provided for volatile organic pollutants. According to GB/T18883-2002, the concentration of formaldehyde in the indoor house is not higher than 0.10mg/m3The concentration of toluene is not higher than 0.2mg/m3And the like.
The photocatalysis technology is a green environmental technology and has the advantages of mild reaction conditions and high free radical reaction rate. The active oxygen species can be generated in situ on the surface of the catalyst by utilizing light energy, and the active oxygen species and pollutant molecules adsorbed on the surface of the catalyst interact with each other to decompose and convert the pollutant molecules so as to purify air pollutants. At present TiO2Is the most common air purification photocatalyst, but TiO2The forbidden band width is 3.2eV, so that the ultraviolet light can only excite electron holes under the ultraviolet light, and the ultraviolet light only accounts for about 5% of the solar spectrum; simultaneous TiO 22In the process of degrading volatile organic pollutants, the carbonaceous intermediate species in the degradation process are easy to be strongly adsorbed on TiO2Surface, active site masking, resulting in TiO2Is inactivated. The volatile organic compounds in the indoor air often produce various intermediate products in a large quantity in the degradation process, and the intermediate products are applied to the bodyMay still pose a hazard. Therefore, the development of a photocatalyst with high stability, wide spectral response and high mineralization rate for indoor air purification has important significance, and becomes a technical problem to be solved urgently.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects in the prior art, and provides the boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants and the preparation method thereof.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
a preparation method of a boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants comprises the following steps:
a. pretreatment of raw materials:
fully grinding a boron source, a nitrogen source and a carbon source in a certain content ratio to uniformly mix the boron source, the nitrogen source and the carbon source to obtain raw material powder; wherein the boron source accounts for 75-100% of the nitrogen source by mass, and the carbon source accounts for 2-20% of the nitrogen source by mass;
b. high-temperature pyrolysis:
under the atmosphere protection condition, obtaining a blocky solid by using a high-temperature pyrolysis method, then grinding the blocky solid into powder, cleaning by using dilute acid, then carrying out suction filtration, then fully washing, collecting and drying to obtain intermediate product powder;
c. and (3) heat treatment:
and placing the obtained intermediate product powder in a tubular furnace, carrying out heat treatment, washing the obtained catalyst material powder with dilute acid, carrying out suction filtration, fully washing and drying to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
As a preferred technical scheme of the present invention, in the step a, the boron source is any one or a mixture of any several of borax, boric acid, boric anhydride, elemental boron and boron carbide.
In the step a, the nitrogen source is any one or a mixture of any several of melamine, dicyandiamide, thiourea and urea.
In the step a, the carbon source is any one or a mixture of any several of graphite, urea, thiourea, glucose and starch.
As a preferred technical scheme of the invention, in the step b, the heating rate of the high-temperature pyrolysis reaction is 2-10 ℃/min, and the temperature of the high-temperature pyrolysis is 700-1500 ℃.
In the step b, the high-temperature pyrolysis reaction is carried out for 3-8 hours, and then the temperature is naturally reduced.
As a preferable technical scheme of the invention, in the step b, the protective atmosphere of the high-temperature pyrolysis is N2、Ar、H2Any one or a mixture of any several of the mixed gases of/Ar.
In the step c, the initial temperature for heat treatment is not lower than 20 ℃, the heating rate is not lower than 4 ℃/min, and the temperature is increased to 500-900 ℃ for heat treatment.
In the step c, the heat treatment and heat preservation time is 1-8 hours, and then the temperature is naturally reduced.
In a preferred embodiment of the present invention, in the step c, the atmosphere for the heat treatment is N2、Ar、O2And any one or a mixture of any more of high-purity air.
In the step b and the step c, the diluted acid is any one or a mixture of any more of diluted hydrochloric acid, diluted nitric acid and diluted sulfuric acid.
The invention relates to a boron nitrogen carbon broadband response photocatalyst capable of removing air pollutants, which is prepared by adopting the preparation method of the boron nitrogen carbon broadband response photocatalyst capable of removing air pollutants.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the method can prepare the photocatalyst for indoor air purification with high stability, wide spectral response and high mineralization rate, and provides a method for preparing the photocatalyst for indoor air purification, which has the advantages of easily obtained raw materials and simple preparation;
2. the method is simple, low in cost, good in air purification effect and suitable for popularization and application.
Drawings
Fig. 1 is a TEM photograph of the boron-nitrogen-carbon photocatalyst material prepared by the method of embodiment 1 of the present invention.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
example 1:
in this embodiment, a method for preparing a boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants includes the following steps:
weighing 4g of urea, 3g of boric acid and 0.1g of starch, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, introducing nitrogen for 1 hour under a high-temperature tube furnace, and removing impurity gas in the tube; heating to 1200 ℃ from an initial temperature of 50 ℃ at a heating rate of 3 ℃/min under a nitrogen atmosphere, preserving heat for 5 hours, recovering to room temperature to obtain a hard block solid, scraping the hard block solid, grinding the hard block solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at 60 ℃ to obtain powder.
And then placing the obtained powder in a tubular furnace, heating to 700 ℃ at a speed of 5 ℃/min in the air atmosphere, preserving heat for 3 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the above-described photocatalyst prepared by the method of this exampleMicroscopic observation is carried out by taking the agent material as a sample, as shown in fig. 1, fig. 1 is a TEM photograph of the boron-nitrogen-carbon photocatalyst material prepared by the method in this embodiment, and it can be seen that the boron-nitrogen-carbon photocatalyst material prepared by the method in this embodiment forms a mineralized material. The ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is tested to determine the light absorption range. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, blowing the reactor with 30ppm toluene standard gas before reaction, performing catalytic degradation on gaseous toluene under the irradiation of a xenon lamp (with a 420nm filter), testing the performance and stability of the gaseous toluene degraded under visible light, wherein the catalytic degradation is performed under 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 2:
this embodiment is substantially the same as embodiment 1, and is characterized in that:
in this embodiment, a method for preparing a boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants includes the following steps:
weighing 4g of melamine, 3g of boric acid and 0.1g of starch, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, and introducing nitrogen for 1 hour under a high-temperature tube furnace to remove impurity gases in the tube. Heating to 1200 ℃ from an initial temperature of 50 ℃ at a heating rate of 3 ℃/min under a nitrogen atmosphere, preserving heat for 5 hours, recovering to room temperature to obtain a hard block solid, scraping the hard block solid, grinding the hard block solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at 60 ℃ to obtain powder.
And (3) placing the obtained powder in a tubular furnace, heating to 700 ℃ at a speed of 5 ℃/min in the air atmosphere, preserving heat for 3 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
testingThe light absorption range of the ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is determined. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, blowing the reactor with 30ppm toluene standard gas before reaction, performing catalytic degradation on gaseous toluene under the irradiation of a xenon lamp (with a 420nm filter), testing the performance and stability of the gaseous toluene degraded under visible light, wherein the catalytic degradation is performed under 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 3:
this embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a method for preparing a boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants includes the following steps:
weighing 4g of urea, 3g of borax and 0.1g of starch, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, introducing nitrogen for 1 hour under a high-temperature tube furnace, and discharging impurity gas in the tube. Heating to 1200 ℃ from an initial temperature of 50 ℃ at a heating rate of 3 ℃/min under a nitrogen atmosphere, preserving heat for 5 hours, recovering to room temperature to obtain a hard block solid, scraping the hard block solid, grinding the hard block solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at 60 ℃ to obtain powder.
And (3) placing the obtained powder in a tubular furnace, heating to 700 ℃ at a speed of 5 ℃/min in the air atmosphere, preserving heat for 3 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is tested to determine the light absorption range. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, and reactingBlowing the reactor with 30ppm toluene standard gas, catalytically degrading gaseous toluene under the irradiation of xenon lamp (with 420nm filter), and testing the performance and stability of degrading gaseous toluene under visible light, wherein the gas content is 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 4
Weighing 4g of urea, 3g of boric acid and 0.1g of glucose, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, and introducing nitrogen for 1 hour under a high-temperature tube furnace to remove impurity gases in the tube. Heating to 1200 ℃ from an initial temperature of 50 ℃ at a heating rate of 3 ℃/min under a nitrogen atmosphere, preserving heat for 5 hours, recovering to room temperature to obtain a hard block solid, scraping the hard block solid, grinding the hard block solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at 60 ℃ to obtain powder.
And (3) placing the obtained powder in a tubular furnace, heating to 700 ℃ at a speed of 5 ℃/min in the air atmosphere, preserving heat for 3 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is tested to determine the light absorption range. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, blowing the reactor with 30ppm toluene standard gas before reaction, performing catalytic degradation on gaseous toluene under the irradiation of a xenon lamp (with a 420nm filter), testing the performance and stability of the gaseous toluene degraded under visible light, wherein the catalytic degradation is performed under 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 5
Weighing 4g of urea, 3.8g of boric acid and 0.1g of glucose, mixing, grinding the mixture thoroughly for 20min, transferring it to a corundum boat with a cover, and introducing nitrogen gas for 1 hour under a high-temperature tube furnace to remove impurity gases in the tube. Heating to 1200 ℃ from an initial temperature of 50 ℃ at a heating rate of 3 ℃/min under a nitrogen atmosphere, preserving heat for 5 hours, recovering to room temperature to obtain a hard block solid, scraping the hard block solid, grinding the hard block solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at 60 ℃ to obtain powder.
And (3) placing the obtained powder in a tubular furnace, heating to 700 ℃ at a speed of 5 ℃/min in the air atmosphere, preserving heat for 3 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is tested to determine the light absorption range. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, blowing the reactor with 30ppm toluene standard gas before reaction, performing catalytic degradation on gaseous toluene under the irradiation of a xenon lamp (with a 420nm filter), testing the performance and stability of the gaseous toluene degraded under visible light, wherein the catalytic degradation is performed under 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 6
Weighing 4g of urea, 3.8g of boric acid and 0.3g of glucose, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, and introducing nitrogen for 1 hour under a high-temperature tube furnace to remove impurity gases in the tube. Heating to 1200 ℃ from an initial temperature of 50 ℃ at a heating rate of 3 ℃/min under a nitrogen atmosphere, preserving heat for 5 hours, recovering to room temperature to obtain a hard block solid, scraping the hard block solid, grinding the hard block solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at 60 ℃ to obtain powder.
And (3) placing the obtained powder in a tubular furnace, heating to 700 ℃ at a speed of 5 ℃/min in the air atmosphere, preserving heat for 3 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is tested to determine the light absorption range. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, blowing the reactor with 30ppm toluene standard gas before reaction, performing catalytic degradation on gaseous toluene under the irradiation of a xenon lamp (with a 420nm filter), testing the performance and stability of the gaseous toluene degraded under visible light, wherein the catalytic degradation is performed under 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 7
Weighing 4g of urea, 3.8g of boric acid and 0.3g of glucose, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, and introducing argon for 1 hour under a high-temperature tube furnace to remove impurity gases in the tube. Heating to 1200 ℃ from an initial temperature of 50 ℃ at a heating rate of 3 ℃/min under an argon atmosphere, preserving heat for 5 hours, recovering to room temperature to obtain a hard block solid, scraping the hard block solid, grinding the hard block solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at 60 ℃ to obtain powder.
And (3) placing the obtained powder in a tubular furnace, heating to 700 ℃ at a speed of 5 ℃/min in the air atmosphere, preserving heat for 3 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is tested to determine the light absorption range. Uniformly coating the prepared powder catalyst on frosted quartzOn the chip, the performance evaluation is carried out in a steel closed quartz reactor, the reactor is blown by 30ppm toluene standard gas before the reaction, gaseous toluene is catalyzed and degraded under the irradiation of a xenon lamp (with a 420nm filter), the performance and the stability of the gaseous toluene degraded under the visible light are tested, and the performance and the stability of the gaseous toluene are tested under the condition of 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 8
Weighing 4g of urea, 3.8g of boric acid and 0.3g of glucose, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, and introducing argon for 1 hour under a high-temperature tube furnace to remove impurity gases in the tube. Heating to 1200 ℃ from an initial temperature of 50 ℃ at a heating rate of 2 ℃/min under an argon atmosphere, preserving heat for 5 hours, recovering to room temperature to obtain a hard block solid, scraping the hard block solid, grinding the hard block solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at 60 ℃ to obtain powder.
And (3) placing the obtained powder in a tubular furnace, heating to 700 ℃ at a speed of 5 ℃/min in the air atmosphere, preserving heat for 3 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is tested to determine the light absorption range. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, blowing the reactor with 30ppm toluene standard gas before reaction, performing catalytic degradation on gaseous toluene under the irradiation of a xenon lamp (with a 420nm filter), testing the performance and stability of the gaseous toluene degraded under visible light, wherein the catalytic degradation is performed under 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 9
Weighing 4g of urea, 3.8g of boric acid and 0.3g of glucose, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, and introducing argon for 1 hour under a high-temperature tube furnace to remove impurity gases in the tube. Heating to 900 ℃ from the initial temperature of 50 ℃ at the heating rate of 2 ℃/min under the argon atmosphere, preserving the heat for 5 hours, then recovering to the room temperature to obtain a hard block-shaped solid, scraping the solid, grinding the solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at the temperature of 60 ℃ to obtain the powder.
And (3) placing the obtained powder in a tubular furnace, heating to 700 ℃ at a speed of 5 ℃/min in the air atmosphere, preserving heat for 3 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is tested to determine the light absorption range. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, blowing the reactor with 30ppm toluene standard gas before reaction, performing catalytic degradation on gaseous toluene under the irradiation of a xenon lamp (with a 420nm filter), testing the performance and stability of the gaseous toluene degraded under visible light, wherein the catalytic degradation is performed under 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 10
Weighing 4g of urea, 3.8g of boric acid and 0.3g of glucose, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, and introducing argon for 1 hour under a high-temperature tube furnace to remove impurity gases in the tube. Heating to 900 ℃ from the initial temperature of 50 ℃ at the heating rate of 2 ℃/min under the argon atmosphere, preserving the heat for 3 hours, then returning to the room temperature to obtain a hard block-shaped solid, scraping the solid, grinding the solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at the temperature of 60 ℃ to obtain powder.
And (3) placing the obtained powder in a tubular furnace, heating to 700 ℃ at a speed of 5 ℃/min in the air atmosphere, preserving heat for 3 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is tested to determine the light absorption range. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, blowing the reactor with 30ppm toluene standard gas before reaction, performing catalytic degradation on gaseous toluene under the irradiation of a xenon lamp (with a 420nm filter), testing the performance and stability of the gaseous toluene degraded under visible light, wherein the catalytic degradation is performed under 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 11
Weighing 4g of urea, 3.8g of boric acid and 0.3g of glucose, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, and introducing argon for 1 hour under a high-temperature tube furnace to remove impurity gases in the tube. Heating to 900 ℃ from the initial temperature of 50 ℃ at the heating rate of 2 ℃/min under the argon atmosphere, preserving the heat for 3 hours, then returning to the room temperature to obtain a hard block-shaped solid, scraping the solid, grinding the solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at the temperature of 60 ℃ to obtain powder.
The powder obtained is placed in a tube furnace in H2Heating to 700 ℃ at the speed of 5 ℃/min under the atmosphere, preserving heat for 3 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at the temperature of 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the above photocatalyst material prepared by the method of this example was tested for its uv diffuse reflectance curve,the absorption range was determined. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, blowing the reactor with 30ppm toluene standard gas before reaction, performing catalytic degradation on gaseous toluene under the irradiation of a xenon lamp (with a 420nm filter), testing the performance and stability of the gaseous toluene degraded under visible light, wherein the catalytic degradation is performed under 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 12
Weighing 4g of urea, 3.8g of boric acid and 0.3g of glucose, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, and introducing argon for 1 hour under a high-temperature tube furnace to remove impurity gases in the tube. Heating to 900 ℃ from the initial temperature of 50 ℃ at the heating rate of 2 ℃/min under the argon atmosphere, preserving the heat for 3 hours, then returning to the room temperature to obtain a hard block-shaped solid, scraping the solid, grinding the solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at the temperature of 60 ℃ to obtain powder.
The powder obtained is placed in a tube furnace in H2Heating to 500 ℃ at the speed of 5 ℃/min under the atmosphere, preserving heat for 3 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at the temperature of 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is tested to determine the light absorption range. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, blowing the reactor with 30ppm toluene standard gas before reaction, performing catalytic degradation on gaseous toluene under the irradiation of a xenon lamp (with a 420nm filter), testing the performance and stability of the gaseous toluene degraded under visible light, wherein the catalytic degradation is performed under 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 13
Weighing 4g of urea, 3.8g of boric acid and 0.3g of glucose, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, and introducing argon for 1 hour under a high-temperature tube furnace to remove impurity gases in the tube. Heating to 900 ℃ from the initial temperature of 50 ℃ at the heating rate of 2 ℃/min under the argon atmosphere, preserving the heat for 3 hours, then returning to the room temperature to obtain a hard block-shaped solid, scraping the solid, grinding the solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours by using dilute hydrochloric acid, performing suction filtration, washing the powder for 3 times by using deionized water, collecting a sample, and drying the sample at the temperature of 60 ℃ to obtain powder.
The powder obtained is placed in a tube furnace in H2Heating to 500 ℃ at the speed of 5 ℃/min under the atmosphere, preserving heat for 5 hours, washing the obtained powder sample with dilute hydrochloric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at the temperature of 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is tested to determine the light absorption range. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, blowing the reactor with 30ppm toluene standard gas before reaction, performing catalytic degradation on gaseous toluene under the irradiation of a xenon lamp (with a 420nm filter), testing the performance and stability of the gaseous toluene degraded under visible light, wherein the catalytic degradation is performed under 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
Example 14
Weighing 4g of urea, 3.8g of boric acid and 0.3g of glucose, mixing, fully grinding the mixture for 20min, transferring the mixture into a corundum boat with a cover, and introducing argon for 1 hour under a high-temperature tube furnace to remove impurity gases in the tube. Heating to 900 ℃ from an initial temperature of 50 ℃ at a heating rate of 2 ℃/min under an argon atmosphere, preserving heat for 3 hours, then returning to room temperature to obtain a hard block-shaped solid, scraping the solid, grinding the solid into powder, placing the powder into a serum bottle, washing the powder for 4 hours with dilute nitric acid, performing suction filtration, washing the powder for 3 times with deionized water, collecting a sample, and drying the sample at 60 ℃ to obtain powder.
The powder obtained is placed in a tube furnace in H2Heating to 500 ℃ at the speed of 5 ℃/min under the atmosphere, preserving heat for 5 hours, washing the obtained powder sample with dilute nitric acid, performing suction filtration, washing with deionized water for 3 times, collecting the sample, and drying at the temperature of 60 ℃ to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
Experimental test analysis:
the ultraviolet diffuse reflection curve of the photocatalyst material prepared by the method of the embodiment is tested to determine the light absorption range. Uniformly coating the prepared powder catalyst on a frosted quartz plate, performing performance evaluation in a steel closed quartz reactor, blowing the reactor with 30ppm toluene standard gas before reaction, performing catalytic degradation on gaseous toluene under the irradiation of a xenon lamp (with a 420nm filter), testing the performance and stability of the gaseous toluene degraded under visible light, wherein the catalytic degradation is performed under 100mW/cm2Can effectively degrade 30ppm toluene and generate 200ppm CO under the visible light2And has excellent mineralization rate and wide spectral response.
In conclusion, the method can prepare the boron-nitrogen-carbon broadband response photocatalyst for efficiently and stably removing indoor air pollutants, adopts non-metallic elements of boron, nitrogen and carbon as photocatalytic components, and adopts atmosphere heat treatment to adjust the local structure of the photocatalyst, and the boron-nitrogen-carbon material after heat treatment has wide visible light response and good stability, can effectively generate active oxygen species under visible light, and has excellent degradation effect on volatile organic gas pollutants, nitrogen oxides and the like in indoor air. The catalyst has stable and excellent performance, wide photoresponse range, easily obtained raw materials and simple preparation, and can be widely applied to the field of indoor air treatment and other environmental treatment.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitution ways, so long as the purpose of the present invention is met, and the boron nitrogen carbon broadband response photocatalyst capable of removing air pollutants and the technical principle and inventive concept of the preparation method thereof shall fall within the protection scope of the present invention.
Claims (9)
1. A preparation method of a boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants is characterized by comprising the following steps:
a. pretreatment of raw materials:
fully grinding a boron source, a nitrogen source and a carbon source in a certain content ratio to uniformly mix the boron source, the nitrogen source and the carbon source to obtain raw material powder; wherein the boron source accounts for 75-100% of the nitrogen source by mass, and the carbon source accounts for 2-20% of the nitrogen source by mass;
b. high-temperature pyrolysis:
under the atmosphere protection condition, obtaining a blocky solid by using a high-temperature pyrolysis method, then grinding the blocky solid into powder, cleaning by using dilute acid, then carrying out suction filtration, then fully washing, collecting and drying to obtain intermediate product powder;
c. and (3) heat treatment:
and placing the obtained intermediate product powder in a tubular furnace, carrying out heat treatment, washing the obtained catalyst material powder with dilute acid, carrying out suction filtration, fully washing and drying to obtain the boron-nitrogen-carbon photocatalyst material for efficiently and stably removing indoor air pollutants.
2. The method for preparing the boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants according to claim 1, wherein in the step a, the boron source is any one or a mixture of any several of borax, boric acid, boric anhydride, elemental boron and boron carbide;
the nitrogen source is any one or a mixture of any more of melamine, dicyandiamide, thiourea and urea;
the carbon source is any one or a mixture of any several of graphite, urea, thiourea, glucose and starch.
3. The method for preparing a boron nitrogen carbon broadband response photocatalyst capable of removing air pollutants as claimed in claim 1, wherein in the step b, the temperature rise rate of the high-temperature pyrolysis reaction is 2-10 ℃/min, and the temperature of the high-temperature pyrolysis is 700-1500 ℃; or, the high-temperature pyrolysis reaction is carried out for 3-8 hours, and then the temperature is naturally reduced.
4. The method for preparing boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants according to claim 1, wherein in the step b, the protective atmosphere of high-temperature pyrolysis is N2、Ar、H2Any one or a mixture of any several of the mixed gases of/Ar.
5. The method for preparing a boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants according to claim 1, wherein in the step c, the initial temperature for heat treatment is not lower than 20 ℃, the heating rate is not lower than 4 ℃/min, and the temperature is increased to 500-900 ℃ for heat treatment.
6. The method for preparing the boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants according to claim 1, wherein in the step c, the heat treatment and heat preservation time is 1-8 hours, and then the temperature is naturally reduced.
7. The method for preparing boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants according to claim 1, wherein in the step c, the atmosphere for heat treatment is N2、Ar、O2And any one or a mixture of any more of high-purity air.
8. The method for preparing a boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants according to claim 1, wherein in the steps b and c, the dilute acid is any one or a mixture of any several of dilute hydrochloric acid, dilute nitric acid and dilute sulfuric acid.
9. The boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants is characterized by being prepared by the preparation method of the boron-nitrogen-carbon broadband response photocatalyst capable of removing air pollutants according to claim 1.
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| CN103721737A (en) * | 2014-01-07 | 2014-04-16 | 福州大学 | Non-metallic material for driving photocatalytic decomposition of water by using efficient visible light |
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| CN103721737A (en) * | 2014-01-07 | 2014-04-16 | 福州大学 | Non-metallic material for driving photocatalytic decomposition of water by using efficient visible light |
| CN108855187A (en) * | 2018-07-02 | 2018-11-23 | 福州大学 | A kind of fluorine richness boron carbon nitrogen catalysis material and its application in efficiently reduction carbon dioxide |
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