CN115957749A - Platinum-loaded titanium dioxide composite photocatalyst, preparation method thereof and application thereof in degradation of harmful pollutants - Google Patents
Platinum-loaded titanium dioxide composite photocatalyst, preparation method thereof and application thereof in degradation of harmful pollutants Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a platinum-loaded titanium dioxide composite photocatalyst, a preparation method thereof and a method for degrading harmful pollutants such as methyl mercaptan, formaldehyde, ammonia gas and the like under the illumination condition. Catalyst curing supportThe body is flexible porous cellucotton and TiO loaded by platinum 2 The composite material is a catalyst for light reaction. In the experiment of photocatalytic degradation of harmful pollutants, the composite TiO is added 2 The photocatalytic material is solidified on the flexible porous cellucotton, harmful pollutants such as methyl mercaptan, formaldehyde, ammonia gas and the like can be completely degraded in a short time under the condition of all-band illumination, and the composite material still keeps good stability after multiple cycle tests. The composite photocatalyst loaded with the noble metal platinum has wide application prospect in various spaces in which harmful pollutants such as methyl mercaptan, formaldehyde, ammonia gas and the like need to be removed, and the method can bring huge potential economic and social effects.
Description
Technical Field
The invention belongs to the technical field of photocatalytic degradation of pollutants, and particularly relates to a platinum-supported titanium dioxide composite photocatalyst, a preparation method thereof, and a method for degrading harmful pollutants such as methyl mercaptan, formaldehyde, ammonia gas and the like under the condition of illumination by using the material.
Background
Methyl mercaptan is a typical sulfur-containing organic malodorous gas pollutant, has the taste of rotten cabbage, and is mainly produced and living activities such as animal and plant rotting, paper making industry, petroleum refining, sewage treatment and the like. The discharge amount, grade and concentration of common malodorous gases are specified in the emission standard of malodorous pollutants, wherein the influence of methyl mercaptan on human bodies is the largest even at 0.2 ppm (0.3 mg/m) 3 ) Can be unbearable under the concentration. Formaldehyde is a typical oneHydrocarbon malodorous gas pollutants widely exist in living and working places of people, formaldehyde can have adverse effects on human nervous systems, respiratory systems, cardiovascular systems and the like, and can cause diseases such as cancers in serious conditions, so that the hydrocarbon malodorous gas pollutants are generally concerned by people. Ammonia is one of the main malodorous atmospheric pollutants, mainly originating from agricultural emissions or from production processes containing urea or ammonia compounds. Ammonia gas has strong irritation to human body, and can destroy human skin, eyes, organ mucosa, etc. Ammonia can also be oxidized to nitrogen oxides, which can be harmful to the environment.
The traditional main technologies for removing harmful pollutants such as methyl mercaptan, formaldehyde, ammonia gas and the like include physical adsorption, an alkali liquor absorption oxidation method, biological deodorization and the like, but the traditional methods for removing harmful pollutants have certain limitations, and the solar photocatalytic method for removing pollutant gases has the advantages of mild conditions, simplicity in operation, capability of directly utilizing sunlight, no secondary pollution and the like, so that more and more attention is paid. Wherein the TiO is 2 Has the advantages of high photoactivity, low cost, low toxicity, good chemical and thermal stability and the like, and is the most widely researched photocatalyst at present. But TiO 2 2 The photocatalytic activity can be generated only under the condition of ultraviolet light, and only 5 percent of solar energy actually reaching the earth can be utilized, so that the photocatalytic activity can be generated by TiO 2 Surface introduction of noble metals to enhance TiO 2 The efficiency of removing harmful contaminants is a focus of research.
Disclosure of Invention
The invention aims to cure a platinum-loaded titanium dioxide composite photocatalyst on sheet-shaped flexible porous cellucotton and realize efficient and green degradation treatment on harmful pollutants such as methyl mercaptan, formaldehyde, ammonia gas and the like by using a lighting method. The method has the advantages of mild conditions, simple preparation of the catalytic material sheet, excellent treatment performance, and wide practical value and application and research prospects.
In order to realize the purpose, the invention is implemented by the following technical scheme:
synthesis of platinum-supported titanium dioxide composite photocatalyst and degradation of the material under the condition of illumination caused by methyl mercaptan, formaldehyde, ammonia gas and the likeA method for harmful pollution: the composite photocatalyst Pt/TiO 2 Solidifying on porous fiber carrier sheet, placing in purifier device containing ultraviolet lamp tube, and placing in 3m 3 Is arranged in the closed environment evaluation cabin. And (4) introducing the pollutants into the environment evaluation cabin after the environment evaluation cabin is at constant temperature and constant humidity, and then starting the purifier device to degrade the pollutants.
More specifically:
a synthesis of a platinum-loaded titanium dioxide composite photocatalyst and a method for degrading harmful pollutants such as methyl mercaptan, formaldehyde, ammonia gas and the like by using the material under the condition of illumination comprise the following specific steps:
(1) Composite photocatalyst Pt/TiO 2 Preparation of
Preparation of TiO by solution-gel method using isopropyl titanate as precursor 2 A photocatalyst. Firstly, measuring a certain amount of ethanol, and then adding a proper amount of isopropyl titanate to be marked as a solution A; deionized water, absolute ethyl alcohol and glacial acetic acid are mixed according to the volume ratio of 3:20:1 stirring and mixing to obtain a solution B. Continuously stirring the solution B in an ice-water bath, slowly dropping the solution A when the temperature of the solution in a beaker is reduced to 0 ℃, stirring until sol is formed, continuously stirring for 2h, drying the obtained gel for 8-12h in an oven at 80-100 ℃, grinding the dried sample into powder, and calcining in a muffle furnace at 300-500 ℃ for 6-8h in a clean air atmosphere at the heating rate of 2-5 ℃/min.
Weighing a small amount of TiO prepared by the steps 2 Sample and 1 to 5wt% of PtCl 4 Adding into a beaker, adding 100mL deionized water, and magnetically stirring for 8-12h. Then heating and stirring the mixture in a water bath kettle at 80 ℃ until the suspension is completely dried, and then drying the sample in a drying oven at 80-100 ℃ for 8-12h. Then grinding the dried solid sample into powder, calcining the powder in a muffle furnace at the temperature of between 300 and 500 ℃ for 6 to 8h at the heating rate of between 2 and 5 ℃/min to prepare the Pt/TiO 2 . Taking a small amount of prepared Pt/TiO 2 Placing the sample in a tube furnace, heating to a specified temperature (300 ℃, 400 ℃ and 500 ℃) in a hydrogen atmosphere, reducing for 2-3h, wherein the hydrogen flow rate is 20-40 mL/min, and the heating rate is 2-5 ℃/min, and obtaining the Pt-loaded defective TiO 2 Written as Pt/TiO 2 X, X represents the hydrogen reduction temperature.
(2) Curing composite photocatalyst Pt/TiO 2 Preparation of catalytic Material sheet
Taking a certain amount of composite photocatalyst Pt/TiO which passes through a 200-300 mesh sieve 2 Stirring with titanium glue solution in a certain proportion, soaking the flaky porous cellucotton with a certain size in the uniformly stirred suspension, and soaking and drying for multiple times. And (3) placing the soaked flexible porous cellucotton in a vacuum drying box, heating to 100-200 ℃ at the heating rate of 2-5 ℃/min, and drying for 6-8h. After natural cooling, the mixture is sealed and stored for use.
(3) Degradation of contaminants
The solidified catalytic material sheet was placed in a purifier device, and then the purifier device was placed 3m 3 The closed environment evaluation cabin in, treat environment evaluation cabin constant temperature and humidity back, let in a certain amount of pollutant in the cabin, open the evaluation under-deck agitator and with pollutant homogeneous mixing, observe the concentration of indoor pollutant through the detector, when the gaseous concentration of pollution in the evaluation under-deck is stable, open the clarifier device and degrade the pollutant.
(4) Reaction product detection
When the indication number of the detector in the evaluation cabin becomes zero, the purifier device is closed to stop reaction, the catalytic material sheet is taken out, and a certain amount of gas after reaction is sampled to analyze the gas components after reaction by using a gas chromatograph.
The invention has the advantages that:
1) The invention uses the composite photocatalyst Pt/TiO 2 The catalyst is efficient and stable, and is green and pollution-free;
2) The invention can completely remove various harmful pollutants in a short time;
3) The invention adopts full-wave band illumination, the reaction cost is low, and the reaction condition is simple and mild;
4) The catalytic material sheet has the advantages of simple manufacturing process, simple and easy operation method and wide application prospect.
Drawings
FIG. 1 shows Pt/TiO 2 -X-ray photocatalysisPerformance diagram of agent degradation methyl mercaptan;
FIG. 2 shows Pt/TiO 2 -400 persistence versus stability plot of the behaviour of catalytic materials to degrade methyl mercaptan;
FIG. 3 shows Pt/TiO 2 -400 catalytic material catalytic degradation formaldehyde activity profile;
FIG. 4 shows Pt/TiO 2 -400 catalytic material catalytic degradation ammonia activity profile;
FIG. 5 shows a composite photocatalyst Pt/TiO 2 Scanning Electron Microscope (SEM) images of (a);
FIG. 6 shows a composite photocatalyst Pt/TiO 2 An XRD pattern of (a);
FIG. 7 shows a composite photocatalyst Pt/TiO 2 UV-Vis absorption spectrum of (a);
FIG. 8 shows a composite photocatalyst Pt/TiO 2 Electron Paramagnetic Resonance (EPR) spectra of (a).
Detailed Description
The present invention is further illustrated by the following examples. The results are shown in FIG. 1.
Example 1
Composite photocatalyst Pt/TiO 2 The synthesis and the method for degrading the pollution caused by methyl mercaptan, formaldehyde, ammonia gas and the like under the condition of illumination of the material comprise the following specific steps:
preparation of TiO by solution-gel method using isopropyl titanate as precursor 2 A photocatalyst. Firstly, 100ml of ethanol is measured, and 5g of isopropyl titanate is added to be marked as a solution A; deionized water, absolute ethyl alcohol and glacial acetic acid are mixed according to the volume ratio of 3:20:1 stirring and mixing to obtain a solution B. And (3) continuously stirring the solution B in an ice-water bath, slowly dripping the solution A when the temperature of the solution in the beaker is reduced to 0 ℃, stirring until the solution A is formed, continuously stirring for 2h, drying the obtained gel in an oven at 80 ℃ for 12h, grinding the dried sample into powder, and calcining for 6 hours at 500 ℃ in a muffle furnace in a clean air atmosphere at the temperature rise rate of 2 ℃/min.
Weighing a small amount of TiO prepared by the steps 2 Sample and 3wt% PtCl 4 Adding into a beaker, adding 100ml deionized water, and magnetically stirring for 8h. Heating and stirring in 80 deg.C water bath until the suspension is completely dried, placing the sample at 80 deg.CAnd drying in a drying oven for 8h. Then grinding the dried solid sample into powder, putting the powder into a muffle furnace to calcine 6h at 500 ℃, and heating up at a rate of 2 ℃/min to prepare the Pt/TiO 2 . Taking a small amount of prepared Pt/TiO 2 Placing the sample in a tubular furnace, heating to 400 ℃ in a hydrogen atmosphere, reducing for 2h, wherein the hydrogen flow rate is 20 mL/min, and the heating rate is 2 ℃/min, and obtaining the Pt-loaded defective TiO 2 。
Weighing a certain mass of composite photocatalyst Pt/TiO 2 The mixture was placed in a beaker and added to a solution of 500 mL in titanium gel and stirred for 12h to form a suspension. And immersing the whole substrate material in the suspension by adopting an immersion method for 30min, taking out, draining, then placing in an oven at 80 ℃ for drying, taking out, and carrying out multiple immersion drying until the catalyst on the surface of the catalytic material reaches the required loading capacity. And finally, placing the catalytic material sheet in an air drying box, heating to 100 ℃ by a program, drying 6h, naturally cooling, and taking out to obtain the catalytic material sheet.
The solidified flaky flexible porous cellucotton is arranged between lamp tubes in a photocatalytic reactor in a parallel stacking mode, 3 ultraviolet lamp tubes with the wavelength of 254nm and the power of 8W are arranged in the reactor, and a shell and a reaction chamber are made of magnesium-aluminum alloy. The prepared photocatalytic reactor is placed on an operation platform frame with the height of 1 m in a closed environment evaluation cabin, the constant temperature and humidity function of the closed environment evaluation cabin is started, and the temperature and the humidity are kept constant at 25 ℃ (± 1 ℃) and 50% (± 2%) of the room temperature. And after the temperature and the humidity are stable, opening an air inlet valve of the closed environment evaluation cabin, and opening a standard pollutant steel cylinder pressure reducing valve. And stopping air inflow when the concentration of the pollutants reaches a set value of 10-10.5ppm, starting the photocatalytic reactor after the concentration shown by the detector is stable for 30min and does not change (< 5%), and starting a pollutant removal test.
When the reading of the detector is reduced to zero, the test data is recorded, the photocatalytic reactor is closed, and the pollutant removing process is finished. And (5) starting an air exhaust system of the closed evaluation cabin, fully replacing the atmosphere in the closed evaluation cabin, and finishing the test.
Example 2
The specific experimental procedure was substantially the same as in example 1 of this section, except that the photocatalysis was carried outPt/TiO agent 2 The temperature of the hydrogen reduction was 300 ℃.
Example 3
The specific experimental procedure is essentially the same as in example 1 of this section, except that the photocatalyst Pt/TiO is 2 The temperature of hydrogen reduction was 500 ℃.
Example 4
The specific experimental procedure is essentially the same as in example 1 of this section, except that the photocatalyst Pt/TiO is 2 No hydrogen reduction was performed.
The specific experimental method is basically the same as that of example 1 in this part, and is a repeated experiment.
As shown in FIG. 1, the degraded methyl mercaptan test was performed at a degradation concentration of about 10 ppm, pt/TiO 2 The best photocatalytic activity was shown for methyl mercaptan after reduction at 400 ℃. For initial concentrations of methyl mercaptan of around 10 ppm, tiO 2 The conversion rate of 89.5 percent can be achieved within 300 min, the degradation rate is 0.09 mL/min, and the Pt/TiO can achieve the conversion rate under the same condition 2 The degradation can be completed in only 150 min at 400 ℃ below zero, the degradation rate is 0.20 mL/min, the degradation rate is improved by 122%, and the conversion rate of methyl mercaptan can reach 99.9%.
As shown in figure 2, the methyl mercaptan can be degraded within about 170 min in the first cycle experiment, the degradation rate is 0.18 mL/min, and the degradation rate reaches 99.9%. After 10 cycles of experiments, the activity of the catalytic material is reduced to some extent, and the methyl mercaptan can be degraded within 270 min, wherein the degradation rate is 0.12 mL/min, and is reduced by 33.33%, but the degradation rate of the methyl mercaptan can reach 99.9%. The total time for 10 experiments was 2440 min, during which time 315.21 mL methyl mercaptan was purged with an average degradation rate of 0.14mL/min. Thus, the prepared Pt/TiO can be known 2 The photocatalytic material has excellent photocatalytic stability and durability with respect to methyl mercaptan.
As shown in FIG. 3, tiO was added to formaldehyde at an initial concentration of 8 ppm 2 The photocatalysis takes 430 min to complete the degradation, the degradation rate is 0.056 mL/min, and the Pt/TiO degradation rate is 2 The-400 photocatalyst can be degraded in 180 min, the degradation rate is 0.134 mL/min, the degradation rate is improved by 139.3 percent, and the formaldehyde is treatedThe degradation rate of the catalyst reaches 99.9 percent. The experimental results show that Pt/TiO 2 400 photo-catalysis can remove formaldehyde well.
As shown in FIG. 4, tiO was present at an initial concentration of 60 ppm ammonia 2 The photocatalyst is degraded in 82 min, the degradation rate is 2.20 mL/min, pt/TiO 2 The-400 photocatalyst can be degraded in 44 min, the degradation rate is 4.09 mL/min, and the degradation rate of the photocatalyst on ammonia gas can reach more than 99.9%. The experimental results show that Pt/TiO 2 400 also has good photocatalysis effect on ammonia gas.
As shown in FIG. 5, pt/TiO can be seen 2 400 catalyst is irregular spherical particle, pt in TiO 2 The load was successful on the surface.
As shown in FIG. 6, pt/TiO 2 TiO in-X 2 Mainly anatase phase, accompanied by H 2 Increase in reduction temperature, rutile phase TiO 2 The characteristic diffraction peak of (A) is more and more obvious, which is illustrated in H 2 TiO in reduction process 2 There is a phase transition from the anatase phase to the rutile phase.
As shown in FIG. 7, H 2 Reduced Pt/TiO 2 X to Pt/TiO 2 Showing a stronger visible light absorption response. It can be concluded that Pt/TiO 2 The synergistic effect exists between X and Pt, and Pt/TiO is enhanced 2 The light absorption capacity of the X catalyst, which facilitates the activation of the contaminant molecules under light irradiation.
As shown in FIG. 8, intrinsic TiO 2 No peak of V0 signal was detected, but at H 2 Pt/TiO calcined in atmosphere high-temperature environment 2 The X material shows a distinct V0 signal peak at g =2.003, which is an absorption peak generated by binding one electron to V0 on the catalyst surface, and the signal peak intensity at g =2.003 gradually increases with increasing reduction temperature, indicating that the concentration of V0 increases. The above results are shown in Pt/TiO 2 Oxygen vacancy defects are generated in the X material and the concentration thereof increases with the increase of the reduction temperature.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (9)
1. A preparation method of a platinum-loaded titanium dioxide composite photocatalyst is characterized by comprising the following steps: the method comprises the following steps:
（1）TiO 2 the preparation of (1): mixing ethanol and isopropyl titanate to obtain a solution A, and mixing deionized water, absolute ethanol and glacial acetic acid according to a volume ratio of 3:20:1 stirring and mixing to obtain a solution B, slowly dripping the solution A into the solution B under the ice bath condition, continuously stirring until sol is formed, drying, grinding and calcining to obtain TiO 2 A powder;
（2）Pt/TiO 2 preparing a composite photocatalyst: mixing the TiO obtained in the step (1) 2 Powder, ptCl 4 Mixing with deionized water, stirring, heating in 80 deg.C water bath, stirring until the suspension is completely dried, drying at 80-100 deg.C for 8-12h, and grinding into powder; then calcining 6-8h at 300-500 ℃, with the heating rate of 2-5 ℃/min to prepare the Pt/TiO 2 Finally, reducing the Pt in a hydrogen atmosphere to obtain Pt-loaded defect state Pt/TiO 2 Namely a platinum-loaded titanium dioxide composite photocatalyst.
2. The preparation method of the platinum-supported titanium dioxide composite photocatalyst as claimed in claim 1, wherein the preparation method comprises the following steps: ptCl in step (2) 4 With TiO 2 The mass ratio of (A) is 1~5%.
3. The method for preparing the platinum-supported titanium dioxide composite photocatalyst as claimed in claim 1, wherein the method comprises the following steps: the calcination in the step (1) is specifically as follows: calcining at 300-500 deg.C for 6-8 hr at a heating rate of 2-5 deg.C/min.
4. The preparation method of the platinum-supported titanium dioxide composite photocatalyst as claimed in claim 1, wherein the preparation method comprises the following steps: the temperature of reduction in the step (2) is 300-500 ℃, the hydrogen flow rate is 20-40 mL/min, and the heating rate is 2-5 ℃/min.
5. A platinum-supported titanium dioxide composite photocatalyst produced by the production method as described in any one of claims 1 to 4.
6. Use of the platinum-supported titanium dioxide composite photocatalyst as defined in claim 5, wherein: the platinum-loaded titanium dioxide composite photocatalyst is solidified on the flaky flexible porous cellucotton, and methyl mercaptan, formaldehyde and ammonia gas harmful pollutants are degraded under the irradiation of light.
7. Use according to claim 6, characterized in that: the method for curing the platinum-loaded titanium dioxide composite photocatalyst on the flaky flexible porous cellucotton comprises the following specific steps: mixing and stirring the platinum-loaded titanium dioxide composite photocatalyst and a titanium glue solution uniformly to obtain a suspension, then soaking the flaky flexible porous fiber cotton in the suspension, draining, heating to 100-200 ℃ at a heating rate of 2-5 ℃/min, and drying for 6-8h.
8. Use according to claim 7, characterized in that: the titanium glue solution is used as an adhesive, and the mass ratio of the titanium glue solution to the platinum-supported titanium dioxide composite photocatalyst is 100:1.
9. use according to claim 6, characterized in that: the wavelength of the light source for illumination is a full waveband.
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