CN113856717B - Super-stable photocatalytic material accelerator and preparation method thereof - Google Patents

Super-stable photocatalytic material accelerator and preparation method thereof Download PDF

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CN113856717B
CN113856717B CN202111177469.9A CN202111177469A CN113856717B CN 113856717 B CN113856717 B CN 113856717B CN 202111177469 A CN202111177469 A CN 202111177469A CN 113856717 B CN113856717 B CN 113856717B
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photocatalytic
accelerator
solution
promoter
photocatalytic material
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CN113856717A (en
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乔秀清
王紫昭
胡杰杰
侯东芳
李东升
兰亚乾
张其春
刘彬
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China Three Gorges University CTGU
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/20—Carbon compounds
    • B01J27/22—Carbides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/04—Sulfides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24—Nitrogen compounds
    • B01J35/23—
    • B01J35/39—
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • C01B3/042—Decomposition of water
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C02F2101/22—Chromium or chromium compounds, e.g. chromates
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/36—Organic compounds containing halogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/10—Photocatalysts
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention discloses a super-stable photocatalytic material accelerator and a preparation method thereof, belonging to the fields of nano material preparation and photocatalysis. The accelerator is formed by embedding nano cocatalyst on a charge transport body, wherein the nano cocatalyst material contains symbiotic MoO 2 And Mo (Mo) 2 The two components are connected through tight interface contact, and the charge carrier is a C material with good conductivity, so that charges can be rapidly transmitted from the photocatalytic material main body to the cocatalyst electron collector. The accelerator is used for modifying the photocatalytic material, and can obviously improve the photocatalytic activity and stability of the material. More importantly, the accelerator has higher stability, and can still maintain the original structural stability and chemical activity after being stored in the air for 2 years. The accelerator provides a brand new strategy for the practical application of the photocatalytic material.

Description

Super-stable photocatalytic material accelerator and preparation method thereof
Technical Field
The invention relates to a preparation method and application of a super-stable photocatalytic material accelerator, and belongs to the field of material preparation and photocatalytic materials.
Background
With the development of economy, human beings face two major challenges of energy shortage and environmental pollution. One relatively promising technique to solve these two problems is the photocatalytic technique. The photocatalysis technology can utilize photocatalysis material to absorb solar energy rich in the earth, thoroughly degrade toxic and harmful pollutants in the environment or decompose the toxic and harmful pollutants in the environment to generate clean energy H 2 Is a green pollution-free technology. However, the actual use of the existing photocatalysis technology is still in the sprouting stage, and the main reasons are that the efficiency of the photocatalysis material is low, the utilization rate of sunlight is not high, the stability of the photocatalysis material is poor, the durability of the material is not enough, and the like, so that the actual application of the photocatalysis technology is limited. Therefore, the photocatalytic material is modified, and the efficiency and stability of the photocatalytic material are further improved, so that the method has important significance for promoting the application of the photocatalytic technology.
Among the photocatalytic materials available today, cdS is the most popular one for visible light response. CdS material has proper energy band structure and oxidation-reduction potential, and can absorb visible light and H + Reduction to H 2 Is the most potential semiconductor material. But the recombination rate of photo-generated electrons and holes in the CdS material is faster, and S 2- Is easily oxidized into simple substance S under the action of photo-generated holes, thereby destroying the structure of the material and having poor stability. CdS has low photocatalytic activity and is easily corroded. At present, the loading of noble metal Pt on the CdS surface is an effective mode for improving the photocatalytic activity. However, pt reserves on earth are scarce and expensive, and there is a need to prepare economical promoters for improving the photocatalytic activity of CdS.
Disclosure of Invention
The invention aims at the defects and provides a novel, efficient, stable and low-cost photocatalysis promoter, and a preparation method and application thereof.
A super-stable photocatalytic material accelerator is formed by uniformly embedding non-noble metal oxide/carbide active nano cocatalysts on a charge transport body, wherein the active cocatalysis is formed by closely contacting two symbiotic active species, and a conductive carrier is generated in situ and has strong interface contact and electronic interaction with the active cocatalyts.
A super-stable photocatalytic material accelerator is composed of non-noble metal oxide/carbide active nano promoter uniformly inlaid on a charge transport body, wherein the active nano promoter contains in-situ generated MoO 2 And Mo (Mo) 2 And C active species of two different components, wherein the two components have an interface structure of close contact, and the charge transporter is a C material with good conductivity.
The accelerator is prepared by adopting an in-situ thermal decomposition method, and Mo 2 C is in situ carbonized MoO 2 The heterogeneous structure of two components is obtained by controlling the carbonization degree, and the charge transporter C material is prepared by in-situ thermal decomposition of a precursor and has strong interface contact and electronic interaction with an active cocatalyst.
Said MoO 2 Said MoO 2 And Mo (Mo) 2 The mass fraction of C is 80-90%, and the MoO is formed by 2 And Mo (Mo) 2 The molar ratio of C is 10:1-5:1.
The preparation method of the super-stable photocatalytic material accelerator adopts an in-situ thermal decomposition method and comprises the following steps:
(1) Mixing an aminobenzene solution with the concentration of 0.5-1.2 mol/L with a hydrochloric acid solution with the concentration of 0.8-1.2 mol/L to obtain an aniline hydrochloride solution with the pH of 3-4, and then mixing the prepared aniline hydrochloride solution according to the molar ratio of the aminobenzene to the ammonium heptamolybdate of 20: dropwise adding the mixture into an aqueous solution of ammonium heptamolybdate with the concentration of 0.02-0.1 mmol/L at the ratio of 1-15:1, and stirring the obtained mixed solution in a water bath at the temperature of 40-70 ℃ for 4-12 h to obtain a white precipitate.
(2) And drying the obtained white precipitate in vacuum for 8-14 h, and then carrying out high-temperature in-situ thermal decomposition for 1-5 h at 720-800 ℃ in nitrogen atmosphere to obtain the photocatalytic material promoter.
The super stable photocatalytic material promoter has the structure and morphology maintained in the original state after being set in air for 2 years.
The invention also provides an application of the photocatalytic material promoter in promoting photocatalytic agent to decompose water into hydrogen and degrade toxic pollutants.
The super stable photocatalytic material promoter is mixed with CdS, tiO in the presence of alcohol solvent 2 ，C 3 N 4 ，ZnIn 2 S 4 The photocatalytic materials are mixed (ball-milled or ultrasonic) and the photocatalytic hydrogen production activity and stability can be obviously improved.
The photocatalyst comprises CdS and TiO 2 、C 3 N 4 、ZnIn 2 S 4 Any one of the following.
The addition amount of the photocatalytic material accelerator is 20-40wt% relative to the mass of the photocatalyst.
The toxic pollutants comprise one or more of heavy metal cations, organic dyes, rhodamine B, polychlorinated biphenyl and nitenpyram.
Compared with the existing photocatalysis promoting agent, the photocatalysis promoting agent prepared by the invention has the beneficial effects that:
the photocatalytic material promoter is formed by embedding a non-noble metal promoter active material on a charge transport body, wherein the active promoter material contains symbiotic MoO 2 And Mo (Mo) 2 C species of two different components, the two components being generated by in situ carbonization and thus having an interface structure of intimate contact; the charge transporter is a C material with good conductivity. The in situ thermal decomposition of the charge transport ensures intimate contact between the promoter material and the derivatized C material. Meanwhile, the C material can serve as a carrier to improve the dispersibility of the cocatalyst material and the main catalyst material, so that more active sites are exposed, and the material is beneficial to the transmission of substances. Thus, the synergistic effect of the various advantages ensures the improvement of the activity and stability of the photocatalytic material.
Drawings
Fig. 1: SEM image of the photocatalytic material promoter prepared in example 1.
Fig. 2: a TEM image of the photocatalytic material promoter prepared in example 1.
Fig. 3: a photo-catalytic hydrogen-generating activity profile for the photo-catalytic composite of example 3.
Fig. 4: the results of the photocatalytic hydrogen production stability of the photocatalytic composite material according to example 3.
Fig. 5: SEM images of the photocatalytic composite material prepared in example 4.
Fig. 6: SEM images of samples of the photocatalytic composite material prepared in example 4 after 29 cycles.
Fig. 7: TEM pictures of the photocatalytic material prepared in example 1 after 2 years of standing.
Fig. 8: the photocatalytic material prepared in example 5 promotes the photocatalytic hydrogen production activity enhancing effect of the body on P25.
Detailed Description
The present invention is further illustrated below in conjunction with specific embodiments, it being understood that these embodiments are meant to be illustrative of the invention only and not limiting the scope of the invention, and that modifications of the invention, which are equivalent to those skilled in the art to which the invention pertains, will fall within the scope of the invention as defined in the claims appended hereto.
Example 1
A preparation method of a super-stable photocatalytic material accelerator comprises the following steps:
(1) Preparing 36 mmol of aminobenzene into 0.9 mol/L solution, adding 1 mol/L hydrochloric acid solution, stirring to obtain aniline hydrochloride solution with pH of 4, dropwise adding the prepared aniline hydrochloride solution into 0.05 mmo/L ammonium heptamolybdate aqueous solution, stirring, and stirring the obtained mixed solution in a water bath at 50 ℃ for 6 h to obtain white precipitate;
(2) The obtained white precipitate was dried in vacuo for 12 hours, and then subjected to high-temperature in-situ thermal decomposition at 775 ℃ for 2 hours in a nitrogen atmosphere to obtain a photocatalytic material promoter.
The scanning electron microscope image of the prepared photocatalytic material accelerator is shown in figure 1, and the accelerator is formed by dispersing and distributing nano particles on a matrix. XRD diffraction pattern and XPS analysis confirm that the prepared accelerator is prepared from MoO 2 /Mo 2 And C, the active cocatalyst is dispersed and inlaid on the C material. TEM images are shown in FIG. 2, and the structure of the nanoparticle and the C matrix can be clearly seen.
Example 2
A preparation method of a super-stable photocatalytic material accelerator comprises the following steps:
(1) Preparing 36 mmol of aminobenzene into 0.9 mol/L solution, adding 1 mol/L hydrochloric acid solution, stirring to obtain aniline hydrochloride solution with pH of 4, dropwise adding the prepared aniline hydrochloride solution into 0.08 mmo/L ammonium heptamolybdate aqueous solution, stirring, and stirring the obtained mixed solution in a water bath at 40 ℃ for 6 h to obtain white precipitate;
(2) The obtained white precipitate was dried in vacuo for 12 hours, and then subjected to high-temperature in-situ thermal decomposition at 750 ℃ for 2 hours in a nitrogen atmosphere to obtain a photocatalytic material promoter.
Example 3
The super-stable photocatalytic material accelerator prepared in the embodiment 1 is mixed with the CdS photocatalytic material prepared in advance according to the mass percentage of 20-40%. The preparation process of CdS comprises the following steps: 16.2 48.6 mmol of thiourea of the tetrahydrate cadmium nitrate is dissolved in 80ml of ethylenediamine and is vigorously stirred to obtain a transparent light green solution, 40ml of the solution is placed in a reaction kettle to react for 24 hours at 160 ℃ to finally obtain a light yellow CdS photocatalytic material. 100mg of CdS photocatalytic material, 20mg,25mg,30mg,35mg and 40mg of accelerator are respectively dispersed in 50ml of methanol solution by ultrasonic, and the composite material is obtained by ultrasonic for 30 min. 30mg of the compounded material is placed in a reaction vessel, 8ml of lactic acid and 80ml of aqueous solution are added into the reaction vessel, and the photocatalysis hydrogen production test is carried out under a xenon lamp light source provided with a 420nm optical filter. The hydrogen production performance is shown in figure 3. As can be seen, when the mass of the accelerator is different, the photocatalytic hydrogen production activity is different, and when the mass percentage of the accelerator is 30%, the photocatalytic hydrogen production activity of the composite material is 18.43 mmol/h * g, 5 times more than pure CdS. SEM (scanning electron microscope) pictures of the composite material with the mass percentage of 30% are shown in FIG. 4, and it can be seen that CdS nanorods and promotion body nanoparticles are evenly distributedIs distributed on the C matrix. The photocatalytic hydrogen production activity cycle test of the composite material shows that the catalyst can obviously improve the stability of CdS, the hydrogen production activity of pure CdS is only 45% of that of the initial state after 6 cycles, and the activity of CdS modified by the catalyst still remains 100% after 29 cycles (figure 5), and the morphology of the composite material is not obviously changed (figure 6).
Example 4
The photocatalytic material acceleration body prepared in example 1 was tested after being left for 2 years, and a TEM image (fig. 7) shows that the acceleration body still maintains an initial structure and morphology after being left for a long time. The placed accelerator and the prepared CdS photocatalytic material are subjected to ultrasonic compounding, the steps are the same as those reported in the example 3, the mass percent of the accelerator is 30%, the photocatalytic hydrogen production activity test is the same as that of the step 3, the photocatalytic hydrogen production activity of the composite material is basically the same as that of the composite material which is just prepared, the high activity can still be maintained, and the stability of the material can still be circulated for 29 cycles.
Example 5
The super stable photocatalytic material promoter prepared in example 2 was ball-milled and mixed with commercial P25 photocatalytic material in the presence of ethanol in the same manner as in example 4. When the mass percentage of the accelerator is 20 percent wt percent, tiO 2 The photocatalytic activity of the photocatalytic material under the full spectrum is improved by nearly 20 times (figure 8), the long-term stability of the photocatalytic material is obviously improved, and the pure TiO is prepared 2 The hydrogen-generating activity after 6 cycles is only 82% of the initial state, and the TiO modified by the accelerator 2 The activity remained 100% after 30 cycles.
Example 6
The super stable photocatalytic material accelerator prepared in example 2 is mixed with C 3 N 4 The procedure of example 4 was followed by ultrasonic intermixing of the photocatalytic material in the presence of ethanol. Wherein C is 3 N 4 The synthesis method of (2) is as follows: weighing 1g of dicyandiamide, placing the dicyandiamide in a muffle furnace, capping at 550 ℃ and calcining for 2 hours, and heating at a rate of 5 ℃/min to obtain C 3 N 4 Photocatalytic material. When the mass percentage of the accelerator isC at 30 wt% 3 N 4 The visible light photocatalysis hydrogen production activity of the photocatalysis material is improved by about 10 times, and the long-term stability of the photocatalysis material is obviously improved.
Example 7
The super stable photocatalytic material accelerator prepared in the example 2 and ZnIn 2 S 4 The photocatalytic materials are ultrasonically intermixed in the presence of ethanol. The procedure is as in example 4. Wherein ZnIn 2 S 4 The synthesis method of (2) is as follows: taking 2ml of prepared ZnCl2 solution with the concentration of 0.5M, 4ml of InCl3 solution with the concentration of 0.5M, mixing the solution with 14ml of ethanol solution, adding 0.3g of thioacetamide, uniformly mixing, and then placing the mixture in a reaction kettle for reacting for 12 hours at 120 ℃ to obtain ZnIn 2 S 4 Photocatalytic material. Dispersing 20mg of the composite material with the accelerator mass percentage of 25% in 50mL of potassium dichromate solution with the concentration of 20mg/L, and detecting the concentration of the potassium dichromate solution by an ultraviolet spectrophotometer, wherein ZnIn 2 S 4 The degradation rate of the photocatalytic material to hexavalent Cr reaches 40% in 40 minutes, the composite material can completely reduce Cr in 40 minutes, and the efficiency of the composite photocatalytic material does not change obviously after the composite photocatalytic material is used for 10 times.

Claims (7)

1. The application of a photocatalytic material promoter in promoting photocatalytic agent to perform photocatalytic decomposition of water to prepare hydrogen and photocatalytic degradation of toxic pollutants is disclosed, wherein the promoter is formed by uniformly embedding non-noble metal oxide/carbide active nano promoter on a charge transport body, and the active nano promoter contains in-situ generated MoO 2 And Mo (Mo) 2 C two active species with different components, wherein the two components have an interface structure of close contact, the charge transporter is a C material with good conductivity, and the MoO 2 And Mo (Mo) 2 The mass fraction of C is 80-90%, and the MoO is formed by 2 And Mo (Mo) 2 The molar ratio of C is 10:1-5:1, and the photocatalyst comprises CdS and TiO 2 、C 3 N 4 、ZnIn 2 S 4 Any one of the following.
2. Use according to claim 1, characterized in that the photocatalytic material promoter is added in an amount of 20-40% by weight relative to the mass of the photocatalyst.
3. The use according to claim 1, wherein the toxic contaminants comprise one or more of heavy metal cations, organic dyes, polychlorinated biphenyls, nitenpyram.
4. The use according to claim 1, characterized in that the preparation method of the photocatalytic material promoter comprises the following steps:
(1) Mixing a certain amount of aminobenzene solution with hydrochloric acid solution to obtain aniline hydrochloride solution, then dropwise adding the prepared aniline hydrochloride solution into aqueous solution of ammonium heptamolybdate, and stirring for a period of time to obtain white precipitate;
(2) The obtained white precipitate is dried in vacuum, and then is subjected to high-temperature in-situ thermal decomposition in inert atmosphere to obtain the photocatalytic material promoter.
5. The use according to claim 4, wherein the concentration of the aminobenzene solution is 0.5-1.2 mol/L, the concentration of the hydrochloric acid solution is 0.8-1.2 mol/L, the pH of the prepared aniline hydrochloride solution is 3-4, and the concentration of the ammonium heptamolybdate solution is 0.02-0.1 mmol/L.
6. The use according to claim 4, wherein the molar ratio of aminobenzene to ammonium heptamolybdate is 20: 1-15:1, wherein the temperature of water bath stirring is 40-70 ℃, and the stirring time is 4-12 h.
7. The use according to claim 4, wherein the white precipitate in step 2 is dried in vacuum for 8-14 hours at a high temperature in situ thermal decomposition temperature of 720-800 ℃; the thermal decomposition time is 1-5 h, and the inert atmosphere is nitrogen.
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