CN115739118A - Iron-doped bismuth oxysulfide photocatalyst and preparation method and application thereof - Google Patents
Iron-doped bismuth oxysulfide photocatalyst and preparation method and application thereof 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
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Abstract
The invention discloses an iron-doped bismuth oxysulfide photocatalyst and a preparation method and application thereof, and belongs to the technical field of novel environmental catalytic materials. The invention mainly uses Bi 2 O 2 S crystal and Fe (NO) 3 ) 3 ·9H 2 Preparing an iron-doped bismuth oxysulfide photocatalyst by using O as a raw material and adopting a high-energy ball milling method; wherein the doping amount of Fe in the Fe-doped bismuth oxysulfide photocatalyst is 1.7-5.6%. The iron-doped bismuth oxysulfide photocatalyst obtained by the method has high transmission efficiency of photon-generated carriers, abundant reaction active sites and strong capacity of activating persulfate.
Description
Technical Field
The invention belongs to the technical field of new environmental catalysis materials, and particularly relates to an iron-doped bismuth oxysulfide photocatalyst as well as a preparation method and application thereof.
Background
The growing accumulation of a large number of antibiotics in the world through domestic, hospital, pharmaceutical companies, wastewater treatment plants and the discharge of aquaculture and livestock farms has prompted the formation of Antibiotic Resistance Genes (ARG) and Antibiotic Resistant Bacteria (ARB) in aquatic ecosystems, threatening public health. Tetracycline (TC), a typical antibiotic, has adverse effects on human health and ecosystem due to its chemical stability and environmental persistence. Moreover, the antimicrobial properties of tetracycline make it difficult to eradicate it by traditional biological wastewater treatment techniques. Therefore, there is an urgent need to develop an economical and effective method for treating antibiotic wastewater.
In recent years, advanced oxidation technology has been widely used to degrade refractory organic pollutants and mineralize them into CO 2 And H 2 And O. Based on hydroxyl radicals (. OH) and sulfate radicals (SO) 4 - The advanced oxidation technology of) is an effective method for degrading common organic pollutants, such as organic dyes, surfactants, hydrocarbons, phenols, pharmaceutically active ingredients, pesticides and the like. However, advanced OH-based oxidation technologies degrade organic pollutants by non-selective multi-step reactions, often requiring an acidic environment. Based on SO 4 - The advanced oxidation technology of (1) has a more stable reaction process, fewer restrictions and a faster reaction rate than the advanced oxidation technology based On (OH), and has been rapidly developed in recent years, and has been increasingly used in sewage treatment.
Currently, many metal ion and heterogeneous catalysts are used for SO-based catalysts 4 - In the advanced oxidation technology, especially the heterogeneous photocatalyst has larger application potential in the aspect of photocatalytic activation of persulfate to degrade pollutants. In addition, the transition metal is doped into the photocatalyst, so that the catalytic activity of the photocatalyst can be obviously improved, and the aim of efficiently activating persulfate to degrade pollutants is fulfilled. However, the transition metal doping is usually prepared by a hydrothermal method or a solvothermal method, which takes a long time, may cause secondary contamination, and the sample cannot be prepared in large quantities.
Disclosure of Invention
In view of the above, the present invention provides an iron-doped bismuth oxysulfide photocatalyst, and a preparation method and an application thereof, so as to overcome the defects in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
iron-doped bismuth oxysulfide photocatalystWith Bi 2 O 2 S crystal and Fe (NO) 3 ) 3 ·9H 2 Preparing an iron-doped bismuth oxysulfide photocatalyst by using O as a raw material and adopting a high-energy ball milling method; wherein the doping amount of Fe in the Fe-doped bismuth oxysulfide photocatalyst is 1.7-5.6%.
Further, said Bi 2 O 2 The grain size of the S crystal is a nano sheet structure.
The invention also provides a preparation method of the iron-doped bismuth oxysulfide photocatalyst, which comprises the following steps:
with Bi 2 O 2 S crystal and Fe (NO) 3 ) 3 ·9H 2 O is used as a raw material, and a high-energy ball milling method is adopted to prepare the iron-doped bismuth oxysulfide photocatalyst, wherein Bi is 2 O 2 S crystal and Fe (NO) 3 ) 3 ·9H 2 The mass ratio of O is 0.5: (0.0625-0.2142).
Furthermore, in the ball milling process, the ball milling transport strength is 800rpm, and the ball milling time is 20min.
Further, the ball-milled sample was added to water at room temperature and stirred to remove excess iron salt, and then dried.
Further, the stirring time was 120min.
The invention also provides application of the iron-doped bismuth oxysulfide photocatalyst in treating waste water containing organic matters by photocatalytic activation of persulfate.
Further, the organic substance is tetracycline.
Compared with the prior art, the invention has the beneficial effects that:
1) The preparation of the iron-doped bismuth oxysulfide photocatalyst adopts a high-energy ball milling method, and has the advantages of relatively simple operation, safety, low cost, large-scale preparation and the like;
2) The obtained iron-doped bismuth oxysulfide photocatalyst has higher transmission efficiency of photon-generated carriers, abundant reaction active sites and stronger capacity of activating persulfate, and the reason is that the energy band structure of the bismuth oxysulfide photocatalyst is changed and generates new energy level by iron doping, so that the separation of the photon-generated carriers can be promoted; the surface of the ground bismuth oxygen-sulfur photocatalyst can expose more reaction active sites, thereby being beneficial to the activation of persulfate;
3) The obtained iron-doped bismuth oxysulfide photocatalyst shows excellent activity and stability for photocatalytic activation of persulfate to degrade tetracycline.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is an X-ray diffraction pattern of an iron-doped bismuth oxysulfide photocatalyst prepared in examples 1-3 of the present invention and a catalyst prepared in a control group;
FIG. 2 is a diagram showing the effect of photocatalytic activation of persulfate to degrade tetracycline in the Fe-doped Bi-O-S photocatalyst prepared in examples 1-3 of the present invention and in the catalyst prepared in the control;
FIG. 3 is a TEM image of an iron-doped bismuth oxysulfide photocatalyst prepared in example 2 of the present invention;
FIG. 4 is an XRD diagram before and after the photocatalytic reaction of the Fe-doped Bi-O-S photocatalyst prepared in example 2 of the present invention;
FIG. 5 is a graph showing the effect of the iron-doped bismuth oxysulfide photocatalysts prepared in the examples 2, 1 and 2 of the invention on degrading tetracycline by activating persulfate photocatalytically.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but rather as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated herein by reference to disclose and describe the methods and/or materials in connection with which the documents are cited. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The "room temperature" in the present invention is, unless otherwise specified, 25. + -. 2 ℃ inclusive.
Fe (NO) as raw material for the present invention 3 ) 3 ·9H 2 O (analytically pure) was purchased from the national drug group;
an Fe-doped Bi-O-S photocatalyst is prepared from Bi 2 O 2 S crystal and Fe (NO) 3 ) 3 ·9H 2 Preparing an iron-doped bismuth oxysulfide photocatalyst by using O as a raw material and adopting a high-energy ball milling method; wherein the doping amount of Fe in the Fe-doped bismuth oxysulfide photocatalyst is 1.7-5.6%.
In some preferred embodiments, the Bi 2 O 2 The S crystal is of a nano flaky structure.
The invention also provides a preparation method of the iron-doped bismuth oxysulfide photocatalyst, which comprises the following steps:
with Bi 2 O 2 S crystal and Fe (NO) 3 ) 3 ·9H 2 O is used as a raw material, and a high-energy ball milling method is adopted to prepare the iron-doped bismuth oxysulfide photocatalyst, wherein Bi is 2 O 2 The mass of the S crystal is 0.5g; fe (NO) 3 ) 3 ·9H 2 The O mass is 0.0625-0.2142g, more preferably 0.0625g, 0.125g, 0.2142g.
In some preferred embodiments, the ball milling transport intensity is 800rpm and the ball milling time is 20min during the ball milling process.
In some preferred embodiments, the ball-milled sample is added to water at room temperature, stirred, and dried.
In some preferred embodiments, the stirring time is 120min.
The invention also provides application of the iron-doped bismuth oxysulfide photocatalyst in activating persulfate to degrade tetracycline under simulated solar illumination.
Example 1
A preparation method of an iron-doped bismuth oxysulfide photocatalyst comprises the following steps:
1) 0.5g of Bi is weighed 2 O 2 S crystal, 0.0625g of Fe (NO) 3 ) 3 ·9H 2 Adding O into a ball milling tank, and grinding for 20min in a ball mill with the working strength of 800rpm to obtain a ball-milled sample;
2) Adding the ball-milled sample into 250mL of water at room temperature, stirring for 120min, washing with water and drying to obtain the iron-doped bismuth oxysulfide photocatalyst, mark 1.7% Fe/BiOS.
Example 2
A preparation method of an iron-doped bismuth oxysulfide photocatalyst comprises the following steps:
1) 0.5g of Bi is weighed 2 O 2 S crystal, 0.125g of Fe (NO) 3 ) 3 ·9H 2 Adding O into a ball milling tank, and grinding for 20min in a ball mill with the working strength of 800rpm to obtain a ball-milled sample;
2) Adding the ball-milled sample into 250mL of water at room temperature, stirring for 120min, washing with water and drying to obtain the iron-doped bismuth oxysulfide photocatalyst, mark 3.3% Fe/BiOS.
Example 3
A preparation method of an iron-doped bismuth oxysulfide photocatalyst comprises the following steps:
1) 0.5g of Bi are weighed 2 O 2 S crystal, 0.2412g of Fe (NO) 3 ) 3 ·9H 2 Adding O into a ball milling tank, and grinding for 20min in a ball mill with the working strength of 800rpm to obtain a ball-milled sample;
2) Adding the ball-milled sample into 250mL of water at room temperature, stirring for 120min, washing with water and drying to obtain the iron-doped bismuth oxysulfide photocatalyst, mark 5.6% Fe/BiOS.
Control group 1
A preparation method of an iron-doped bismuth oxysulfide photocatalyst comprises the following steps:
Bi 2 O 2 preparation of S crystal: 1.9403g of Bi (NO) 3 ) 3 ·5H 2 O was added to 60mL of deionized water, stirred well, and 0.1522g of SC (NH) was added thereto 2 ) 2 Stirring is continued for 10min, then 12g of LiOH & H are added 2 Slowly adding O into the mixed solution, and continuously stirring for 60min to form a brownish black mixed solution; the stirred homogeneous mixture was transferred to a 80mL PPL lined autoclave. The autoclave was placed in a forced air drying oven and heated to 200 ℃ and maintained at this temperature for 72h. After the autoclave was cooled to room temperature, the remaining sample was collected and washed several times with deionized water. Finally, the washed sample was dried in a vacuum oven at 60 ℃ for 12h. Collecting the dried sample to obtain Bi 2 O 2 S sample (labeled as BiOS).
FIG. 1 is an X-ray diffraction pattern of iron-doped bismuth oxysulfide photocatalysts prepared in examples 1-3 of the present invention and a catalyst prepared in a control group. As can be seen from the figure, 1.7% of Fe/BiOS prepared in example 1, XRD diffraction peak position and Bi 2 O 2 The standard peak positions of S (PDF # 34-1493) are corresponding to each other, which shows that Bi in the doped photocatalyst 2 O 2 S phase is not changedAnd no other impurities are generated; 3.3% of Fe/BiOS prepared in example 2 XRD diffraction peak position and Bi 2 O 2 The standard peak position of S (PDF # 34-1493) corresponds to that of Bi in the doped photocatalyst 2 O 2 The S phase is not changed, and other impurities are not generated; 5.6% of Fe/BiOS XRD diffraction peak position and Bi prepared in example 3 2 O 2 The standard peak position of S (PDF # 34-1493) corresponds to that of Bi in the doped photocatalyst 2 O 2 The S phase is not changed, and other impurities are not generated.
Application example 1
The iron-doped bismuth oxysulfide photocatalyst prepared in examples 1 to 3 and the catalyst prepared in the control group 1 were subjected to a performance test of photocatalytic activation of persulfate to degrade tetracycline, and the specific method was as follows:
0.05g of the iron-doped bismuth oxysulfide photocatalyst prepared in examples 1-3 and the catalyst prepared in control 1 were weighed into 100mL of a tetracycline solution with a concentration of 30mg/L, stirred in the shade for 0.5h to uniformly mix the catalyst and the contaminants and achieve adsorption balance, 5mL of the solution was taken out into a centrifuge tube, and 1mL of methanol was added. Then, 0.03g of persulfate (potassium persulfate is used in the experiment) is rapidly added into the beaker, a xenon lamp (300W) is turned on to perform a light reaction for 30min, 5mL of solution is taken into a centrifuge tube every 5min, and 1mL of methanol is added. And (3) measuring the absorbance of the tetracycline at the 357nm maximum absorption wavelength of the tetracycline by using a spectrophotometer, and analyzing the change of the tetracycline concentration according to the test result, thereby calculating the degradation effect of the photocatalyst on the tetracycline.
FIG. 2 is a graph showing the effect of the iron-doped bismuth oxysulfide photocatalyst prepared in examples 1 to 3 of the present invention on the degradation of tetracycline by photocatalytic activation of persulfate with the catalysts prepared in the control group. As can be seen from FIG. 2, the 1.7% Fe/BiOS catalyst prepared in example 1 was found to degrade 83% of tetracycline in the test of degrading tetracycline by photocatalytically activating persulfate; 3.3% Fe/BiOS catalyst prepared in example 2 in the test for degrading tetracycline by photocatalytically activating persulfate, 90% of tetracycline was degraded; 5.6% Fe/BiOS catalyst prepared in example 3 in the test for degrading tetracycline by photocatalytically activating persulfate, 86% of tetracycline was degraded; without coming into contact withModified Bi 2 O 2 S in the experiment that the persulfate is photocatalytically activated to degrade the tetracycline, 57 percent of the tetracycline is degraded, thereby showing that the performance of the catalyst prepared in the embodiments 1-3 of the invention in the experiment that the persulfate is photocatalytically activated to degrade the tetracycline is obviously higher than that of unmodified Bi 2 O 2 S。
Fig. 3 is a TEM image of an iron-doped bismuth oxysulfide photocatalyst prepared in example 2 of the present invention. As can be seen from the figure, the iron-doped bismuth oxysulfide photocatalyst prepared by the ball milling method is in a nano-flake shape.
Fig. 4 is an XRD chart before and after the photocatalytic reaction of the iron-doped bismuth oxysulfide photocatalyst prepared in example 2 of the present invention. As can be seen from the figure, XRD of the iron-doped bismuth oxysulfide photocatalyst before and after the photocatalytic reaction has no obvious change, which shows that the iron-doped bismuth oxysulfide photocatalyst has good stability.
Comparative example 1
The difference from example 2 is that the ball milling time was 10min.
As a result of subjecting it to the performance test for degrading tetracycline by photocatalytically activating persulfate in the same manner as in example 2, 84% of tetracycline was degraded.
Comparative example 2
The difference from example 2 is that the ball milling time was 40min.
The same method as that of example 2 was used to carry out the photocatalytic activation persulfate degradation tetracycline performance test, and it was found that 90% of tetracycline was degraded.
FIG. 5 is a graph showing the effect of the iron-doped bismuth oxysulfide photocatalysts prepared in the examples 2, 1 and 2 of the present invention on degrading tetracycline by activating persulfate through photocatalysis. As can be seen from the figure, after 30min of photocatalytic reaction, the effect of photocatalytic activation of persulfate by the iron-doped bismuth oxysulfide photocatalyst obtained by grinding for 10min on tetracycline degradation is inferior to that of the iron-doped bismuth oxysulfide photocatalyst obtained by grinding for 20 min; the iron-doped bismuth-oxygen-sulfur photocatalyst obtained by grinding for 20min and 40min has the same effect of photocatalytic activation of persulfate to degrade tetracycline. But the method for grinding for 20min to obtain the iron-doped bismuth oxysulfide photocatalyst is more suitable in consideration of energy consumption and cost.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. The Fe-doped Bi-O-S photocatalyst is characterized in that Bi is used 2 O 2 S crystal and Fe (NO) 3 ) 3 ·9H 2 Preparing an iron-doped bismuth oxysulfide photocatalyst by using O as a raw material and adopting a high-energy ball milling method; wherein the doping amount of Fe in the Fe-doped bismuth oxysulfide photocatalyst is 1.7-5.6%.
2. The iron-doped bismuth oxysulfide photocatalyst according to claim 1, wherein said Bi 2 O 2 The S crystal is of a nano flaky structure.
3. A method of preparing an iron-doped bismuth oxysulfide photocatalyst as claimed in claim 1 or 2, characterized by comprising the following steps:
with Bi 2 O 2 S crystal and Fe (NO) 3 ) 3 ·9H 2 O is used as a raw material, and a high-energy ball milling method is adopted to prepare the iron-doped bismuth oxysulfide photocatalyst, wherein Bi is 2 O 2 S crystal and Fe (NO) 3 ) 3 ·9H 2 The mass ratio of O is 0.5: (0.0625-0.2142).
4. The method for preparing the Fe-doped Bi-O-S photocatalyst according to claim 3, wherein in the ball milling process, the ball milling transport intensity is 800rpm, and the ball milling time is 20min.
5. The method for preparing the Fe-doped Bi-O-S photocatalyst according to claim 3, wherein the ball-milled sample is added into water at room temperature, stirred and dried.
6. The method according to claim 5, wherein the stirring time is 120min.
7. Use of an iron-doped bismuth oxysulfide photocatalyst as claimed in claim 1 or 2 for the photocatalytic activation of persulfates in the treatment of waste water containing organic matter.
8. The use of claim 7, wherein the organic substance is tetracycline.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211573611.6A CN115739118B (en) | 2022-12-08 | 2022-12-08 | Iron-doped bismuth oxygen sulfur photocatalyst and preparation method and application thereof |
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