CN115301273A - O-g-C 3 N 4 Photocatalytic coupling persulfate, preparation method thereof and application thereof in degradation of resistance genes - Google Patents
O-g-C 3 N 4 Photocatalytic coupling persulfate, preparation method thereof and application thereof in degradation of resistance genes Download PDFInfo
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- 230000008878 coupling Effects 0.000 title claims abstract description 22
- 238000010168 coupling process Methods 0.000 title claims abstract description 22
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 22
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 title claims abstract description 21
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- 238000005406 washing Methods 0.000 claims abstract description 10
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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
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B01J35/61—
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
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- 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
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- 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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/007—Contaminated open waterways, rivers, lakes or ponds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
-
- 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
- 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 O-g-C 3 N 4 Photocatalytic coupling persulfate, preparation method thereof and application thereof in degrading resistance gene, O-g-C 3 N 4 The preparation method of the photocatalytic coupling persulfate comprises the following steps: adding urea into water, stirring to dissolve, adding sodium chloride, stirring overnight, adding ascorbic acid, stirring for 5 min, freezing at-80 deg.C for 2 hr, drying at 550 deg.C in a tubular furnace, grinding, washing with water, and oven drying to obtain O-g-C 3 N 4 . O-g-C obtained by the invention 3 N 4 The structure is an ultrathin porous flaky structure, and the specific surface area is large; obtained O-g-C 3 N 4 The coupling persulfate has excellent effect and good resistance gene degradation effect, and has great application potential in water purification.
Description
Technical Field
The invention relates to the technical field of photocatalysis materials and water body disinfection, in particular to O-g-C 3 N 4 A photocatalytic coupling persulfate, a preparation method thereof and application thereof in degrading resistance genes.
Background
Antibiotics are the most widely used and most diverse medicines in various clinical applications at home and abroad at present, and are one of effective means for preventing and treating infection. However, about 80% of antibiotics are not completely metabolically absorbed in humans, which induces a large number of resistant bacteria (ARBs), even "superbacteria" that are resistant to almost all antibiotics. The human expels the antibiotics and the ARB out of the body through activities such as defecation, urination and the like and enters the environmental medium. The selective pressure brought by antibiotics remained in the environment accelerates the Appearance of Resistance Genes (ARGs) in the environment, the ARGs can be transmitted in and among species through heredity, horizontal gene transfer and the like, and the ARGs form a great hidden danger of gene pollution to the ecological environment and human health.
The traditional sewage treatment technology mainly adopts a periodic cycle activated sludge method and a chlorine dioxide disinfection process, and although the treatment process can effectively reduce pathogenic microorganisms in water, the removal effect on antibiotics, resistant bacteria and resistant genes is limited. The removal effect of the disinfection technologies such as ultraviolet rays, liquid chlorine, ozone and the like on the ARB and the ARGs is very limited. Therefore, the development of a safe, efficient and environment-friendly key technology for removing the resistant bacteria and the resistant genes in water is urgently needed, and the key technology has important significance for realizing water purification.
The semiconductor photocatalysis technology is an advanced oxidation technology based on hydroxyl free radical (. OH), can thoroughly kill microorganisms by utilizing sunlight and degrade resistance genes, and is considered as the most potential 'green' water body purification technology in recent years. Among the numerous semiconductor photocatalysts, the graphite phase carbon nitride (g-C) 3 N 4 ) The two-dimensional layered semiconductor photocatalytic material is a typical two-dimensional layered semiconductor photocatalytic material, has a unique electronic and energy band structure, is narrow in forbidden band width (2.7 eV), can absorb visible light, is low in preparation cost, is stable in chemical structure, and has a good application prospect in the aspect of photocatalytic inactivation of resistant bacteria. But as a visible light responsive material, g-C 3 N 4 The valence band position is too high to directly generate the-OH, so that the content of the-OH in the system is low, and the photocatalytic activity of the system is influenced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention firstly provides O-g-C 3 N 4 The preparation method of the photocatalytic coupling persulfate solves the problems of low sunlight utilization rate and difficult degradation of resistance genes, and has important practical application value.
O-g-C 3 N 4 The preparation method of the photocatalytic coupling persulfate comprises the following steps: adding urea into water, stirring to dissolve, adding sodium chloride, stirring overnight, adding ascorbic acid, stirring for 5 min, freezing at-80 deg.C for 2 hr, drying at 550 deg.C in a tubular furnace, grinding, washing with water, and oven drying to obtain O-g-C 3 N 4 。
Preferably, said O-g-C 3 N 4 The preparation method of the photocatalytic coupling persulfate comprises the following steps: adding 2.0g of urea into 100mL of water, stirring until the urea is dissolved, adding 10g of sodium chloride, stirring overnight, adding 0.5g to 2.0g of ascorbic acid, continuously stirring for 5 min, freezing at-80 ℃ for 2h, and placing a samplePumping in a freeze drier, maintaining at 550 deg.C for 2 hr in a tube furnace, grinding, washing with water, and oven drying to obtain O-g-C 3 N 4 。
Preferably, the temperature rise rate of the tube furnace is 2.3 ℃/min, and nitrogen is introduced into the tube furnace.
Preferably, the water washing is centrifugal washing, and the number of times is 10.
O-g-C prepared by the invention 3 N 4 Application of photocatalysis coupling persulfate in inactivating resistant bacteria and degrading resistant genes in water.
Compared with the prior art, the invention has the following beneficial effects: O-g-C obtained by the invention 3 N 4 The material is an ultrathin porous sheet structure, and the specific surface area is large; obtained O-g-C 3 N 4 The coupling persulfate has excellent effect, when the resistant bacteria and the degradation resistance genes in the water body are inactivated by photocatalysis, the resistant bacteria are completely inactivated, the degradation effect of the resistance genes is good, and the coupling persulfate has great application potential in water body purification.
Drawings
Fig. 1 XRD pattern of nanomaterial;
FIG. 2 g-C 3 N 4 And 1.0Vc-g-C 3 N 4 FESEM (a-b), TEM (C-d) and 1.0Vc-g-C 3 N 4 A scan (e-h);
FIG. 3 is a UV-vis diagram of the nanomaterial;
FIG. 4N of nanomaterial 2 Adsorption-desorption curve chart;
FIG. 5 sample antagonizes tetracyclineE. coli(1.6×10 7 cfu/mL) inactivation effect profile: dark conditions (a), light conditions (b);
FIG. 6.0Vc-g-C 3 N 4 To pairtetBAnd16srRNAthe degradation effect of (2).
FIG. 7 actual water 1.0Vc-g-C 3 N 4 Degradation effect of antagonistic bacteria.
Detailed Description
O-g-C 3 N 4 Preparation of heterojunction photocatalyst:
adding 2.0g urea into 100ml water, stirring to dissolveAdding 10g of sodium chloride, stirring overnight, adding (0.5 g, 1.0g and 2.0g respectively) ascorbic acid, continuing stirring for 5 min, freezing at-80 ℃ for 2h, putting the sample into a freeze dryer, pumping, keeping at 550 ℃ for 2h in a tube furnace (introducing nitrogen, increasing the temperature at the rate of 2.3 ℃/min), grinding, centrifugally washing for 10 times, and drying to obtain O-g-C 3 N 4 Respectively marked as 0.5Vc-g-C 3 N 4 、1.0Vc-g-C 3 N 4 、2.0Vc-g-C 3 N 4 . Pure g-C 3 N 4 The preparation procedure of (a) was identical to the above except that no ascorbic acid was added.
FIG. 1 is an XRD pattern of nanomaterials made according to embodiments of the present invention. Pure g-C 3 N 4 At 13.0 o And 27.6 o Characteristic diffraction peak of (A) is attributed to g-C 3 N 4 (100) and (002) crystal planes of (2), 27.6 o The diffraction peak is stronger and is the structural accumulation between graphite-like layers, which shows that g-C 3 N 4 Has a layered structure similar to graphite. After doping with oxygen, O-g-C 3 N 4 The diffraction peak intensity of (2) is remarkably reduced, 13.0 o Has substantially disappeared diffraction peak at 27.6 o The diffraction peak shifts to the left, the interplanar spacing becomes larger, which indicates that the oxygen element is doped in g-C 3 N 4 Inside.
FIG. 2 shows g-C prepared according to an embodiment of the present invention 3 N 4 And 1.0Vc-g-C 3 N 4 FESEM, TEM and 1.0Vc-g-C of 3 N 4 A scan of (2). Undoped g-C can be clearly seen 3 N 4 In a block structure (FIG. 2a, c). O-g-C 3 N 4 Exhibits an ultra-thin porous structure (FIG. 2 b), whose TEM image further demonstrates O-g-C 3 N 4 Is an ultra-thin porous structure (fig. 2 d). In addition, fig. 2e-h show that the composite material is composed of three elements, C, N, O, and all elements are uniformly distributed. Shows that O-g-C is successfully prepared 3 N 4 。
FIG. 3 is a UV-vis diagram of nanomaterials made according to embodiments of the present invention. As can be seen in FIG. 3a, g-C 3 N 4 The absorption band edge of (A) is 450 nm, indicating that it is a visible light responseA photocatalytic material. And g-C 3 N 4 In contrast, O-g-C 3 N 4 Has absorption in the whole visible and ultraviolet range. FIG. 4 is N for nanomaterials 2 Adsorption-desorption curve chart. g-C 3 N 4 Is a typical type III isotherm and has no significant hysteresis loop, indicating that it is a non-porous structure. And all of O-g-C 3 N 4 All belong to IV-type isotherms, which indicate that a mesoporous structure exists.
O-g-C 3 N 4 Use of coupled persulfate:
mixing O-g-C 3 N 4 Adding into the Escherichia coli (containing anti-tetracycline)E. coli) The concentration of the photocatalyst in the wastewater of (2) was 100. Mu.g/mL, the concentration of PS was 6 mmoL/L,E. colihas a concentration of 1X 10 7 cfu/mL. Examine the material coupling of PS pairsE. coliSterilization effect and resistance to tetracycline (b)tetB) And16S rRNAthe degradation effect of (1). In addition, it is also directed to O-g-C 3 N 4 And analyzing the sterilization effect of the coupling PS system in the actual water body.
FIG. 5 is g-C of an embodiment of the present invention 3 N 4 And O-g-C 3 N 4 Antagonizing tetracyclineE. coli(1.6×10 7 cfu/mL). Under dark conditions (FIG. 5 a), all materials had little sterilization activity, indicating that the catalyst and PS pairsE. coliHas less toxicity. As shown in FIG. 5b, there was little effect on bacteria under illumination alone or in synergy with PS. g-C in the presence of a catalyst and PS in the reaction system under illumination 3 N 4 、0.5Vc-g-C 3 N 4 、1.0Vc-g-C 3 N 4 、2.0Vc-g-C 3 N 4 2.18 lg, 2.58 lg, 7.08 lg and 0.48 lg in the system respectivelyE. coliInactivation, wherein 1.0Vc-g-C 3 N 4 The sterilization effect of (2) is best.
FIG. 6 is a graph of 1.0Vc-g-C made by an embodiment of the present invention 3 N 4 To pairtetBAnd16srRNAthe degradation effect of (2). As can be seen from FIG. 6, after 80 min of reaction,tetBand16S rRNAsignificant degradation occurred.tetBThe concentration of (2) was reduced from 6.61 lg to 1.83 lg.16S rRNAThe concentration of (2) was reduced from 11.91 lg to 5.48 lg copies/mL. Indicating 1.0Vc-g-C 3 N 4 Has excellent photocatalytic degradation effect and can effectively block the transmission of resistance genes in water.
FIG. 7 shows 1.0Vc-g-C prepared according to an embodiment of the present invention 3 N 4 And (3) a degradation effect diagram on tetracycline resistant bacteria in an actual water body. In order to investigate the practical application effect of the material, tap water, plain lakes, fengquan lakes, guogong lakes and Muyanghu lakes are respectively used as media to research the inactivation effect of the tetracycline-resistant Escherichia coli in the natural water bodies, and 6.57 lg, 6.03 lg and 4.23 lg of Escherichia coli are inactivated respectively. These results show that 1.0Vc-g-C 3 N 4 Has satisfactory degradation efficiency in natural water with complex components.
Various modifications may be made to the above without departing from the spirit and scope of the invention as defined by the appended claims. The scope of the invention is therefore intended to be limited not by the foregoing description, but rather by the scope of the appended claims.
Claims (8)
1. O-g-C 3 N 4 The preparation method of the photocatalytic coupling persulfate is characterized by comprising the following steps of: adding urea into water, stirring to dissolve, adding sodium chloride, stirring overnight, adding ascorbic acid, stirring for 5 min, freezing at-80 deg.C for 2 hr, drying at 550 deg.C in a tubular furnace, grinding, washing with water, and oven drying to obtain O-g-C 3 N 4 。
2. O-g-C as claimed in claim 1 3 N 4 The preparation method of the photocatalytic coupling persulfate is characterized by comprising the following steps of: adding 2.0g of urea into 100mL of water, stirring until the urea is dissolved, adding 10g of sodium chloride, stirring overnight, adding 0.5g to 2.0g of ascorbic acid, continuously stirring for 5 min, freezing at-80 ℃ for 2h, putting the sample into a freeze dryer, pumping, drying in a tubular furnaceMaintaining at 550 ℃ for 2h, grinding, washing and drying to obtain O-g-C 3 N 4 。
3. O-g-C as claimed in claim 1 3 N 4 The preparation method of the photocatalytic coupling persulfate is characterized by comprising the following steps: ascorbic acid was added in an amount of 1.0g.
4. O-g-C as claimed in claim 1 3 N 4 The preparation method of the photocatalytic coupling persulfate is characterized by comprising the following steps: the temperature rise rate of the tubular furnace is 2.3 ℃/min, and nitrogen is introduced into the tubular furnace.
5. O-g-C as claimed in claim 1 3 N 4 The preparation method of the photocatalytic coupling persulfate is characterized by comprising the following steps: the water washing is centrifugal washing, and the times are 10 times.
6. O-g-C obtainable by the process of any of claims 1 to 5 3 N 4 Coupling persulfate in a photocatalysis mode.
7. O-g-C as claimed in claim 6 3 N 4 Application of photocatalysis coupling persulfate in degrading resistance genes.
8. O-g-C as claimed in claim 6 3 N 4 Application of photocatalysis coupling persulfate in degrading tetracycline resistance genes.
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Citations (5)
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CN107298477A (en) * | 2017-06-22 | 2017-10-27 | 武汉纺织大学 | A kind of method for being catalyzed organic pollution in persulfate degrading waste water |
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