CN107570191B - Preparation method and application of visible light catalyst - Google Patents
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- 239000000843 powder Substances 0.000 claims abstract description 15
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- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- 229910052573 porcelain Inorganic materials 0.000 claims description 13
- 239000012279 sodium borohydride Substances 0.000 claims description 9
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 230000001580 bacterial effect Effects 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 239000002953 phosphate buffered saline Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- LOKCTEFSRHRXRJ-UHFFFAOYSA-I dipotassium trisodium dihydrogen phosphate hydrogen phosphate dichloride Chemical compound P(=O)(O)(O)[O-].[K+].P(=O)(O)([O-])[O-].[Na+].[Na+].[Cl-].[K+].[Cl-].[Na+] LOKCTEFSRHRXRJ-UHFFFAOYSA-I 0.000 claims description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 4
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- 238000007865 diluting Methods 0.000 claims 1
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- 239000002105 nanoparticle Substances 0.000 abstract description 12
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Abstract
The invention relates to a preparation method and application of a visible light catalyst, belonging to the field of preparation of environmental materials. In particular to Au and Ag nano-particle modified g-C3N4Catalyst (Au/Ag/g-C)3N4) The preparation method and the sterilization under the irradiation of visible light mainly comprise the following steps: (1) g-C3N4Preparing powder; (2) Au/Ag/g-C3N4Preparing powder; (3) visible light catalytic sterilization. The invention adopts Au and Ag nano particles in g-C3N4The surface load improves the capability of absorbing visible light, so that the catalyst can generate good catalytic effect under the irradiation of sunlight, thereby reducing the energy consumption and simultaneously achieving better sterilization effect.
Description
Technical Field
The invention relates to a preparation method and application of a visible light catalyst, in particular to g-C modified by Au and Ag nano particles3N4Catalyst (Au/Ag/g-C)3N4) The preparation method and sterilization under visible light irradiation belong to the field of environmental material preparation.
Background
The photocatalysis technology is a green technology with important application prospect in the fields of energy and environment. Photocatalysis has been widely studied and applied as a natural phenomenon in the fields of electrochemistry, photochemistry, catalytic chemistry, biochemistry, and the like. In 1972, Fujiehima et al published "Electrochemical catalysis of water at elementary electrode" in Nature, and opened the introduction of a new era of photocatalysis. In the next decades, the photocatalytic technology has attracted much attention, and has led to a number of important research directions, such as photocatalytic sterilization, water treatment, and air purification.
g-C3N4Is a metal-free semiconductor with a medium band gap (2.65eV) in the polymer, and itPossesses a two-dimensional layered structure of pi-conjugated graphite planes formed by hybridization of carbon and nitrogen sp 2. g-C3N4Due to its unique properties, such as physical and chemical stability, response to visible light, ease of preparation, etc., applications in the field of photocatalysis, such as photodegradation of various pollutants, hydrogen generation by water decomposition, and photocatalytic reduction of CO2, have been brought about. However, pure g-C3N4In the field of photocatalysis, the defects of low utilization efficiency of visible light, rapid recombination of photo-generated electron pairs and the like still limit the further improvement of the photocatalytic activity. Thus, several approaches have been taken to increase g-C3N4Such as nano/mesoporous structure design, doping with metallic or non-metallic elements, surface modification, heterostructure nanocomposite preparation, and the like. The Surface Plasmon Resonance (SPR) effect of noble metals derived from collective coherent oscillations of surface electrons makes noble metal Nanoparticles (NPs) promising candidates for harvesting ultraviolet and visible light. Therefore, noble metal-semiconductor composite materials have been widely developed as effective visible light-induced plasma-excited photocatalysts. For example, Au/TiO2Systems and Ag/AgX (X ═ Cl, Br) systems have been well utilized as such plasma photocatalysts. In these systems, the new metal NPs can be considered as an effective medium for absorbing light, and then the hot electrons generated on the NPs increase the light energy and further migrate to the conduction band of the semiconductor. In addition, the combination of two different novel metal NPs has shown excellent bimetallic synergy in many important reactions in the catalytic field.
Thus, the present invention is in g-C3N4Au and Ag NPs are loaded on the film, and the SPR of the film is adjusted to the visible light region through the Au NPs, so that the visible light absorption efficiency of the film is improved. The Ag NPs are used for promoting the separation of charge carriers and receiving separated photogenerated electrons, so that the photocatalytic efficiency of the material is improved. The loaded catalyst can well absorb visible light, generates better photocatalysis efficiency, and can be better applied to the field of photocatalysis sterilization.
Disclosure of Invention
The invention modifies g-C by Au and Ag nano particles3N4Preparing the visible light catalystAu/Ag/g-C3N4And is applied to sterilization under the irradiation of visible light. The method has the advantages that the prepared catalyst can obtain a catalytic effect under visible light and can be well applied to sterilization.
The technical scheme of the invention is as follows:
visible light catalyst (Au/Ag/g-C)3N4) The preparation method comprises the following steps:
step 1, preparing graphite-like carbon nitride (g-C)3N4): a certain amount of urea is weighed in a porcelain boat, and the porcelain boat with the same size is reversely buckled on the porcelain boat, so that the urea is in a relatively sealed environment. Then the porcelain boat is placed in a tube furnace, and the temperature is raised to 550 ℃ at a certain heating rate under the protection of nitrogen for calcination. Finally naturally cooling to room temperature to obtain a light yellow solid, and then grinding in an agate mortar to obtain g-C3N4And (3) powder.
Step 2, preparing visible-light-driven photocatalyst Au/Ag/g-C3N4: measuring a certain volume of silver nitrate (AgNO)3) Solution and chloroauric acid (HAuCl)4) The solutions were added to a beaker together, then a measured amount of polyvinyl alcohol (PVA) solution was added to the beaker and stirred magnetically at room temperature to obtain a homogeneous solution. Then weighing a certain amount of g-C prepared in step (1)3N4The powder, added to the solution and stirred for an additional 1 hour. Then, sodium borohydride solution prepared by ice water with certain concentration is measured, the sodium borohydride solution is slowly dripped into the solution while stirring, and then the stirring is continued for 3 hours. Finally, filtering and washing, drying in a 40 ℃ oven, grinding with an agate mortar to obtain Au/Ag/g-C3N4And (3) powder. In the step 1, the heating rate is 5-10 ℃/min, and the calcining time is 2-4 h.
In the step 2, the concentration of silver nitrate is 1g/10mL, the measured volume is 0.079-0.314mL, namely the final Ag and g-C3N4Is 0.25-1 wt.%.
In the step 2, the concentration of the chloroauric acid is 1g/10mL, the measured volume is 0.418-1.672mL, namely the final Au and g-C3N4Is 1-4 wt.%.
In step 2, the mass fraction of Au and Ag was 5.3 wt.%.
In step 2, the concentration of polyvinyl alcohol used is 1%, i.e. 1g of polyvinyl alcohol is dissolved in 99mL of deionized water. The volume of the polyvinyl alcohol measured was 5 mL.
In step 2, g-C is weighed3N4The mass of the powder was 2 g.
In the step 2, the concentration of the sodium borohydride used is 0.1mol/L, and the volume is 5 mL.
Visible light catalyst (Au/Ag/g-C)3N4) The use of (a) for photocatalytic disinfection: weighing a certain amount of Au/Ag/g-C3N4The powder was added to a centrifuge tube containing 5mL of the bacterial dispersion and sealed with a sealing film, followed by irradiation with simulated sunlight for a certain period of time. Then, 5. mu.L of the irradiated bacterial solution was diluted 10000 times with Phosphate Buffered Saline (PBS), 100. mu.L of the diluted solution was applied to a solid LB medium and placed in a CO2Culturing at 37 deg.C for 12h, counting the number of colonies, and calculating the sterilization efficiency.
In step 3, the amount of the catalyst weighed is 50-200. mu.g, i.e., the final catalyst concentration is 10-40. mu.g/mL.
In the step 3, the irradiation time is 1-3 h.
In step 3, the bacteria used is one of gram-positive bacteria staphylococcus aureus (s.aureus, ATCC 25923) or gram-negative bacteria escherichia coli (e.coil, IFO 3301), provided by life science research institute of Jiangsu university.
The silver nitrate and the chloroauric acid in the technical scheme have the functions of providing Ag+And Au3+。
The polyvinyl alcohol solution in the above technical scheme is used as a surfactant.
The sodium borohydride solution in the technical scheme is used as a reducing agent.
The phosphate buffer solution in the technical scheme has the function of simulating the liquid environment in the human body.
The invention adopts Au and Ag nano-particlesThe particles are in g-C3N4The surface load improves the capability of absorbing visible light, so that the catalyst can generate good catalytic effect under the irradiation of sunlight, thereby reducing the energy consumption and simultaneously achieving better sterilization effect.
Detailed Description
The catalyst prepared by the technical scheme is applied to visible light catalytic sterilization, and the invention is further explained by combining specific implementation examples.
Example 1
(1)g-C3N4Preparation of
A certain amount of urea is weighed in a porcelain boat, and the porcelain boat with the same size is reversely buckled on the porcelain boat, so that the urea is in a relatively sealed environment. Then the porcelain boat is placed in a tube furnace, the temperature is raised to 550 ℃ at the temperature rise rate of 5 ℃/min under the protection of nitrogen, and the porcelain boat is calcined for 4 hours. Finally, the mixture is naturally cooled to room temperature to obtain a light yellow solid, and then the light yellow solid is ground in an agate mortar to obtain g-C3N4 powder.
(2)Au/Ag/g-C3N4Preparation of
0.157mL of silver nitrate (AgNO) was measured3) And 0.836mL of chloroauric acid (HAuCl)4) The solutions were added together in a beaker, then 5ml of polyvinyl alcohol (PVA) solution was measured and added to the beaker, and stirred magnetically at room temperature to obtain a homogeneous solution. Then 2g of g-C prepared in step (1) are weighed3N4The powder, added to the solution and stirred for an additional 1 hour. Then 5ml of sodium borohydride solution prepared by ice water with certain concentration is measured, the sodium borohydride solution is slowly dripped into the solution while stirring, and then the stirring is continued for 3 hours. Finally, filtering and washing, drying in a 40 ℃ oven, grinding with an agate mortar to obtain Au/Ag/g-C3N4And (3) powder.
(3) Catalytic sterilization
Weighing 200 mu g of Au/Ag/g-C3N4The powder was added to a centrifuge tube containing 5mL of a dispersion of gram-positive bacteria staphylococcus aureus and sealed with a sealing film, followed by irradiation with simulated sunlight for 3 hours. Then, 5. mu.L of the irradiated bacterial solution was diluted with Phosphate Buffered Saline (PBS)10000 times, 100 μ L diluted solution is coated on solid LB culture medium and placed in CO2Culturing at 37 deg.C for 12h, counting the number of colonies, and calculating the sterilization efficiency. The resulting bactericidal efficiency is shown in table 1.
Example 2
Just changing the volume of the silver nitrate solution measured in the step (2) of the example 1 into 0.079mL and 0.314mL as in the example 1; the volume of the corresponding chloroauric acid solution was 0.418mL, 1.672 mL. Namely prepared Au/Ag/g-C3N4Ag and g-C in the powder3N4Is 0.25 wt.% and 1 wt.%; corresponding Au and g-C3N4Is 1 wt.% and 4 wt.%. The sterilization efficiency of the prepared catalyst is shown in table 1. The result shows that the larger the loading amount of the Ag and Au nano particles is, the better the visible light catalytic sterilization efficiency is.
Table 1 influence of different noble metal nanoparticle loading amounts on the catalytic sterilization efficiency of the obtained visible light catalyst
| Noble metal loading (Ag, Au, wt.%) | Sterilization efficiency (%) |
| 0.25，1 | 70 |
| 0.5，2 | 85 |
| 1，4 | 92 |
Example 3
Just as in example 1, the amount of the catalyst used in step (3) of example 1 was changed to 0, 50, 100. mu.g, i.e., the final catalyst concentration was 0, 10, 20. mu.g/mL. The resulting sterilization efficiencies are shown in table 2. The results show that the efficiency of visible light catalytic sterilization is increased along with the increase of the using amount of the catalyst. This is because the amount of catalyst increases, with the consequent release of more ROS after illumination and therefore easier killing of bacteria.
TABLE 2 Effect of different catalyst concentrations on the efficiency of visible light photocatalytic sterilization
| Catalyst concentration (μ g/mL) | Sterilization efficiency (%) |
| 0 | 5 |
| 10 | 62 |
| 20 | 73 |
| 40 | 85 |
Example 4
Just as in example 1, the light irradiation time in step (3) of example 1 was changed to 0, 1, 2 h. The resulting bactericidal efficiency is shown in table 3. The result shows that the visible light catalytic sterilization efficiency is increased along with the prolonging of the illumination time.
TABLE 3 influence of different illumination time on the visible light catalytic sterilization efficiency
Example 5
As in example 1, only the gram-negative bacterium Escherichia coli was used in step (3) of example 1. The resulting bactericidal efficiency is shown in table 4. The result shows that the catalyst has good bactericidal effect on gram-positive bacteria and gram-negative bacilli under the irradiation of visible light. But, in contrast, the bactericidal effect on gram-positive bacteria is better. This is probably because the cell wall structure of gram-negative bacilli is more complex than that of gram-positive bacteria, thus resulting in a stronger ability to resist ROS.
TABLE 4 comparison of the catalytic sterilization efficiency of visible light catalyst for different kinds of bacteria
| Bacterial species | Sterilization efficiency (%) |
| S.aureus | 85 |
| E.coil | 80 |
Claims (1)
1. The use of a visible light catalyst is characterized by being used for photocatalytic sterilization, and the visible light catalyst is prepared by the following steps: weighing a certain amount of Au/Ag/g-C3N4Adding a visible light catalyst into a centrifugal tube containing 5mL of bacterial dispersion, sealing the centrifugal tube with a sealing film, and irradiating the centrifugal tube with simulated sunlight for a certain time; then, 5. mu.L of the irradiated bacterial solution was dissolved in Phosphate Buffered Saline (PBS)Diluting 10000 times, applying 100 μ L diluted solution to solid LB culture medium, and placing in CO2Culturing for 12h at 37 ℃ in an incubator, counting the number of colonies, and calculating the sterilization efficiency;
wherein the concentration of the final catalyst is 10-40 mug/mL; the irradiation time is 1-3 h; the bacteria is one of gram-positive bacteria staphylococcus aureus or gram-negative bacteria escherichia coli;
the preparation method of the visible light catalyst comprises the following steps:
step 1, preparing graphite-like carbon nitride (g-C)3N4): weighing a certain amount of urea in a porcelain boat, and reversely buckling the porcelain boat with the same size on the porcelain boat to enable the urea to be in a relatively sealed environment; then placing the porcelain boat in a tube furnace, heating to 550 ℃ at a certain heating rate under the protection of nitrogen, and calcining; finally naturally cooling to room temperature to obtain a light yellow solid, and then grinding in an agate mortar to obtain g-C3N4Powder;
step 2, preparing visible-light-driven photocatalyst Au/Ag/g-C3N4: measuring a certain volume of silver nitrate (AgNO)3) Solution and chloroauric acid (HAuCl)4) Adding the solutions into a beaker together, then measuring a certain amount of polyvinyl alcohol (PVA) solution and adding the PVA solution into the beaker, and magnetically stirring the PVA solution at room temperature to obtain a uniform solution; then weighing a certain amount of g-C prepared in step 13N4Adding the powder into the solution and continuously stirring for 1 hour; then measuring a sodium borohydride solution prepared by ice water with a certain concentration, slowly dripping the sodium borohydride solution into the solution while stirring, and then continuously stirring for 3 hours; finally, filtering and washing, drying in a 40 ℃ oven, grinding with an agate mortar to obtain Au/Ag/g-C3N4A visible light catalyst;
in the step 1, the heating rate is 5-10 ℃/min, and the calcining time is 2-4 h;
in the step 2, the concentration of the silver nitrate solution is 1g/10mL, and finally Ag and g-C are obtained3N40.25-1 wt.%;
in step 2, the concentration of the chloroauric acid solution is 1g/10mL, and finally Au is mixed withg-C3N41-4 wt.%;
in the step 2, the concentration of the polyvinyl alcohol solution is 1 percent, namely 1g of polyvinyl alcohol is dissolved in 99mL of deionized water; the volume of the polyvinyl alcohol is 5 mL;
in step 2, g-C is weighed3N4The mass of the powder was 2 g;
in the step 2, the concentration of the sodium borohydride solution is 0.1mol/L, and the volume is 5 mL.
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| CN108704657B (en) * | 2018-05-31 | 2020-12-11 | 广东工业大学 | A kind of red phosphorus/graphite phase carbon nitride composite nanosheet and its preparation method and application |
| CN109550049B (en) * | 2018-12-03 | 2021-06-18 | 浙江大学 | Application of carbon quantum dots-graphite-like carbon nitride photocatalytic materials in the preparation of drugs for sterilization and skin scar healing |
| CN110339859A (en) * | 2019-07-12 | 2019-10-18 | 河南省口岸食品检验检测所 | Preparation method and application of a multifunctional paper-based composite material loaded with bimetallic nanoparticles |
| CN112375804B (en) * | 2020-09-30 | 2023-12-12 | 长春理工大学 | Au/g-C 3 N 4 All-weather photocatalytic antibacterial material and light-dark dual-mode antibacterial mechanism thereof |
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| Title |
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| Facile synthesis, characterization and photocatalytic performance of Au-Ag alloy nanoparticles dispersed on graphitic carbon nitride under visible light irradiations;Mohammed A. Gondal, et al.;《Journal of Molecular Catalysis A: Chemical》;20160616;第423卷;第114-125页 * |
| Visible-light-driven enhanced antibacterial and biofilm elimination activity of graphitic carbon nitride by embedded Ag nanoparticles;Wei Bing, et al.;《Nano Research》;20151231;第8卷(第5期);第1648-1658页 * |
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