CN101618322A - Photocatalysis antibacterial material excited by visible light and application thereof - Google Patents

Photocatalysis antibacterial material excited by visible light and application thereof Download PDF

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Publication number
CN101618322A
CN101618322A CN200910055720A CN200910055720A CN101618322A CN 101618322 A CN101618322 A CN 101618322A CN 200910055720 A CN200910055720 A CN 200910055720A CN 200910055720 A CN200910055720 A CN 200910055720A CN 101618322 A CN101618322 A CN 101618322A
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metal
visible light
load
excited
photocatalysis antibacterial
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王文中
任佳
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention relates to a photocatalysis antibacterial material excited by visible light and an application thereof. The photocatalysis antibacterial material excited by visible light is characterized in that the noble metal of Pd, Pt, Au or Ag or any metal of Cu and Ni is loaded on a Bi2WO6 material in a form of nitrate when Bi2WO6 is generated to form a metal loaded Bi2WO6 material system. The loading content is controlled by adjusting the content of the loaded noble metal or any metal of the Ni and the Cu. The loaded metal content is 0.0025-0.05 M. The visible light photocatalysis antibacterial performance of the Bi2WO6 is greatly improved by combining the synergetic effect between the noble metal or any metal of the Ni and the Cu and a semiconductor and loading the noble metal on the surface of the Bi2WO6, and the illumination 30-min antibacterial rate reaches more than 99.9 percent. The loading process is simple, and the visible light photocatalysis antibacterial material is potential. The limit for increasing an ultraviolet light source when the photocatalysis material is applied in a room or outside the room is overcome, if sunlight is used as a light source, the utilization ratio of the sunlight can be also greatly improved.

Description

The photocatalysis antibacterial material of excited by visible light and application thereof
Technical field
The present invention relates to a kind of photocatalysis antibacterial material of excited by visible light, be used for sewage disposal, indoor-outdoor air purifies and sterilization, also has each building materials field and small stores fields such as coating, glass, light fixture, highway.
Background technology
From Fujishima in 1972 (Nature, 238 (1972), 37-38) wait and find monocrystalline TiO first 2After can photochemical catalyzing on the electrode, Carey etc. be successfully with TiO 2Be used for photocatalytic degradation water organic pollution, conductor photocatalysis is subjected to various countries' environment and energy research person's common concern rapidly.Because there are some shortcomings in traditional water sterilization technology, such as cholorination, shows after deliberation, can produce the toxic byproduct that has of harmful person health, so the traditional water disinfection technology can not be by excellent popularization.And in 1985, (FEMS Microbiology Letters 29 (1985) 211-214) waited discovery TiO to Japanese scientist Matsunaga 2Under UV-irradiation bactericidal action is arranged, this discovery makes the traditional water sterilization technology of the potential replacement of photocatalysis technology.TiO 2Because of its safety, stable and advantage with low cost, its photocatalysis antibacterial performance has been subjected to extensive studies.But TiO 2Only response is arranged in ultraviolet light range, and the ultraviolet light part not enough sunshine gross energy of wavelength below 400nm 5%, therefore in order to improve solar energy utilization rate, the photochemical catalyst of novel visible response is referred on the schedule.The research of the photocatalysis antibacterial agent of novel visible response has two big thinkings at present: a kind of is to TiO 2Modification make its response wave length red shift to visible region, mainly contain means such as metal/non-metal doping, dye photoactivation, narrow-band semiconductor (CdS etc.) be compound.Another kind is the novel visible-light response nano catalysis material of design, and this research direction also more and more is subjected to people's attention.
Bi 2WO 6Be one of the simplest composite oxides among the Aurivillius family, its molecular formula is Bi 2A N-1B nO 3n+3(A=Ca, Sr, Ba, Pb, Bi, Na, K, B=Ti, Nb, Ta, Mo, W, Fe).Previous relevant Bi 2WO 6Bibliographical information show (J.Phys.Chem.B, 109 (2005), 22432-22439): Bi 2WO 6The activity that high photocatalysis to degrade organic matter is arranged, and good stability more and more receive publicity.
Summary of the invention
The object of the invention is to provide a kind of non-TiO 2System, the photocatalysis antibacterial material of excited by visible light and application thereof.Described visible light catalytic anti-biotic material Bi 2WO 6The Bi of material and metal load 2WO 6Material system, the latter does not appear in the newspapers so far, described metal be Ag, Pt, Pd or Au at interior noble metal, also comprise the Bi of metal loads such as Ni or Cu 2WO 6Thereby realize the lifting of its photocatalysis antibacterial performance.
Described metal load Bi 2WO 6Material system is characterised in that any metal among Pd, Pt, Au or Ag noble metal or Cu and the Ni with the form of nitrate, at Bi 2WO 6Load to Bi when generating 2WO 6On the material, form the Bi of metal load 2WO 6Material system.The quality of any metal among noble metal by adjusting described load or Ni and the Cu realizes the control of load capacity.The amount of metal of load is 0.0025M～0.05M.
Bi 2WO 6The preparation of carried noble metal or metal is:
(a) Bi (NO of 0.01M～0.1M 3) 35H 2The Na of O and 0.01M～0.1M 2WO 42H 2O is a raw material, presses Bi 2WO 6Stoichiometric, add the nitrate of the metal supported ionic of 0.025M～0.05M, be solvent with ethanol, glycerine or ethylene glycol, stir into precursor solution;
(b) with the precursor solution of step a preparation, put into water heating kettle, heat treatment under 100～200 ℃ of conditions;
(c) sedimentation and filtration after step b reaction finishes is used deionized water earlier, uses absolute ethanol washing again, then in 40～80 ℃ of oven dry;
Described metal supported ionic is any among Pt, Pd, Au or Ag noble metal and Ni or the Cu.
Wherein,
(1) heat treatment time of water heating kettle is 6～24 hours among the step b;
(2) filtering among the step c is to use deionized water earlier, respectively washs 5～10 times with absolute ethyl alcohol again;
(3) ethanol, glycerine or ethylene glycol had not only been made solvent but also as the reducing agent of source metal.
Component provided by the invention is Bi 2WO 6And the Bi of metal load 2WO 6Material system is in conjunction with any metal and Bi among noble metal or Ni and the Cu 2WO 6Synergy, under radiation of visible light, can be at short notice to the gramnegative bacterium Escherichia coli, gram-positive bacterium surface staphylococcus, staphylococcus aureus etc. have good inhibitory action.
Visible light photocatalysis anti-biotic material of the present invention, make at outdoor sunshine, have good photocatalysis antibacterial activity under the indoor natural light, improved utilization rate, also overcome catalysis material and can only be used for outdoor or when indoor application, must add the limitation of ultraviolet source visible light.Simultaneously, provide the method for a kind of noble metal and Cu or Ni load, realized lifting its performance.
Description of drawings
Fig. 1 is the Bi of preparation among the embodiment 1 2WO 6The XRD diffracting spectrum;
Fig. 2 is the blank sample of plate count experimental result picture: A.; B. do not add sample illumination 2h; C. add sample not only according to 2h; D. add sample illumination 2h;
Fig. 3 is Bi 2WO 6Antibiotic curve map;
Fig. 4 is Ag load Bi 2WO 6The XRD diffracting spectrum;
Fig. 5 is Ag load Bi 2WO 6Ultraviolet/visible diffuse reflectance spectra;
Fig. 6 is pure Bi 2WO 6With Ag load Bi 2WO 6The antibiotic rate block diagram.
The specific embodiment
Embodiment 1 pure Bi 2WO 6Preparation and be used for that photocatalysis antibacterial is active to be detected
Bi 2WO 6Use Bi (NO 3) 25H 2O and Na 2WO 42H 2O is that raw material is synthetic, according to stoichiometric proportion, takes by weighing 0.97g Bi (NO 3) 25H 2O (analyzing pure) is dissolved in the 20mL water, adds the 0.210g citric acid then, stirs 30 minutes, with 0.329g Na 2WO 42H 2O (analyzing pure) is dissolved in the 20mL water, and both mix stirring and form white suspension pioneer liquid.Get certain volume then and put into water heating kettle, under 180 ℃ of conditions of temperature, handled 24 hours.Reaction with the faint yellow sedimentation and filtration that obtains, is respectively washed 5 times with deionized water, absolute ethyl alcohol, then 80 ℃ of dryings after finishing.As Fig. 1, be defined as Bi through the XRD material phase analysis 2WO 6, by the mensuration to product ultraviolet/visible diffuse reflectance spectra, until the visible region all has photoresponse, the estimation band gap is 2.76eV to this photochemical catalyst from ultraviolet region.
Estimate prepared Bi with colony counting method 2WO 6The photocatalysis antibacterial activity.To spend the night with the Escherichia coli that the LB nutrient solution is cultivated, collect, centrifugal, the physiological saline washing with 0.9% three times, dilution is～10 more at last 7The suspension of cfu/ml is with standby.The 500W-Xe lamp is a light source, adds a λ＞420nm filter plate to guarantee the elimination ultraviolet band, and photochemical catalyst concentration is 0.5mg/ml, illumination 2h, and antimicrobial efficiency reaches more than 95%.As shown in Figure 2, do not add sample illumination 2h and add sample not only according to two contrast and experiment demonstrations of 2h, bacterial number does not change substantially yet, illustrates that the sample of test itself does not have toxicity to bacterium.Two contrast experiment's explanation Bi under illumination 2WO 6Bacterium there is killing action, anti-microbial property is arranged.
The Bi of the Ag ion load of embodiment 2 different amounts 2WO 6The preparation of material and be used for the photocatalysis antibacterial skewer and survey
A) whole system is an ethanol system, with the Bi (NO of 0.01M 3) 25H 2The Na of O (analyzing pure) and 0.01M 2WO 42H 2O (analyzing pure) stirs, and adds the AgNO of 0.0025M 3, stirred 10 minutes, evenly mix.Get the predecessor of certain volume then and put into water heating kettle, under 160 ℃ of conditions of temperature, handled 24 hours.Reaction with the sedimentation and filtration that obtains, is respectively washed 5 times with deionized water, absolute ethyl alcohol, then 60 ℃ of dryings after finishing.As Fig. 4, because the amount of Ag is few, the characteristic peak of Ag can not obviously be seen (AB-0.1) in the XRD spectrum, but in ultraviolet/visible diffuse reflectance spectra, can see because the surface plasma body resonant vibration of Ag absorbs caused bulge (Fig. 5), simultaneously in power spectrum, can see the peak that Ag is arranged, can confirm that in conjunction with both the load of Ag successfully realizes.The visible light photocatalysis antibacterial experiment is the result show, Ag load Bi 2WO 6The photocatalysis antibacterial performance improve greatly.Illumination 30min, antibiotic rate reaches 99%.
B) whole system is the glycerine system, with the Bi (NO of 0.1M 3) 25H 2The Na of O (analyzing pure) and 0.1M 2WO 42H 2O (analyzing pure) stirs, and adds the AgNO of 0.05M 3, stirred 10 minutes, evenly mix.Get the predecessor of certain volume then and put into water heating kettle, under 160 ℃ of conditions of temperature, handled 24 hours.After reaction finishes, with the sedimentation and filtration that obtains, earlier with deionized water, respectively wash 8 times with absolute ethyl alcohol again, 60 ℃ of dryings then.The characteristic peak of Ag can obviously be seen (AB-1.0) in the XRD spectrum, also can see because the surface plasma body resonant vibration of Ag absorbs caused bulge (Fig. 5) in ultraviolet/visible diffuse reflectance spectra.As Fig. 6, the visible light photocatalysis antibacterial experiment is the result show, the photocatalysis antibacterial performance is slightly higher than embodiment 1, and is close with embodiment (a).
C) whole system is a glycol system, with the Bi (NO of 0.05M 3) 25H 2The Na of O (analyzing pure) and 0.05M 2WO 42H 2O (analyzing pure) stirs, and adds the AgNO of 0.005M 3, stirred 10 minutes, evenly mix.Get the predecessor of certain volume then and put into water heating kettle, under 160 ℃ of conditions of temperature, handled 24 hours.After reaction finishes, with the sedimentation and filtration that obtains, earlier with deionized water, respectively wash 10 times with absolute ethyl alcohol again, 60 ℃ of dryings then.Product is defined as Ag/Bi through XRD and energy spectrum composition analysis 2WO 6, Ag load Bi 2WO 6The photocatalysis antibacterial performance improve greatly.Illumination 30min, antibiotic rate reaches 99.9%.
The Ag load changes Pd, Pt into or Au has similar result in the present embodiment.
The Bi of embodiment 3Ni ion load 2WO 6The preparation of material and be used for the photocatalysis antibacterial skewer and survey
Whole system is a glycol system, with the Bi (NO of 0.05M 3) 25H 2The Na of O (analyzing pure) and 0.05M 2WO 42H 2O (analyzing pure) stirs, and adds the Ni (NO of 0.005M 3) 26H 2O stirred 10 minutes, evenly mixed.Get the predecessor of certain volume then and put into water heating kettle, under 160 ℃ of conditions of temperature, handled 24 hours.Reaction with the sedimentation and filtration that obtains, is respectively washed 5 times with deionized water, absolute ethyl alcohol, then 60 ℃ of dryings after finishing.Product is defined as Ni/Bi through XRD and energy spectrum composition analysis 2WO 6, Ni load Bi 2WO 6The photocatalysis antibacterial performance improve greatly.Illumination 30min, antibiotic rate reaches 99%.All the other are with embodiment 2.
The Bi of embodiment 4Cu ion load 2WO 6The preparation of material and be used for the photocatalysis antibacterial skewer and survey
Whole system is the glycerine system, with the Bi (NO of 0.1M 3) 25H 2The Na of O (analyzing pure) and 0.1M 2WO 42H 2O (analyzing pure) stirs, and adds the Cu (NO of 0.05M 3) 23H 2O stirred 10 minutes, evenly mixed.Get the predecessor of certain volume then and put into water heating kettle, under 160 ℃ of conditions of temperature, handled 24 hours.Reaction with the sedimentation and filtration that obtains, is respectively washed 8 times with deionized water, absolute ethyl alcohol, then 60 ℃ of dryings after finishing.Product is defined as Cu/Bi through XRD and energy spectrum composition analysis 2WO 6, Cu load Bi 2WO 6The photocatalysis antibacterial performance improve greatly.The photocatalysis antibacterial performance is slightly higher than embodiment 1, and is more lower slightly than embodiment 2 (c).All the other are with embodiment 2.

Claims (8)

1, the catalysis material of excited by visible light comprises Bi 2WO 6, it is characterized in that any metal among Pd, Pt, Au or Ag noble metal or Cu and the Ni with the form of nitrate, at Bi 2WO 6Load to Bi when generating 2WO 6On the material, form the Bi of metal load 2WO 6Material system.
2, by the catalysis material of the described excited by visible light of claim 1, it is characterized in that the quality of any metal among noble metal by adjusting described load or Ni and the Cu, realize the control of load capacity.
3, by the catalysis material of claim 1 or 2 described excited by visible light, the amount of metal that it is characterized in that load is 0.0025M～0.05M.
4, the method for the catalysis material of preparation excited by visible light as claimed in claim 1 is characterized in that comprising:
(a) Bi (NO of 0.01M～0.1M 3) 35H 2The Na of O and 0.01M～0.1M 2WO 42H 2O is a raw material, presses Bi 2WO 6Stoichiometric, add the nitrate of the metal supported ionic of 0.025M～0.05M, be solvent with ethanol, glycerine or ethylene glycol, stir into precursor solution;
(b) with the precursor solution of step a preparation, put into water heating kettle, heat treatment under 100～200 ℃ of conditions;
(c) it is to use deionized water earlier that the sediment after step b reaction finishes filters, and uses absolute ethanol washing again, then in 40～80 ℃ of oven dry;
Described metal supported ionic is any among Pt, Pd, Au or Ag noble metal and Ni or the Cu.
5, press the preparation method of the catalysis material of the described excited by visible light of claim 4, it is characterized in that:
(1) heat treatment time of water heating kettle is 6～24 hours among the step b;
(2) filtering among the step c is to use deionized water earlier, respectively washs 5～10 times with absolute ethyl alcohol again.
6,, it is characterized in that ethanol, glycerine or ethylene glycol are again as the reducing agent of source metal by the preparation method of the catalysis material of the described excited by visible light of claim 4.
7, press the application of the catalysis material of the described excited by visible light of claim 1, it is characterized in that:
(1) pure Bi 2WO 6Material has anti-microbial property under the illumination again, and antimicrobial efficiency reaches more than 95%;
(2) by Pt, Pd, Au or Ag noble metal; Or the Bi of any load among Ni and the Cu 2WO 6The material cording has the Bi of ratio 2WO 6Good anti-microbial property;
Described bacterium is the gramnegative bacterium Escherichia coli, gram-positive bacterium surface staphylococcus or staphylococcus aureus.
8, press the application of the catalysis material of the described excited by visible light of claim 1, it is characterized in that:
A) Ag load Bi 2WO 6The photocatalysis antibacterial of material, under 30min illumination, antibiotic rate reaches 99～99.9%;
B) Bi of Ni load 2WO 6The photocatalysis antibacterial of material, under 30min illumination, antibiotic rate reaches 99%;
C) Bi of Cu load 2WO 6The photocatalysis antibacterial of material is than pure Bi 2WO 6Height, but be lower than the Bi of Ag load 2WO 6Material.
CN200910055720A 2009-07-30 2009-07-30 Photocatalysis antibacterial material excited by visible light and application thereof Pending CN101618322A (en)

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