CN102085481A - Preparation and application of composite photo-catalysis bactericide for visible light response - Google Patents

Preparation and application of composite photo-catalysis bactericide for visible light response Download PDF

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CN102085481A
CN102085481A CN 201010609018 CN201010609018A CN102085481A CN 102085481 A CN102085481 A CN 102085481A CN 201010609018 CN201010609018 CN 201010609018 CN 201010609018 A CN201010609018 A CN 201010609018A CN 102085481 A CN102085481 A CN 102085481A
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catalyst
photo
sterilization
tio
composite photo
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阎建辉
张丽
唐课文
易健民
侯朝辉
潘阳
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Hunan Institute of Science and Technology
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Hunan Institute of Science and Technology
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Abstract

The invention relates to application of a nano composite material serving as a photo-catalysis sterilization antibacterial agent responding to visible light. The photo-catalysis material is a complex of copper chromate and titanium dioxide, and has good killing effect on escherichia coli under the irradiation of the visible light. In suspension, the photo-catalyst performs an analog sunlight catalysis sterilization experiment for 104CFU/mL escherichia coli; and when the consumption of the photo-catalyst is 1.0 to 3.0mug/mL, the mass percentage of TiO2 in the composite photo-catalyst is 70 to 90 percent, and the sterilization rate after 30 minutes reaches over 90 percent. When the analog sunlight catalysis sterilization experiments are performed on a ceramic tile coated with the photo-catalyst and a veneer coated with a coating containing the photo-catalyst, the sterilization rates after 30 minutes are over 90 percent and 85 percent respectively; and when the sunlight sterilization experiments are performed under the same condition, the sterilization rates after 30 minutes are over 90 percent and 83 percent respectively, so the sterilization effect of the composite photo-catalyst is obviously superior to that of a single photo-catalyst.

Description

A kind of preparation and application of visible light-responded composite photo-catalysis bactericide
Technical field
The present invention relates to a kind ofly has the nano composite material of response as preparation method and the application of photo-catalyst antiseptic to visible light, this catalysis material is CuCr 2O 4With TiO 2Compound, it has preferably killing action to large intestine sense bacterium etc. under radiation of visible light.
Background technology
From it is found that TiO 2TiO has been arranged under UV-irradiation since the good bactericidal effect 2Photocatalysis and sterilization mechanism receive publicity always.The antibacterial action of photochemical catalyst is based on its photocatalytic semiconductor material photoelectric characteristic, and photocatalytic semiconductor is to be made of valence band of filling up electronics low energy and empty high energy conduction band.When the light of certain wavelength is radiated at the catalysis material grain surface, it can absorb less than with the light wave that equals energy gap, make electron excitation in its valence band to conduction band, thereby form light induced electron-hole (e -And h +).The H of catalyst surface absorption this moment 2O and O 2Effectively capture light is given birth to electron-hole pair, makes them form activity hydroxy (OH) and the superoxide ion (O with strong oxidizing property 2-).Both are very strong oxidation, reducing agents, and their penetrable cell membranes destroy cellulose, enter the transmission that thalline stops film forming matter, block its respiratory system and electric transmission system, thus kill bacteria effectively.
Nano-TiO 2Because of it is nontoxic, cheap, chemical property is stable, and oxidability is strong, the photocatalytic activity advantages of higher is the photocatalysis antibacterial research emphasis always.Chinese patent in the past few years discloses several preparation method and application about photo-catalyst, antiseptic, is to use TiO mostly 2As photochemical catalyst, because TiO 2The restriction of its semiconductor energy gap can only absorb the ultraviolet light that accounts for sunshine 5% and its application is restricted, and TiO 2Quantum efficiency as photochemical catalyst is lower.For improving its practicality, antibiotic photochemical catalyst must enlarge its photoresponse scope and improve photo-quantum efficiency.Many scholars have carried out the modification research of various ways by semiconductor surface noble metal loading, semiconductor alloy, nonmetallic ion (atom) doping, compound other semiconductors and photoactivate etc. to titanium dioxide in recent years, wish to prepare effectively to absorb visible light, improve the photochemical catalyst of quantum efficiency.
Spinel-type CuCr 2O 4Be the catalyst of kind of function admirable, be widely used in oxidation, hydrogenation, dehydrogenation, dehydrocyclization, organic degraded, pollutant processing and propellant burning catalyst etc.CuCr 2O 4Be kind of a p-type semiconductor, its energy gap is about 1.4eV, and is better to visible absorption; And N-shaped semiconductor TiO 2Because its energy gap is about 3.2eV, there is not absorption in visible light, but it has higher photocatalytic activity.The quality of comprehensive two class catalysis materials, with its composite design is p-n junction hetero-junctions composite semiconductor catalyst, both advantages are fully used, particularly can suppress the compound of light induced electron-hole effectively, will improve the visible light catalytic bactericidal activity effectively by hetero-junctions.
Utilize citric acid assisting sol-gel method to prepare CuCr 2O 4/ TiO 2Heterojunction composite photocatalyst, and compare with the sample of the multiple method preparation of chemically composited method and physics, be research object with Escherichia coli, inquire into this composite photo-catalyst at different complex methods, n CuCr2O4: n TiO2Bactericidal effect under the conditions such as ratio, sintering temperature, activity, illumination condition and bacterium physical signs draws the optimal sterilization conditions of composite photo-catalyst.This research provides a new way for we solve anti-biotic material.
Summary of the invention
The objective of the invention is to the technical deficiency for existing inorganic sterilization material, a kind of response under visible light, the CuCr with spinel structure that quantum efficiency is high are provided 2O 4With TiO 2Composite photo-catalyst and preparation method thereof, this photochemical catalyst have stronger photo-catalyst ability in the aqueous solution, ceramic tile coating and coating under the effect of visible light.It is simple that the while photochemical catalyst has the preparation method, and raw material is easy to get, the characteristics of long service life.
The present invention in technical scheme with commodity copper nitrate, chromic nitrate, butyl titanate, citric acid and nano-TiO 2Adopt citric acid assisting sol-gel method to synthesize CuCr Deng reagent 2O 4, and have p-n junction CuCr with having prepared with liquid phase method and solid phase method respectively 2O 4/ TiO 2The hetero-junctions catalyst.Its concrete preparation method is as follows:
CuCr 2O 4Preparation: with 0.005mol Cu (NO 3) 2With 0.01mol Cr (NO 3) 2Be dissolved in the 50mL deionized water, under 80 ℃ of stirred in water bath, dropwise add in gained solution subsequently in the citric acid solution of 100mL0.3M and obtain vitreosol, continuation is heated in 80 ℃ of water-baths and is obtained colloidal sol, change in the baking oven, 120 ℃ of lower dry 4h obtain predecessor, calcine at a certain temperature at last 2h, namely get CuCr 2O 4Product.
TiO 2Preparation: under the room temperature with 10mL Ti (OBu) 4Join under vigorous stirring in the 20mL absolute ethyl alcohol, obtain evenly faint yellow transparent solution A, the solution that 6mL redistilled water and 30mL absolute ethyl alcohol are made into slowly drips the anhydrous acetic acid of 3mL under vigorous stirring, obtain solution B.Under vigorous stirring, A is slowly dropwise joined among the B, stir until till the formation gel, still aging, 120 ℃ of lower dryings obtain predecessor, calcine at a certain temperature 1h and namely get TiO 2
CuCr 2O 4/ TiO 2Preparation: with 0.003～0.005mol Cu (NO 3) 2With 0.006～0.01molCr (NO 3) 2Be dissolved in 30～50mL deionized water, under 80 ℃ of stirred in water bath, dropwise add in gained solution subsequently in the citric acid solution of 80～100ml 0.3M and obtain vitreosol, will contain again 23～35mLTi (OBu) 4Ethanolic solution under vigorous stirring, join in the above-mentioned colloidal sol, continue vigorous stirring until form till the gel, still aging, 500～700 ℃ of temperature lower calcination 1～2h get final product product.In addition, with synthetic CuCr 2O 4With the P25 TiO that buys 2Repeatedly mixed grinding, roasting compare experiment with solid-phase synthesis.
The present invention has carried out relevant characterization to the photochemical catalyst of 500 ℃ of lower roastings, the detection of transmission electron microscope as can be known, the composite photo-catalyst pattern is irregular, particle diameter is inhomogeneous, that particle is bigger is CuCr 2O 4, be the thinner TiO of particle on its surface 2Coat, form the structure of a similar nuclear-shell.This surface texture adsorbs environment and light-catalyzed reaction place preferably for reaction provides.XRD detects and shows CuCr 2O 4/ TiO 2The diffraction maximum of compound is by the sharp stone type of crystalline substance CuCr 2O 4With Detitanium-ore-type TiO 2(contain＜5% Rutile Type), both diffraction maximums formed, and no cenotype occurs, and illustrates that both composite effects are better, does not cause the separately variation of bulk structure, the about 60～80nm of average grain diameter.
The present invention has tested prepared composite Nano photochemical catalyst to colibacillary killing action with three kinds of forms, under the excited by visible light, and CuCr in the aqueous solution and the experiment of filming 2O 4, TiO 2And CuCr 2O 4-TiO 2All show certain bactericidal activity, and active order is CuCr 2O 4＜TiO 2＜CuCr 2O 4-TiO 2Studied the optimum calcination temperature of sample, copper chromate and titanium dioxide best complex amount, Different Light conditions etc. are to the impact of photo-catalyst performance.Because best sintering temperature can make catalysis material have the specific area of the most rational crystal structure and appropriateness; Suitable compound ratio can make photochemical catalyst appropriate lattice deformability and defective occur becomes light induced electron or hole trap, stops right compound in light induced electron-hole, improves photo-quantum efficiency.
The present invention is to Cu Cr 2O 4-TiO 2Composite photo-catalyst kills performance and has carried out respectively the experiment of filming of suspension, ceramic tile and glued board, and concrete experimentation is as follows:
Bacteria Culture: from seed culture fluid, draw the 2mL bacterial solution and join in the beef extract-peptone fluid nutrient medium of fresh sterilization, 37 ℃, shaken cultivation is to exponential phase under the 170r/min condition, (in the following experiment, used bacterium is the bacterium of exponential phase), survey its absorbance, according to OD value and bacterial concentration relation, regulate bacterial concentration with aseptic PBS solution (potassium dihydrogen phosphate 0.012mol/L, sodium hydrogen phosphate 0.055mol/L).
(1) sterilization experiment in the suspension: getting a certain amount of composite photo-catalyst by citric acid assisting sol-gel method preparation (does not have when special instruction, employed composite photo-catalyst all is this catalyst) under aseptic condition, place the reaction vessel of about 500mL distilled water, ultrasonic dispersion 10min, the inoculum and the distilled water that add aequum again, regulating bacterial suspension with aseptic PBS solution is required bacterial concentration, reactant liquor is positioned in the Photoreactor, electromagnetic agitation 15min in the dark, sampling 1mL.Open the 150W xenon lamp, under the room temperature magnetic agitation, begin sterilization experiment.In 60min, get the 1mL bacterial suspension respectively according to the viable bacteria notation and in the light-shading bottle that the 9mL SPSS is housed, dilute 10 times (sample is handled together before the reaction) every 10min, getting 100 μ L bacterium liquid again from the bacteria suspension after the dilution is applied in the culture dish that beef-protein medium is housed, three culture dishes of each coating carry out parallel laboratory test, and the data that obtain are averaged.Place 37 ℃ of lucifuge constant incubators cultivations after 16 hours in coated culture dish, bacterium colony is counted.Do simultaneously dark control experiment and catalyst-free blank assay.
(2) the ceramic tile sterilization experiment of filming: the composite photo-catalyst colloidal sol of lemon acid assisting sol-gel method preparation is applied to certain area (50cm by extraction (more than twice) 2) ceramic tile surface, in the uniform temperature roasting, obtain to contain the antibiotic ceramic tile of this photocatalytic coating.With the antibiotic ceramic tile sample disinfection that obtains, the PBS buffer solution of finite concentration bacterium evenly is applied to antibiotic ceramic tile surface, put into the bacterium of aseptic culture dish after covering with antistaling film immediately with secluding air, the subtraction water evaporates, use again on the black lucifuge sack cover, put together to the 150w xenon lamp after all being coated with, the distance of regulating each ceramic tile and xenon lamp is taken away lucifuge and is carried out the photo-catalyst experiment with sack to remain on same intensity of illumination (apart from the about 30cm of light source).Take out a ceramic tile every 10min, with the flushing of 50mL SPSS.With the physiological saline mixing that washes, draw 100 μ L spread plates with liquid-transfering gun, be coated with three flat boards at every turn.After placing 37 ℃ of lucifuge constant incubators to cultivate 16h the coated flat board, bacterium colony is counted, got the empirical average value.Do the sunshine sterilization experiment with same procedure, weather conditions are: between afternoon in the autumn in the north, Hunan (October) the 1-4 point, the sunshine average illumination is 6.9 * 10 4Lx.Do simultaneously dark control experiment and the catalyst-free blank assay compares.
(3) the glued board sterilization experiment of filming: get and a certain amount ofly prepare and add in the coating at the temperature required nano composite photo-catalyst of roasting down, stir, make that photochemical catalyst reaches certain content in the coating, and this coating is applied to certain area (50cm uniformly 2) plywood facing, the glued board that scribbles photocatalysis antibacterial coating is placed 50 ℃ of dry 3h of baking oven.And with the disinfection of antibiotic glued board sample, the PBS buffer solution of finite concentration bacterium evenly is applied to antibiotic face veneer, put into the bacterium of aseptic culture dish after covering with antistaling film immediately with secluding air, the subtraction water evaporates, use again on the black lucifuge sack cover, put together to the 150w xenon lamp after all being coated with, the distance of regulating each glued board and xenon lamp is taken away lucifuge and is carried out the photo-catalyst experiment with sack to remain on same intensity of illumination (apart from the about 30cm of light source).Take out a glued board every 10min, with the flushing of 50mL SPSS.With the physiological saline mixing that washes, draw 100 μ L spread plates with liquid-transfering gun, be coated with three flat boards at every turn.After placing 37 ℃ of lucifuge constant incubators to cultivate 16h the coated flat board, bacterium colony is counted, got the empirical average value.Also do the sunshine sterilization experiment with same procedure, weather conditions are the same.Do simultaneously dark control experiment and the catalyst-free blank assay compares.
The specific embodiment
Embodiment 1
Take by weighing respectively the CuCr of 500～600 ℃ of lower roastings 2O 4And TiO 2Being mixed with concentration is 10 4The Escherichia coli suspension of CFU/mL, the concentration that makes photochemical catalyst are 1.0～3.0 μ g/mL, carry out the photo-catalyst experiment by above-mentioned experimentation.Carry out the blank assay of control experiment and catalyst-free under the same terms in the dark.Experiment shows: in the 30min, and CuCr 2O 4Sterilizing rate is 71.2%, TiO 2Sterilizing rate is 80.8%, and has in the dark the control experiment of catalyst almost not have bactericidal effect, and the blank assay sterilizing rate of catalyst-free is less than 5% under illumination.By above-mentioned experimentation, after 1～3 lixiviate processing, at 500～600 ℃ of lower roasting 1～3h, obtain to contain respectively CuCr 2O 4And TiO 2Antibiotic ceramic tile, be 10 with concentration 5The Escherichia coli solution 1mL of CFU/mL, with spreading rod be uniformly coated on ceramic tile, face veneer carries out sterilization experiment, behind the 30min, sterilizing rate is respectively 68.9% and 75.8%.The nanometer CuCr for preparing 500～600 ℃ of lower roastings will be added respectively in commercial (production of the gloomy king's coating in Foshan City Co., Ltd) 2O 4And TiO 2, fully stir, making the photochemical catalyst quality is 1～5%, is 10 with concentration 5The Escherichia coli solution 1mL of CFU/mL evenly is coated with ceramic tile, plywood facing with spreading rod.Behind the 30min, sterilizing rate is respectively 63.6% and 70.5%.Carry out sterilization experiment under the sunshine by aforesaid method under the same conditions, the sterilizing rate of ceramic tile, plywood facing is respectively 54.6% and 60.8% behind the 30min.Carry out in the dark under the same terms ceramic tile and glued board the contrast sterilization experiment almost do not have bactericidal effect, the catalyst-free blank assay in 30min sterilizing rate less than 5%.
Embodiment 2
Take by weighing TiO 2Be 70% composite Nano CuCr 2O 4-TiO 2It is 10 that sample ligand is made concentration 4The Escherichia coli suspension of CFU/mL, the concentration of photochemical catalyst are 1.0～3.0 μ g/mL, carry out photocatalysis suspension sterilization experiment by embodiment 1, and the sterilizing rate behind the 30min is 92.2%.Carrying out ceramic tile, face veneer sterilization experiment with this composite photo-catalyst by embodiment 1, is that the Escherichia coli solution of 105CFU/mL experimentizes by embodiment 1 with concentration, and behind the 30min, sterilizing rate is respectively 91.4% and 86.6%.Sterilization experiment under the sunshine under the same terms, behind the 30min, sterilizing rate is respectively 90.1% and 83.6%.Come to the same thing among control experiment under the same terms and blank assay and the embodiment 1.
Embodiment 3
Take by weighing TiO 2Be 80% composite Nano CuCr 2O 4-TiO 2It is 10 that sample ligand is made concentration 4The Escherichia coli suspension of CFU/mL, the concentration of photochemical catalyst are 1.0～3.0 μ g/mL, carry out photocatalysis suspension sterilization experiment by embodiment 1, and the sterilizing rate of 30min is 100%.With this composite Nano CuCr 2O 4-TiO 2Carrying out ceramic tile, face veneer sterilization experiment, is 10 with concentration 5The Escherichia coli solution of CFU/mL is undertaken by embodiment 1, and behind the 30min, sterilizing rate is respectively 96.1% and 93.9%.Sterilization experiment under the sunshine under the same terms, behind the 30min, sterilizing rate is respectively 92.5% and 86.9%.Come to the same thing among control experiment under the same terms and blank assay and the embodiment 1.
Embodiment 4
Take by weighing TiO 2Be 90% composite Nano CuCr 2O 4-TiO 2It is 10 that sample ligand is made concentration 4The Escherichia coli suspension of CFU/mL, the concentration of photochemical catalyst are 1.0～3.0 μ g/mL, carry out photocatalysis suspension sterilization experiment by embodiment 1, and the sterilizing rate of 30min is 94.0%.With this composite Nano CuCr 2O 4-TiO 2Carrying out ceramic tile, face veneer sterilization experiment, is 10 with concentration 5The Escherichia coli solution of CFU/mL is undertaken by embodiment 1, and behind the 30min, sterilizing rate is respectively 92.4% and 87.8%.Sterilization experiment under the sunshine under the same terms, behind the 30min, sterilizing rate is respectively 90.1% and 83.0%.Come to the same thing among control experiment under the same terms and blank assay and the embodiment 1.

Claims (5)

1. a visible light has the nano composite photo-catalyst of response as preparation and the application of photo-catalyst antiseptic, and the chemical composition that it is characterized in that this composite photo-catalyst is CuCr 2O 4-TiO 2
2. CuCr as claimed in claim 1 2O 4-TiO 2The composite photo-catalyst preparation method the steps include:
(1) with 0.003～0.005mol Cu (NO 3) 2With 0.006～0.01mol Cr (NO 3) 2Be dissolved in 30～50mL deionized water, under 80 ℃ of stirred in water bath, dropwise add in gained solution subsequently in the citric acid solution of 80～100ml0.3M and obtain vitreosol;
(2) will contain 23～35mL Ti (OBu) 4Ethanolic solution under vigorous stirring, be added dropwise in step (1) colloidal sol, continue to stir till forming gel;
(3) gel that step (2) is obtained is still aging, 500～700 ℃ of temperature lower calcination 1～2h get final product products C uCr 2O 4-TiO 2
3. according to composite photo-catalyst described in the claim 1, it is characterized in that: copper chromate is 1～3: 9～7 (mass ratioes) with titanium dioxide best complex ratio;
4. according to composite photo-catalyst described in the claim 1, it is characterized in that: copper chromate belongs to the sharp stone structure of the semi-conductive crystalline substance of p type, it is semi-conductive anatase structured that titanium dioxide belongs to the n type, contains the rutile structure of a small amount of (molal quantity is less than 5%), the about 60～80nm of average grain diameter;
5. according to composite photo-catalyst described in the claim 1, under various radiation of visible light to the killing actions of various bacteriums such as large intestine sense bacterium.
CN 201010609018 2010-12-28 2010-12-28 Preparation and application of composite photo-catalysis bactericide for visible light response Pending CN102085481A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102423709A (en) * 2011-10-19 2012-04-25 河北工业大学 N-p heterogeneous composite photocatalyst and preparation method and application thereof
CN107384616A (en) * 2017-07-18 2017-11-24 舟山达康科技有限公司 A kind of antifouling anti-aging leather shoes care agent
CN108839144A (en) * 2018-08-29 2018-11-20 含山县金中环装饰材料有限公司 A kind of preparation method of fire-retardant mould proof glued board
CN111250134A (en) * 2020-02-14 2020-06-09 郑州普利飞尔环保科技有限公司 Modified TiO2Composite g-C3N4Visible light photocatalytic antibacterial ceramic and preparation method and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《Proceedings of 2010 First International Conference onCellular; Molecular Biology; Biophysics and Bioengineering》 20101225 Li Zhang et al Photocatalytic Inactivation of the Bacteria Escherichia coli by CuCr2O4/TiO2 Composite Photocatalysts under Simulated Solar Light Irradiation 第547至549页 1,3,5 第1卷, *
《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 20100415 杨海华 尖晶石型CuM_2O_4(M=Fe,Co,Cr)的制备及光催化产氢活性的研究 第45至55页 2,4 第2010年卷, 第04期 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102423709A (en) * 2011-10-19 2012-04-25 河北工业大学 N-p heterogeneous composite photocatalyst and preparation method and application thereof
CN102423709B (en) * 2011-10-19 2014-05-07 河北工业大学 N-p heterogeneous composite photocatalyst and preparation method and application thereof
CN107384616A (en) * 2017-07-18 2017-11-24 舟山达康科技有限公司 A kind of antifouling anti-aging leather shoes care agent
CN108839144A (en) * 2018-08-29 2018-11-20 含山县金中环装饰材料有限公司 A kind of preparation method of fire-retardant mould proof glued board
CN111250134A (en) * 2020-02-14 2020-06-09 郑州普利飞尔环保科技有限公司 Modified TiO2Composite g-C3N4Visible light photocatalytic antibacterial ceramic and preparation method and application thereof

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Application publication date: 20110608