CN104001537A - Method for improving visible-light catalytic activity and antibacterial performance of TiO2/diatomite composite material - Google Patents
Method for improving visible-light catalytic activity and antibacterial performance of TiO2/diatomite composite material Download PDFInfo
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- CN104001537A CN104001537A CN201410270737.5A CN201410270737A CN104001537A CN 104001537 A CN104001537 A CN 104001537A CN 201410270737 A CN201410270737 A CN 201410270737A CN 104001537 A CN104001537 A CN 104001537A
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Abstract
The invention relates to a method for improving the visible-light catalytic activity and antibacterial performance of a TiO2/diatomite composite material. The method includes the steps of firstly, stirring and soaking the prepared TiO2/diatomite composite material in a urea (CO(NH2)2) and silver nitrate (AgNO3) solution with the certain concentration, drying a sample after conducting the soaking reaction for a certain period of time, and obtaining a TiO2/diatomite composite material urea and solver nitrate soaking composite product; secondly, roasting the soaked product at the certain temperature, conducting scattering and depolymerization after cooing, and obtaining the N-TiO2/diatomite silver-carried composite material with the visible-light catalytic activity and antibacterial performance. The method of directly soaking the TiO2/diatomite composite material in the urea and silver nitrate solution is adopted, no other reagents need to be added in the whole process, a large volume of waste water is prevented from being produced in the preparation process, the method has the advantages of being easy and convenient to implement, efficient and clean, and the composite material has a wide visible-light response range and antibacterial performance. The N-TiO2/diatomite silver-carried composite material, prepared through the method, with the visible-light catalytic activity and antibacterial performance can be used for the technical field of indoor environmental pollution purification.
Description
Technical field
The present invention relates to improve TiO
2the method of/diatomite composite material visible light catalysis activity and anti-microbial property, belongs to nonmetallic mineral material preparation, environmental pollution purification techniques field.
Background technology
TiO
2as a kind of catalysis material of efficient, nontoxic and stable chemical nature, under UV-irradiation, the common pollutants such as toluene, phenol, formaldehyde and dyestuff, can be at TiO
2the catalyzed degraded in surface.For improving TiO
2photocatalytic activity, common TiO
2expectation is made into ultra-fine, nano particle, but ultra-fine, nano-TiO
2complicated process of preparation, and exist and easily reunite, reclaim difficult shortcoming in actual use.In recent years, adopt fixedly TiO of the carriers such as diatomite, active carbon, silica gel, zeolite, bentonite, glass and nickel foam
2, can disperse preferably and reclaim ultra-fine, nano-TiO
2, become TiO
2composite photocatalyst material study hotspot.
Diatomite is a kind of natural porous non-metallic mineral material, has that specific surface is large, adsorptivity is strong and the feature of stable in properties, about TiO
2the preparation technology of/diatomite composite material, existing a lot of pertinent literature reports, are mainly to adopt diatomite to make carrier, by technical process such as hydrolytic precipitation method, sol-gal process and hydro-thermal methods, by TiO
2form with hydrated titanium dioxide, titanium hydroxide is fixed on diatomite for the preparation of TiO
2/ diatomite composite material, is shown in below with reference to document: 1. Chinese invention patent " the loaded nano TiO that the super-cell of take is carrier
2the preparation method of catalysis material ", application number: CN200910235208.0, applicant: China Mining Univ. (Beijing); 2. Wang Lijian etc., the preparation of Titania/diatomite Composite, silicate journal, 2006,34 (7); 3. " a kind of sol-gel process is prepared TiO to Chinese invention patent
2the method of/diatomite composite photocatalytic material ", application number: CN201310117399.7, applicant: Kunming University of Science and Technology; 4. just cultivate etc., hydro-thermal method is prepared TiO
2-diatomite composite material and photocatalysis performance thereof, functional material and device journal, 2010,16 (1).Based on TiO
2strong absorption and the Photocatalytic Degradation Property of/diatomite composite material, now by its Application and Development in the environmental friendly indoor building materials such as wallpaper, coating, shutter and timber floor, the volatile harmful gases such as the common toluene of degraded indoor environment, formaldehyde.Yet, TiO
2there is higher energy gap, Detitanium-ore-type TiO
2energy gap be 3.2eV, can only absorbing wavelength be less than the ultraviolet light of 390nm, and ultraviolet light proportion in sunshine very little (being less than 5%), for utilizing preferably indoor light source and sunshine, exploitation has the TiO of visible light catalysis activity
2/ diatomite composite material is significant.
In recent years, people adopt various method of modifying, as element (metal, nonmetal, rare earth) adulterates, semiconductor is compound, dye sensitization etc. attempts to improve TiO
2visible light catalysis activity, wherein N element doping TiO
2show excellent photocatalysis performance, have good application potential.Through searching document, find, 5. Chinese invention patent name is called " a kind of tripolite loading nitrogen-doped nanometer TiO
2the preparation method of catalysis material ", application number is: CN201210205768.3, this patent discloses a kind of high-temperature heat treatment of carrying out in nitrogen, prepares tripolite loading nitrogen-doped nanometer TiO
2the method of catalysis material, there is the shortcoming that nitrogen circulation consumption is large, equipment requirement is high in the method; 6. Chinese invention patent name is called and " a kind ofly take the visible light-responded TiO that diatomite is matrix
2the preparation method of mixed crystal ", application number is: CN200810156050.3, this patent discloses a kind of employing and prepared TiO
2mixed crystal improves with TiO
2-diatomaceous visible light-responded, do not relate to element doping.In addition, due to indoor be the mankind's main life, workplace, be accompanied by the mankind's daily life activity, inevitably can produce some bacteriums, harm humans is healthy, and metal element A g, Cu, Zn etc. show anti-microbial property, wherein the anti-microbial property of Ag is the most outstanding, and silver can be at TiO
2surface can form active sites, is conducive to stop TiO
2surface light induced electron and hole compound, improves TiO greatly
2photocatalytic activity, 7. Chinese invention patent name is called " method of Diatomite-based Porous Ceramics and loading Ag doped with nano TiO 2 thereof ", application number is: CN201010216099.0, this patent discloses a kind ofly decomposes by ultraviolet catalytic silver nitrate, carry out the method for loading Ag doped with nano TiO 2, the method exists silver carrying amount to be difficult to control, easily cause loss, the influence factor of noble silver many and be difficult to realize the shortcoming of suitability for industrialized production, and this product visible light catalysis activity a little less than.
For current TiO
2the shortcoming that/diatomite composite material visible light catalysis activity is low and antibacterial effect is poor, the invention provides and improve TiO
2the method of/diatomite composite material visible light catalysis activity and anti-microbial property.
Summary of the invention
Technical scheme of the present invention is: by the TiO of preparation
2/ diatomite composite material is at pre-configured certain density urea (CO (NH
2)
2) and silver nitrate (AgNO
3) stir dipping in solution, after impregnation certain hour, sample is dried, obtain TiO
2/ diatomite composite material dipping urea, silver nitrate combination product; This impregnation product is calcined at a certain temperature, after calcined product is cooling, break up depolymerization, obtain having the N-TiO of visible light catalysis activity and anti-microbial property
2/ diatomite carries silver composite material product.
Its processing step is as follows:
(1) press TiO
2/ diatomite composite material: urea: the quality proportioning of silver nitrate is 1:(0.08 ~ 1): (0.001 ~ 0.04), takes a certain amount of TiO
2/ diatomite composite material, urea (CO (NH
2)
2) and silver nitrate (AgNO
3), urea and silver nitrate are dissolved in to the aqueous solution that clear water is made into urea and silver nitrate mass concentration 10% ~ 30%;
(2) by TiO
2/ diatomite composite material is scattered in the mixed solution of urea and silver nitrate, stirs dipping 0.5 ~ 2h under normal temperature;
(3) sample after dipping is transferred in evaporimeter or freeze-dryer, at 50 ~ 90 ℃ dry or-10 ~-30 ℃ at freeze drying;
(4) desciccate is placed in to calcining furnace, at 350 ~ 550 ℃ of temperature, calcining 1 ~ 5h;
(5) break up depolymerization after calcined product is cooled to room temperature, obtain having the N-TiO of visible light catalysis activity and anti-microbial property
2/ diatomite carries silver composite material.
The prepared N-TiO with visible light catalysis activity and anti-microbial property
2/ diatomite carries that silver composite material can be used for the contaminative VOCs such as indoor formaldehyde, toluene and benzene degraded and anti-bacteria grows.
This method adopts the method for direct impregnation load in urea and liquor argenti nitratis ophthalmicus, whole process is added without other reagent, avoided producing a large amount of waste water in preparation process, had advantages of easy, efficient, cleanly, and composite has wider visible light-responded scope and anti-microbial property.The N-TiO with visible light catalysis activity and anti-microbial property prepared by the present invention
2/ diatomite carries silver composite material and can be used for indoor environmental pollution purification techniques field.
Accompanying drawing explanation
Fig. 1 is the N-TiO with visible light catalysis activity and anti-microbial property of the specific embodiment of the invention one preparation
2/ diatomite carries silver composite material and TiO
2the ultraviolet-visible absorption spectroscopy of/diatomite composite material (UV-Vis) comparison diagram, N-TiO of the present invention
2/ diatomite carry silver composite material within the scope of visible ray 390 ~ 500nm compared with general T iO
2/ diatomite composite material absorbance significantly promotes, and shows obvious visible light catalysis activity.
Fig. 2 is the N-TiO with visible light catalysis activity and anti-microbial property of the specific embodiment of the invention one preparation
2/ diatomite carries the TEM figure of silver composite material.
The specific embodiment
Embodiment mono-: (1) takes respectively TiO
2/ diatomite composite material 10g, urea 3g, silver nitrate 0.01g, and urea and silver nitrate are dissolved in 10ml water to obtain to solution A, then by TiO
2/ diatomite composite material is scattered in solution A, is placed in normal temperature and stirs dipping 0.5h.
(2) sample after dipping is transferred in rotary evaporator, at 70 ℃ of Rotary dryings.
(3) dried sample is placed in to calcining furnace, at 400 ℃ of temperature, calcining 2h.Calcined product is cooled to room temperature, is ground into after powder, obtain having the N-TiO of visible light catalysis activity and anti-microbial property
2/ diatomite carries silver composite material product.
Embodiment bis-: (1) takes respectively TiO
2/ diatomite composite material 10g, urea 2g, silver nitrate 0.05g, and urea and silver nitrate are dissolved in 10ml water to obtain to solution B, then by TiO
2/ diatomite composite material is scattered in solution B, is placed in normal temperature and stirs dipping 1h.
(2) sample after dipping is transferred in rotary evaporator, at 75 ℃ of Rotary dryings.
(3) dried sample is placed in to calcining kiln, at 450 ℃ of temperature, calcining 3h.Calcined product is cooled to room temperature, after breaing up, obtains having the N-TiO of visible light catalysis activity and anti-microbial property
2/ diatomite carries silver composite material product.
Embodiment tri-: (1) takes respectively TiO
2/ diatomite composite material 10g, urea 4g, silver nitrate 0.15g, and urea and silver nitrate are dissolved in 25ml water to obtain to solution C, then by TiO
2/ diatomite composite material is scattered in solution C, is placed in normal temperature and stirs dipping 1h.
(2) sample after dipping is transferred in freeze-dryer to freeze drying.
(3) dried sample is placed in to calcining kiln, at 420 ℃ of temperature, calcining 5h.Calcined product is cooled to room temperature, after breaing up, obtains having the N-TiO of visible light catalysis activity and anti-microbial property
2/ diatomite carries silver composite material product.
Effect experiment: (1) visible light catalysis activity experiment: at 1m
3environmental chamber in to regulate initial concentration of formaldehyde be 10mg/m
3, take the N-TiO with visible light catalysis activity and anti-microbial property preparing in 10g embodiment
2/ diatomite carries silver composite material and is evenly coated on glass plate, adopts 20W daylight lamp as light source Continuous irradiation 48h, carries out formaldehyde degradation by photocatalytic oxidation process experiment, and carries out general T iO under the same conditions
2/ diatomite composite material contrast experiment, experimental result is as shown in table 1.
(2) anti-microbial property experiment: take staphylococcus aureus as experimental strain with reference to < < nano inorganic material anti-microbial property detection method > > (GB/T 21510-2008), adopt the anti-microbial property of colony counting method test sample, test respectively general T iO
2the N-TiO with visible light catalysis activity and anti-microbial property preparing in/diatomite composite material and embodiment
2/ diatomite carries the anti-microbial property of silver composite material, and experimental result is as shown in table 1.
The detection analysis result of table 1 embodiment sample
Claims (1)
1. improve the method for TiO2/ diatomite composite material visible light catalysis activity and anti-microbial property, it is characterized in that significantly promoting the absorbance of composite within the scope of visible ray 390 ~ 500nm, and have anti-microbial property, its processing step is as follows:
(1) by TiO2/ diatomite composite material: urea: the quality proportioning of silver nitrate is 1:(0.08 ~ 1): (0.001 ~ 0.04), take a certain amount of TiO2/ diatomite composite material, urea (CO (NH2) 2) and silver nitrate (AgNO3), urea and silver nitrate are dissolved in to the aqueous solution that clear water is made into urea and silver nitrate mass concentration 10%30%;
(2) TiO2/ diatomite composite material is scattered in the mixed solution of urea and silver nitrate, under normal temperature, stirs dipping 0.5 ~ 2h;
(3) sample after dipping is transferred in evaporimeter or freeze-dryer, at 50 ~ 90 ℃ dry or-10 ~-30 ℃ at freeze drying;
(4) desciccate is placed in to calcining furnace, at 350 ~ 550 ℃ of temperature, calcining 1 ~ 5h;
(5) break up depolymerization after calcined product is cooled to room temperature, the N-TiO2/ diatomite that obtains having visible light catalysis activity and anti-microbial property carries silver composite material.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105211103A (en) * | 2015-10-22 | 2016-01-06 | 苏州科大微龙农业科技有限公司 | The green compound control agent of a kind of control two spotted spider mite |
| CN106334396A (en) * | 2016-09-24 | 2017-01-18 | 上海大学 | Method capable of inhibiting formation of NBaP in atmospheric particulates |
| CN106984306A (en) * | 2017-04-28 | 2017-07-28 | 成都理工大学 | One kind has antibacterial and the difunctional surrounding purifying material of photocatalysis and preparation method thereof |
| CN107162546A (en) * | 2017-07-13 | 2017-09-15 | 江苏新大乘环保科技有限公司 | A kind of diatom plate with antibacterial functions and preparation method thereof |
| CN108244145A (en) * | 2018-02-07 | 2018-07-06 | 广州市凯卫莎环保科技有限公司 | Triple effect all-weather light catalyst indoor air purification agent and preparation method and application |
| CN108940339A (en) * | 2018-07-12 | 2018-12-07 | 浙江正洁环境科技有限公司 | A kind of N-TiO2/ calcium system bentonite composite adsorption catalyst and application |
| CN109046340A (en) * | 2018-08-21 | 2018-12-21 | 中科广化（重庆）新材料研究院有限公司 | Modified visible light catalytic material in a kind of surface and its preparation method and application |
| CN109806765A (en) * | 2019-03-26 | 2019-05-28 | 中国建筑材料科学研究总院有限公司 | Composite material for air cleaning and preparation method thereof |
| CN111974156A (en) * | 2019-05-24 | 2020-11-24 | 宁夏大学 | Preparation method of scavenger for efficiently degrading gaseous pollutants |
| CN113383793A (en) * | 2021-07-15 | 2021-09-14 | 曲靖师范学院 | Cu/TiO2/diatom ooze composite antibacterial material, preparation method and application thereof |
| CN115039791A (en) * | 2022-07-13 | 2022-09-13 | 塔里木大学 | Vermiculite antibacterial functional material and preparation method thereof |
-
2014
- 2014-06-18 CN CN201410270737.5A patent/CN104001537B/en active Active
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| PINGGUI WU ET AL.: "Visible-Light-Induced Bactericidal Activity of Titanium Dioxide Codoped with Nitrogen and Silver", 《ENVIRON. SCI. TECHNOL.》, vol. 44, no. 18, 20 August 2010 (2010-08-20), pages 6992 * |
| 危琼辉等: "TiO2-X NX/硅藻土复合光催化剂的制备及其可见光催化剂活性", 《西南科技大学学报》, vol. 26, no. 2, 30 June 2011 (2011-06-30) * |
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Cited By (14)
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| CN105211103A (en) * | 2015-10-22 | 2016-01-06 | 苏州科大微龙农业科技有限公司 | The green compound control agent of a kind of control two spotted spider mite |
| CN106334396A (en) * | 2016-09-24 | 2017-01-18 | 上海大学 | Method capable of inhibiting formation of NBaP in atmospheric particulates |
| CN106984306B (en) * | 2017-04-28 | 2019-08-06 | 成都理工大学 | One kind having antibacterial and the difunctional surrounding purifying material of photocatalysis and preparation method thereof |
| CN106984306A (en) * | 2017-04-28 | 2017-07-28 | 成都理工大学 | One kind has antibacterial and the difunctional surrounding purifying material of photocatalysis and preparation method thereof |
| CN107162546A (en) * | 2017-07-13 | 2017-09-15 | 江苏新大乘环保科技有限公司 | A kind of diatom plate with antibacterial functions and preparation method thereof |
| CN108244145A (en) * | 2018-02-07 | 2018-07-06 | 广州市凯卫莎环保科技有限公司 | Triple effect all-weather light catalyst indoor air purification agent and preparation method and application |
| CN108940339A (en) * | 2018-07-12 | 2018-12-07 | 浙江正洁环境科技有限公司 | A kind of N-TiO2/ calcium system bentonite composite adsorption catalyst and application |
| CN109046340A (en) * | 2018-08-21 | 2018-12-21 | 中科广化（重庆）新材料研究院有限公司 | Modified visible light catalytic material in a kind of surface and its preparation method and application |
| CN109046340B (en) * | 2018-08-21 | 2021-09-24 | 中科广化（重庆）新材料研究院有限公司 | Surface-modified visible light catalytic material and preparation method and application thereof |
| CN109806765A (en) * | 2019-03-26 | 2019-05-28 | 中国建筑材料科学研究总院有限公司 | Composite material for air cleaning and preparation method thereof |
| CN109806765B (en) * | 2019-03-26 | 2021-12-07 | 中国建筑材料科学研究总院有限公司 | Air purification composite material and preparation method thereof |
| CN111974156A (en) * | 2019-05-24 | 2020-11-24 | 宁夏大学 | Preparation method of scavenger for efficiently degrading gaseous pollutants |
| CN113383793A (en) * | 2021-07-15 | 2021-09-14 | 曲靖师范学院 | Cu/TiO2/diatom ooze composite antibacterial material, preparation method and application thereof |
| CN115039791A (en) * | 2022-07-13 | 2022-09-13 | 塔里木大学 | Vermiculite antibacterial functional material and preparation method thereof |
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| CN104001537B (en) | 2016-02-17 |
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