CN101773820B - Method for preparing visible light active photocatalyst through dye sensitization - Google Patents
Method for preparing visible light active photocatalyst through dye sensitization Download PDFInfo
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- CN101773820B CN101773820B CN 200910226766 CN200910226766A CN101773820B CN 101773820 B CN101773820 B CN 101773820B CN 200910226766 CN200910226766 CN 200910226766 CN 200910226766 A CN200910226766 A CN 200910226766A CN 101773820 B CN101773820 B CN 101773820B
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Abstract
The invention provides a method for preparing visible light active photocatalyst through dye sensitization. The method comprises the following steps that: (1) industrial grade titanium sulfate is taken as the main raw material, alkali liquid is taken as precipitant and hydrated titanium dioxide sediment is obtained through reaction; (2) deionized water is taken as dialysate, and SO4- and other ions in gel are removed by adopting electrodialysis method; (3) the concentration of Ti4+ is determined by adopting spectrophotometry and 0.1M turbid liquid is prepared, H2O2 of certain proportion is slowly dropped under the condition of agitation and the obtained sol is aged for more than 24h; and (4) dye photosensitizer or precious metal salt is added into the sol according to certain proportion, hydro-thermal reaction is taken place for 4-12 under 60-100 DEG C, and high-concentration and high-stability photocatalyst product with visible light activity is obtained. The photocatalyst preparation method of the invention has the advantages that anatase phase nano titanium dioxide particles can be synthesized without requiring high-temperature heat treatment, the dimension of the anatase phase nano titanium dioxide particles can be controlled to be about 10nm, the dispersion degree of the obtained sol is good, the visible light activity and the sterilization performance are greatly improved through the dye sensitization and precious metal surface deposition technology, the synthesis technology is simple, the raw materials and the device are low in price and can be obtained easily, and the method is very suitable for industrial mass production.
Description
Technical field
The present invention relates to nano material preparation and application, specifically, relate to a kind of method of preparing visible light active photocatalyst through dye sensitization.
Background technology
The nano titanium dioxide photocatalysis technique functions comes from the seventies in 20th century, and obtains in recent years using comparatively widely.This technology is carried out at normal temperatures and pressures; Receive the optical excitation of suitable intensity and wavelength as long as guarantee photochemical catalyst, just being enough to the nearly all organic pollution of oxidative degradation and making it mineralising is harmless material, can not produce secondary pollution; And energy consumption is low; Therefore cost is low, is widely used in depollution of environment field, especially has significant advantage aspect the purification of drinking water and room air and the sterilization.
The nano-TiO that will have photocatalytic activity
2The hydrosol is sprayed at matrix or carrier surface, forms fine and close, mushy nano-TiO
2Film, thus its photochemical catalytic oxidation function of performance is a kind of efficient ways in the present photocatalyst actual application under ultraviolet light or visible light condition.The preparation nano-TiO
2The method of the hydrosol has a lot, and wherein the simplest method is with the nano-TiO for preparing
2Powder adds dispersant and is distributed in the water, but this method is easy to cause reunion, is difficult to guarantee nano-TiO
2The high dispersion of powder in the aqueous solution, and the part dispersant also can change the chemical property of colloidal sol, and matrix is produced corrosion even causes secondary pollution.The preparation nano-TiO
2Other a kind of method commonly used of the hydrosol is a sol-gel process, and promptly the organic matter (like butyl titanate, tetraethyl titanate) through titaniferous is hydrolyzed in acid, alkali or alcoholic solution and synthesizes TiO
2Colloidal sol.Patent CN1224036A, 00109176.X all adopt this method to prepare the TiO of various performances
2Colloidal sol, but this method is raw material with the organic titanium, industrial production cost is high, and prepared colloidal sol needs high-temperature heat treatment just to have good photocatalysis performance after being coated with into film, thereby has limited its practical application.
The preparation nano-TiO
2The third method of the hydrosol is a peptisation, is raw material with inorganic matter (titanium tetrachloride, titanium sulfate) promptly, heats or add alkali to make it hydrolysis or deposition, and with adding sour peptization after the washing of precipitate, crystallization obtains nano-TiO at a certain temperature
2Colloidal sol.Because this method synthesis temperature is low, technology is simple, equipment investment is little, do not need the later stage high-temperature heat treatment just can obtain well-crystallized's anatase type nano TiO
2Colloidal sol is prone to realize suitability for industrialized production, is the preparation nano-TiO
2Perfect method.Patent CN1583888A is raw material with the titanyl nitrate, through 70～109 ℃ of hydrolysis or add inorganic base deposition, contains TiO with being distributed to again after the washing of precipitate to process in the water
20.1 the photo-catalytic coating of～31% mass percentage concentration, but this method need adopt modes such as ultrasonic dispersion, mulser dispersion, sand mill dispersion to disperse again.Patent CN100396372C is with TiSO
4NH
2The O clear solution adds alkali and stirs washing again after the ageing, adds the oxidant peptization, and leaving standstill behind the 24-30h in autoclave pressure heat treatment, can to obtain length be 100nm, and particle diameter is the needle-like photocatalysis coating liquid of 20nm, but this method has increased the requirement to consersion unit.
Peptisation generally is divided into deposition, washing, peptization and four processes of crystallization, and wherein washing is a very critical step, and it will directly influence the TiO of preparation
2The dispersiveness of the hydrosol and stable.The method of washing comprises filtration, centrifugal, ion-exchange, extraction etc.; That CN101580276A, Japan Patent JP10-158015 and CN1834020A adopt respectively is centrifugal, the mode of ion-exchange and extraction has been carried out purifying to deposition, but all there is defective in above-mentioned washing methods.Big and the inefficiency of filtration method water consumption, less employing; Centrifugation is all bigger to the loss of the consumption of water and titanium; Ion-exchange is inappropriate for the ion in the solution of removing high concentration.
Simultaneously, improving photocatalyst photocatalytic activity under the visible light condition also is one of focus of paying close attention to of people.Patents such as CN1769184A, CN101049961A, CN1654335A, CN1583252A have prepared TiO through modes such as transition metal and rear-earth-doped, noble metal loadings
2The hydrosol, the photocatalytic activity of product has obtained large increase.
The present invention is on the basis of above-mentioned work; Titanyl sulfate with cheapness is the titanium source; Adopt deposition-hydro-thermal method, need not high-tension apparatus, need not the later stage high-temperature heat treatment, under comparatively gentle condition, can make the well-crystallized, stablize, have the anatase type nano TiO of certain visible light catalysis activity
2The hydrosol.Propose simultaneously employing electrodialytic technique washing removal of contamination ion first, improved the TiO2 yield, reduced the water consumption, reduced cost; And employing dye sensitization technology and Ag
+Surface diposition further improves photocatalytic activity and the sterilization ability of photocatalyst under the visible light condition.
Summary of the invention
The objective of the invention is to overcome the deficiency that exists on the existing photocatalyst technology of preparing, a kind of method of preparing visible light active photocatalyst through dye sensitization is provided.This method need not can carry out under special installation, the normal temperature and pressure; Utilize the preparation of this method the photocatalyst non-corrosiveness, stablize not stratified, particle is tiny, adhesiveness is strong, photocatalytic activity and sterilization ability improve greatly; It is fungi-proofing to can be applicable to outdoor coating, indoor air purification and furniture mildew-resistant; Also can be used as the nano titanium oxide source and be coated on other carriers, the preparation loaded photocatalyst.
A kind of method of preparing visible light active photocatalyst through dye sensitization comprises the steps:
(1) the technical grade titanyl sulfate is soluble in water, filter to remove residue and other impurity, obtain clear solution, dripping alkali liquid and constantly stirring and adjusting generate the hydrated titanium dioxide deposition to the pH=8;
(2) adopting electroosmose process, is dialysate with the deionized water, removes the SO in the deposition
4 2-With other ion, until the supernatant electrical conductivity less than 20us/cm;
(3) deposition is added water mixing, making beating, adopt spectrophotometry Ti
4+Concentration also is made into the suspension of 0.1M, slowly splashes into a certain proportion of H under the stirring condition
2O
2Solution obtains the orange-yellow colloidal sol of clear more than the ageing 24h;
(4) in colloidal sol, add dyestuff sensitising agent or precious metal salt according to a certain percentage, hydro-thermal reaction 4～12h under 60～100 ℃ of conditions can obtain finite concentration, the stable photocatalyst product with visible light activity.
In above-mentioned preparation method, the said alkali lye of step (1) is selected from NaOH, potassium hydroxide or ammoniacal liquor.
In above-mentioned preparation method, the pH of system is adjusted in 7.5～8.5 when said titanyl sulfate of step (1) and alkali lye generation co-precipitation.System pH can't generate stable sols less than 7.5; PH is greater than 8.5, H
2O
2Consumption increases.
In above-mentioned preparation method, the said employing electrodialytic technique of step (2) carries out purifying to hydrated titanium dioxide deposition, until the supernatant electrical conductivity less than 20us/cm.
In above-mentioned preparation method, the said employing AAS of step (3) is measured Ti exactly
4+Concentration, thereby the photocatalyst product of the peptization course of conveniently regulating and controlling back and preparation ideal concentration.
In above-mentioned preparation method, the said H of step (3)
2O
2With Ti
4+Mol ratio be 4: 1～6: 1, add H
2O
2After colloidal sol need more than the ageing 24h.
In above-mentioned preparation method; Colloidal sol hydro-thermal reaction 4～12h under 60～100 ℃ condition after the said ageing of step (4); Can obtain mass concentration about 1%, photocatalyst product stable, that have visible light activity, this product is placed can not produce any deposition and lamination more than 1 year.
In above-mentioned preparation method; The said dye sensitizing agent of step (4) comprises the pyridines complex compound of common dye (like red scarlet B, eosin, phthalein flower cyanogen class), chlorophyll, humic acid and ruthenium; What in this patent, adopt is eosin or chlorophyll etc., and addition is the 0.25%-1.0% of solid content.
In above-mentioned preparation method, the said precious metal salt of step (4) is a silver nitrate, presses Ag
+/ Ti
4+Mol ratio is 0.05～0.10 ratio adding.
Advantage of the present invention is:
1. adopt dye sensitization technology, improved the photocatalytic activity of product under the visible light condition; Adopt the silver ion surface diposition to improve the sterilization ability of product.
2. adopt electrodialytic technique washing SO
4 2-And NH
4 +, separative efficiency is high, and clean result is good, greatly reduces water consumption and cost.
3. photocatalyst is faint yellow, translucent, neutrality, and odorlessness, nothing corrosion, good dispersion, stability height, placing for a long time or dilute can layering or deposition.
4. the titanium dioxide granule particle diameter in the photocatalyst is little, and for about 10nm, specific area is big, and adhesiveness is strong; Particle is a Detitanium-ore-type, and crystallization degree is high, need not high-temperature calcination and handles
5. raw material are cheap and easy to get, and preparation technology is simple, suitable for mass production.
Description of drawings
Fig. 1, deposition-hydro-thermal method low-temperature synthesis of nanometer photocatalyst of titanium dioxide process chart
The TEM figure of Fig. 2, photocatalyst
The XRD figure of sample under Fig. 3, the differential responses temperature conditions
The XRD figure of sample under Fig. 4, the differential responses time conditions
Fig. 5, photocatalytic degradation formaldehyde waste water effect
Fig. 6, gaseous formaldehyde degradation experiment result
Fig. 7, anti-microbial property testing result
The specific embodiment
Further specify the present invention through instance and accompanying drawing below, but be not construed as limiting the invention.
Embodiment 1. deposition-hydro-thermal method low temperature prepare high-purity nm TiO
2Photocatalyst
In the 1000mL round-bottomed flask, add the 200mL deionized water solution; Regulate pH=8 as end liquid; Continuing under the churned mechanically situation; The titanyl sulfate solution of 400mL0.25mol/L and the ammonia spirit of 3mol/L are added drop-wise in the end liquid jointly, keep pH constant in the dropping process, generate the muddy liquid that contains the titanium hydroxide deposition.Above-mentioned muddy liquid is stirred ageing adopts electroosmose process after 30 minutes, clean foreign ion, up to the electrical conductivity of cleaning the deposition supernatant less than 20us/cm.Be made into suspension after titanium hydroxide deposition is scattered in the 200mL deionized water, utilize hydrogen peroxide spectrphotometric method for measuring Ti
4+Concentration and add distilled water it be made into the suspension of 0.1mol/L.According to Ti
4+/ H
2O
2Mol ratio is that 1: 4 ratio drips hydrogenperoxide steam generator (concentration 30%) and stirs 60min, leaves standstill more than the 24h, generates orange-yellow transparent [TiO (H
2O
2)]
2+Colloidal sol.Above-mentioned solution is placed water-bath or electric jacket, and under 60 ℃ of conditions, that hydro-thermal reaction can obtain in 12 hours is faint yellow, translucent, pH is neutral, stable photocatalyst of titanium dioxide.For preventing colloidal sol, need on there-necked flask, to add cork and condensing unit by evaporate to dryness.Fig. 2 is the TEM figure of prepared photocatalyst, can know about product cut size 10nm by Fig. 2, and the well-crystallized, decentralization is high.
High-purity nm TiO under the embodiment 2. preparation different water thermal response temperature conditions
2Photocatalyst
Change the hydrothermal temperature among the embodiment 1 into 60,80,100 ℃ respectively, hydro-thermal reaction can obtain the photocatalyst of titanium dioxide under the different water thermal response temperature conditions in 8 hours.Fig. 3 is the XRD figure of sample under the differential responses temperature conditions.Can know by Fig. 3, be lower than the nano-TiO that can't obtain the well-crystallized under 60 ℃ of conditions
2, along with the rising of temperature, the crystallization of product is more perfect, when hydrothermal temperature is 100 ℃, demonstrates significant Detitanium-ore-type diffraction maximum.
High-purity nm TiO under the embodiment 3. preparation different water thermal response time conditions
2Photocatalyst
Change the hydro-thermal reaction time among the embodiment 1 into 4,6,8,10,12 hours respectively, 100 ℃ of photocatalyst of titanium dioxide that can obtain under the different water thermal response time conditions of hydrothermal temperature.Fig. 4 is the XRD figure of sample under the differential responses time conditions.Can know that by Fig. 4 along with the increase of hydro-thermal reaction time, it is perfect that crystal development is tending towards gradually; When hydro-thermal reaction time 8～10h; Diffraction peak intensity is the highest, and continuing increases the reaction time, and the pertitanic acid complex compound in the colloidal sol decomposes; Collosol stability reduces, the trend that nano particle has mutual reunion to grow up.
Embodiment 4. preparation high activity dye-sensitized nano TiO
2Photocatalyst
Accurately take by weighing the 0.1g eosin and place the 1000mL there-necked flask; The orange-yellow vitreosol 500mL that in wherein adding embodiment 1, generates; After stirring 30min treated its complete dispersing and mixing, hydro-thermal reaction 4h obtained having the dye-sensitized nano TiO of visible light activity under 100 ℃ of conditions
2Photocatalyst.
Embodiment 5. preparation precious metals ags
+Depositing nano TiO
2Photocatalyst
Accurately take by weighing 0.85g AgNO
3And place the 1000mL there-necked flask, and the orange-yellow vitreosol 500mL that in wherein adding embodiment 1, generates, after stirring 30min treated its complete dispersing and mixing, hydro-thermal reaction 8h obtained precious metals ag under 80 ℃ of conditions
+The nano-TiO of deposition
2Photocatalyst.Perhaps get the optical catalyst sol 500mL that behind hydrothermal crystallizing, generates among the embodiment 1, to wherein accurately adding 0.85g AgNO
3, under the condition of ultra violet lamp, constantly stir 1～2h, can obtain precious metals ag
+The nano-TiO of deposition
2Photocatalyst.
The experiment of embodiment 6. photocatalysts degraded gaseous formaldehyde
Experiment is at 1m
3Airtight glass box in carry out, 25 ℃ of the temperature inside the box, humidity 70%～80%RH in the case, testing sample are respectively the prepared sample of embodiment 1 and embodiment 4.The 200mL sample is sprayed on 1m
2Cardboard on dry and be placed in the glass box, certain density formaldehyde gas is injected in the sealing back, fluorescent lamp adopts the air sampler sampling, the concentration of liquid chromatography for measuring removing residue formaldehyde according to handling behind the 72h with phenol reagent as absorption liquid.Testing result can find out that the degradation rate of photocatalyst stoste PARA FORMALDEHYDE PRILLS(91,95) waste gas in 72h that this patent is prepared can reach 85.1% shown in Fig. 6 tabulation, and further improves through degradation rate after the dye sensitization, can reach 95.3%.
The degrade experiment of liquid formaldehyde of embodiment 7. photocatalysts
Experiment is carried out in homemade photocatalytic reaction device.(10 μ g/mL, 40mL), testing sample is respectively the prepared sample of embodiment 1 and embodiment 4 in two culture dishes, to add the formaldehyde standard liquid of equivalent.Fluorescent lamp (power 20W) is placed directly over the liquid level about 5cm.Open fluorescent lamp, every separated 30min sampling 1mL gets 6 appearance, adopts the concentration of Their Determination by Spectrophotometry residual formaldehyde.Can find out that by Fig. 5 the prepared photocatalyst of the present invention has photocatalytic activity preferably under the visible light condition, further improve that the clearance of liquid towards formaldehyde can reach more than 95% behind the 180min through photocatalytic activity after the dye sensitization.
Under aseptic condition, the former bacterium oese of target is moved in the 100ml sterilized water, shake up and obtain former bacterium suspension.Successively embodiment 1 is coated on the clean slide with embodiment 5 prepared samples, in the culture dish as for sterilization (parallel do three parts), is coated on the slide with the object bacteria liquid of rubbing method then equivalent.The irradiation certain hour places sterilized culture medium under the 20W fluorescent lamp, after 25 ℃ aseptic conditions are cultivated 48h down, looks into clump count, the assessment sterilization effect.Can find out Ag by Fig. 7 tabulation
+Depositing nano TiO
2Photocatalyst all is superior to the sample that do not deposit to the antibacterial effect of ETEC, staphylococcus aureus.
Claims (2)
1. the method for a preparing visible light active photocatalyst through dye sensitization is characterized in that comprising the following steps: successively
(1) the technical grade titanyl sulfate is soluble in water, filter the solution that removal residue and other impurity get clear, dripping alkali liquid and continuous stirring and adjusting pH=7.5～8.5 generate the hydrated titanium dioxide deposition;
(2) adopting electroosmose process, is dialysate with the deionized water, removes the SO in the deposition
4 2-(sulfate ion) and other ion, until the supernatant electrical conductivity less than 20 μ s/cm;
(3) deposition is added water mixing, making beating, adopt spectrophotometry Ti
4+(titanium ion) concentration, and adding distil water is made into Ti
4+Concentration is the suspension of 0.1M, slowly splashes into H under the stirring condition
2O
2(hydrogen peroxide) solution obtains the orange-yellow colloidal sol of clear more than the ageing 24h; H
2O
2With Ti
4+Mol ratio be 4: 1～6: 1, add H
2O
2After colloidal sol need more than the ageing 24h;
(4) in colloidal sol, add the dyestuff sensitising agent, hydro-thermal reaction 4～12h under 60～100 ℃ of conditions can obtain finite concentration, the stable photocatalyst product with visible light activity; Dye sensitizing agent is selected from red scarlet B, eosin, chlorophyll or humic acid, and addition is the 0.25%-1.0% of solid content.
2. the method for a kind of preparing visible light active photocatalyst through dye sensitization according to claim 1 is characterized in that alkali lye is selected from NaOH, potassium hydroxide or ammoniacal liquor.
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Cited By (1)
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| RU2565193C1 (en) * | 2014-03-07 | 2015-10-20 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Московский государственный университет тонких химических технологий имени М.В. Ломоносова" (МИТХТ им. М.В. Ломоносова) | Method of producing nanosized titanium dioxide |
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| CN102000566A (en) * | 2010-10-15 | 2011-04-06 | 徐志兵 | Method for preparing photoactivated silver/titanium dioxide complex |
| RU2520100C1 (en) * | 2012-11-28 | 2014-06-20 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Московский государственный университет тонких химических технологий имени М.В. Ломоносова" (МИТХТ им. М.В. Ломоносова) | Method of preparing titanium oxide photocatalyst active in visible spectrum |
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