CN101549895A - Preparation method of carbon aerogel load titanium dioxide electrodes and application thereof - Google Patents
Preparation method of carbon aerogel load titanium dioxide electrodes and application thereof Download PDFInfo
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- CN101549895A CN101549895A CNA2009100498228A CN200910049822A CN101549895A CN 101549895 A CN101549895 A CN 101549895A CN A2009100498228 A CNA2009100498228 A CN A2009100498228A CN 200910049822 A CN200910049822 A CN 200910049822A CN 101549895 A CN101549895 A CN 101549895A
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Abstract
The invention belongs to the technical field of water processing, in particular relates to a preparation method of carbon aerogel load titanium dioxide electrodes and application thereof. The specific steps are as follows: preparation of carbon aerogel, preparation of butyl carbonate sol, load and sintering of butyl carbonate sol gel, thereby obtaining required product. The electrode has the advantages of high porosity, big specific surface, high electrical conductivity, controlled face shaping, strong photocatalytic activity, and the like, and is applied to processing high-chroma dye waste water by electrochemical absorption fill light catalytic degradation. The CA/TiO2 in the invention has good electric absorption performance and photocatalytic activity; with the auxiliary strengthening effect of electric absorption, the concentration range of colored dye waste water degradation removal is wide (100 mg/L to 1000 mg/L); and the removing speed can be improved more than 3 times compared with photocatalytic degradation. The technology has simple and convenient operation and good processing effect for pollutant waste water, is a high-efficient and energy-saving new technology, and has very great application value in the field of waste water processing.
Description
Technical field
The invention belongs to water-treatment technology field, be specifically related to a kind of preparation method and application thereof of carbon aerogel load titanium dioxide electrodes.
Background technology
Use the development of dyestuffs industries along with plastics, rubber, fiber, coating and Yin Mo etc., the output of organic dye constantly rises, wastewater discharge also constantly increases, so the colorful wastewater pollution problem is serious day by day, and this type of waste water has the advantages that colourity is dark, toxicity is big, biochemical degradation is difficult.In recent years, utilize semiconductor grain to come the photodegradation colorful wastewater to become an international research focus as catalyzer.TiO wherein
2Little owing to toxicity, stable and catalytic capability becomes most widely used photocatalyst by force.The waste water from dyestuff of, light transmission difference dark for colourity, the photocatalytic degradation processing efficiency is low.The method of seeking the high efficiency photocatalysis degradation of dye waste water is environmentalist's a target always.
Therefore the electrochemistry adsorption method being introduced in the photocatalytic degradation high-chromaticity dye wastewater, is a kind of novel waste water treatment process.Earlier with TiO
2Be carried on the electrode surface with good electrical absorption property, under electric field action dye molecule be enriched in electrode surface, reduce the colourity of solution, UV-light sees through waste water solution and acts on TiO simultaneously
2Photocatalyst, the degradation treatment pollutent.Along with Degradation electrode surface Pollutant levels reduce gradually, the existence of electric field can make that pollutent further is enriched in electrode surface in the solution, continues the efficient processing power of performance photocatalytic degradation reaction.In handling the high-chromaticity dye wastewater process, the electro-adsorption effect of at first bringing into play electrode materials is adsorbed in electrode surface with dye molecule, thereby reduces the colourity of the pollutent aqueous solution, helps the transmissivity of UV-light, better brings into play TiO
2Photocatalysis performance, play electricity and help light-catalysed effect.
A kind of electro-adsorption fill-in light catalysis electrode of excellent performance must possess two conditions: 1, carrier itself must possess the characteristics of electro-adsorption electrode---high-specific surface area and good electrical conductivity.2, load TiO
2After electrode also should keep the electro-adsorption characteristic of electrode.Carbon aerogels is a kind of bulk material with high-specific surface area, high conductivity, is a kind of electro-adsorption electrode of excellent performance, and than simple adsorption, the existence of electric field can improve speed and the ability that electrode is removed pollutent.Adopt the Sol-Gel method to prepare CA/TiO
2Electrode is used it for electro-adsorption fill-in light catalyzed degradation high chroma organic dye waste water.
Summary of the invention
The objective of the invention is to prepare and a kind ofly have high-ratio surface, high conductivity, face shaping is controlled and is applicable to the preparation method and the application thereof of the carbon aerogel load titanium dioxide electrodes of electrochemistry absorption fill-in light catalyzed degradation technology.
The preparation method of the carbon aerogel load titanium dioxide electrodes that the present invention proposes, concrete steps are as follows:
(1): adopting sol-gel phenolic aldehyde polymerization, is raw material with Resorcinol, formaldehyde, behind the adding catalyst action, leaves standstill the resol that obtains having network-like structure in glass mold, and gauge control is between 5～10mm.Block resol sheet that will be through obtaining carries out solvent exchange in surface tension in less than the organic reagent of 30mN/m, water molecules to its network structure is replaced by organic reagent, at room temperature dry back program in tube furnace then and be warming up to 600～1200 ℃ and keep carrying out carbonization in 3～5 hours, obtain carbon aerogels;
(2) butyl (tetra) titanate, dehydrated alcohol and methyl ethyl diketone are mixed with the magnetic agitation instrument, drip nitric acid then, the mixing solutions that deionized water and dehydrated alcohol are formed continues to stir 2-4 hour then, obtains the collosol and gel of butyl (tetra) titanate.
(3) carbon aerogels with step (1) gained immerses in the butyl (tetra) titanate sol-gel solution of step (2) gained, and keeps 0.5～2 hour, takes out then in 90 ℃ of baking ovens and places 1～3 hour, repeats after cooling 2～6 times.
(4) with the carbon aerogels of the butyl (tetra) titanate sol-gel of step (3) gained, in tube furnace, be warming up to 400 ℃～800 ℃ and carry out high-temperature calcination, promptly get desired product.
Further tell about the preparation method of the carbon aerogel load titanium dioxide electrodes of the present invention's proposition below, concrete steps are as follows:
(1) be that 1: 2: 50～300: 17.5 mixed is even with Resorcinol, formaldehyde, catalyzer and water according to mol ratio, pour in the glass mold, the centre is cut apart with glass partition, the control spacing is 0.5～3cm, puts into encloses container then, standing and reacting, take out resultant resol aerogel, carry out solvent exchange with surface tension less than the organic reagent of 30mN/m again, the time is 5～7 days, and certain interval of time (as 24 hours) is changed organic reagent; Resultant resol aerogel is positioned over carries out drying under the room temperature, the drying at room temperature time is sequence of control intensification in tube furnace after 5～7 days, be warmed up to 600 ℃～1200 ℃ and remain on and reacted under this temperature 3～5 hours with the speed of 1.5 ℃/min～3.5 ℃/min, be cooled to room temperature then at the same rate, obtain carbon aerogels;
(2) butyl (tetra) titanate, dehydrated alcohol, methyl ethyl diketone are mixed with the magnetic agitation instrument by 1: 3: 0.1～0.5 volume ratio, drip the mixing solutions of nitric acid, deionized water, dehydrated alcohol composition then, the volume ratio of nitric acid, deionized water and dehydrated alcohol is 1: 4: 20～30, continue to stir 2～4 hours, obtain the collosol and gel of butyl (tetra) titanate;
(3) carbon aerogels that step (1) is obtained is immersed in the butyl (tetra) titanate sol-gel solution that step (2) obtains, and kept 0.5～2 hour, take out then in 90 ℃ of baking ovens and placed 1～3 hour, repeat this step 2-6 time after cooling, obtain flooding the carbon silica aerogel electrode of butyl (tetra) titanate sol-gel;
(4) with the carbon silica aerogel electrode of the butyl (tetra) titanate sol-gel of step (3) gained, place the tube furnace under the argon shield to be warming up to 400 ℃～800 ℃ and kept 2～4 hours with the speed of 1.5～3.5 ℃/min, cooling promptly gets desired product then.
Among the present invention, the described catalyzer of step (1) be in yellow soda ash, sodium hydroxide or the potassium hydroxide etc. any.
Among the present invention, time of repose is described in the step (1): 20～30 ℃ 20～30 hours down, 50～60 ℃ down 20～30 hours or 80～90 ℃ down in 60～90 hours any.
Among the present invention, organic solvent is acetone or dehydrated alcohol described in the step (1).
The carbon aerogel load titanium dioxide electrodes that utilizes the inventive method to obtain can be used for electro-adsorption fill-in light catalyzed degradation device.The CA/TiO that is connected with platinum filament
2Electrode is a working electrode, and platinized platinum is a counter electrode, and saturated calomel electrode is a reference electrode, adopts electrochemistry constant potential mode that required electric microfield is provided, control constant potential voltage ± 200～± 600mV.The ultraviolet lamp that to adopt a 80W predominant wavelength be 365nm is a light source, the overcoat quartz glass tube inserts the glass a set of cups central authorities of a cylindrical tyre recirculated water, utilize the super constant temperature trough control reaction temperature at 25 ℃, whole device adopts magnetic agitation to make reaction solution keep uniform concentration.
Processing parameter relevant in the aforesaid method is: it is 30～1000ml that water sample is handled volume, and electrode area can be 2～20cm
2, interelectrode distance remains on 0.5～3cm, and the current potential of control working electrode is ± 200～± 600mV.
Carry out the constant potential electro-adsorption in the aforesaid method, the treatment time is carried out the control of respective handling time according to the character of handling waste water and the water yield and electrode area in actual application between 3-8h, be as the criterion to reach last processing requirements.
The carbon aerogel load titanium dioxide electrodes that utilizes the inventive method to obtain can be used for handling typical high density, high-chromaticity dye wastewater, comprises methylene blue or sodium alizarinsulfonate in this waste water from dyestuff.
The CA/TiO that is connected with platinum filament
2As handling electrode, platinum electrode is a counter electrode, and saturated calomel electrode adopts electrochemistry constant potential mode that required electric microfield is provided as reference electrode, carries out electro-adsorption fill-in light catalyzed degradation under UV-irradiation.
Use this device to discovering that high chroma sodium alizarinsulfonate and methylene blue dye waste water are handled, with high-ratio surface CA/TiO
2As working electrode electro-adsorption fill-in light catalyzed degradation waste water, treatment effect is very desirable.The concentration range of pollutant removal is wide, and (100mg/L～1000mg/L), compare with simple photocatalytic Degradation, clearance can improve more than 3 times.
The present invention has following advantage:
1. because the present invention adopts the synthetic route of collosol and gel phenolic aldehyde polymerization-Air drying-high temperature cabonization-titanium dichloride load, prepare novel C A/TiO
2, specific surface area reaches 600m
2More than/the g, TiO
2Charge capacity can reach 10～30%.With same amount TiO
2Be carried on (ITO/TiO on the conductive glass
2) compare, have the katalysis of better electro-adsorption fill-in light, the degradation effect of high-chromaticity dye wastewater there is obvious effects.So CA/TiO
2It is a kind of ideal electrochemistry absorption fill-in light catalyzed degradation electrode.
2. the present invention adopts with specific conductivity height, specific surface area is big, photocatalytic activity is strong block CA/TiO
2As handling electrode, on technology, electro-adsorption method and photocatalytic degradation method are combined, adopt three-electrode system under specific potential, environmental pollutant to be enriched to electrode surface, quicken the photocatalytic degradation speed of reaction of pollutent.
3. electro-adsorption fill-in light catalytic degradation reaction of the present invention is applied to the relatively poor high-chromaticity dye wastewater of transparence, dye molecule can be enriched in electrode surface by the electro-adsorption effect, reduces the concentration of pollutent in the solution, improves the light transmission of solution.Compare with simple photocatalysis, electrochemistry absorption fill-in light catalyzed degradation can significantly improve the translucidus of high-chromaticity dye wastewater, makes it be more suitable for photocatalytic degradation, increases light-catalyzed reaction speed, improves contaminant removal efficiency.
Embodiment
Further specify the present invention below by embodiment.
Embodiment 1:
(1) preparation of carbon aerogels
Sol-gel phenolic aldehyde polymerization is a raw material with Resorcinol, formaldehyde, and yellow soda ash is catalyzer, by 1: 2: 50: leave standstill the resol that obtains having network-like structure under 17.5 the mol ratio; Apparent size according to the required electrode materials of requirement of experiment is prepared mould, and mould generally adopts glass preparation, and according to the thickness degree of required electrode, the interval distance obtains satisfactory resol sheet, and gauge control is at 5mm.Carried out solvent exchange 5 days through the block resol that obtains after leaving standstill in the low acetone of surface tension, the water molecules in its network structure is replaced by acetone, at room temperature dries then, needs 5 days approximately.Dried aerogel program in tube furnace is warming up to 950 ℃ and keep 4h to carry out carbonization, obtains the blocky carbon aerogels of black.
(2) preparation of butyl (tetra) titanate collosol and gel
Butyl (tetra) titanate, dehydrated alcohol, methyl ethyl diketone are mixed with the magnetic agitation instrument by 1: 3: 0.1 volume ratio, drip the mixing solutions of nitric acid, deionized water, dehydrated alcohol composition then, the volume ratio of nitric acid, deionized water and dehydrated alcohol is 1: 4: 20, continue to stir 2～4 hours, obtain the collosol and gel of butyl (tetra) titanate
(3) load of butyl (tetra) titanate collosol and gel
The carbon aerogels that carbonization obtains immerses in the butyl (tetra) titanate sol-gel solution, and keeps 0.5～2 hour, takes out then in 90 ℃ of baking ovens and places 1～3 hour, repeats the carbon aerogels that above-mentioned steps obtains load butyl (tetra) titanate colloidal sol for 3 times after cooling.Final calcining back TiO
2Load quality per-cent reached 15%, and BET numerical value also significantly decreases, and nearly reduced about 20%, dropped to 603m from 744
2/ g.
(4) calcining of electrode
With the carbon aerogels of repeated impregnations butyl (tetra) titanate, place the tube furnace under the argon shield to be warming up to 600 ℃ and kept 2～4 hours respectively with the speed of 1.5～3.5 ℃/min.After 600 ℃ of calcinings, its XRD figure spectrum not only diffraction peak occurred at 25.5 °, locate all to have occurred strong and weak different diffraction peak at 27.4 °, 36.1 ° with 54.3 °, decomposition reaction generation TiO has taken place in the butyl (tetra) titanate collosol and gel that is carried on this moment on the carbon aerogels in argon atmosphere
2, and TiO
2Crystal formation have the part anatase octahedrite to be transformed into rutile gradually.Obtain TiO after the cooling
2Charge capacity is 15%, specific surface area reaches 603m
2The CA/TiO of/g
2Electrode.
Embodiment 2:
(1) preparation of carbon aerogels
Sol-gel phenolic aldehyde polymerization is a raw material with Resorcinol, formaldehyde, and dehydrated alcohol is a catalyzer, by 1: 2: 300: leave standstill the resol that obtains having network-like structure under 17.5 the mol ratio; Apparent size according to the required electrode materials of requirement of experiment is prepared mould, and mould generally adopts glass preparation, and according to the thickness degree of required electrode, the interval distance obtains satisfactory resol sheet, and gauge control is at 8mm.Carried out solvent exchange 5 days through the block resol that obtains after leaving standstill in the low acetone of surface tension, the water molecules in its network structure is replaced by acetone, at room temperature dries then, needs 5 days approximately.Dried aerogel program in tube furnace is warming up to 950 ℃ and keep 4h to carry out carbonization, obtains the blocky carbon aerogels of black.
(2) preparation of butyl (tetra) titanate collosol and gel
Butyl (tetra) titanate, dehydrated alcohol, methyl ethyl diketone are mixed with the magnetic agitation instrument by 1: 3: 0.5 volume ratio, drip the mixing solutions of nitric acid, deionized water, dehydrated alcohol composition then, the volume ratio of nitric acid, deionized water and dehydrated alcohol is 1: 4: 30, continue to stir 2～4 hours, obtain the collosol and gel of butyl (tetra) titanate
(3) load of butyl (tetra) titanate collosol and gel
The carbon aerogels that carbonization obtains immerses in the butyl (tetra) titanate sol-gel solution, and keeps 0.5～2 hour, takes out then in 90 ℃ of baking ovens and places 1～3 hour, repeats the carbon aerogels that above-mentioned steps obtains load butyl (tetra) titanate colloidal sol for 6 times after cooling.Final calcining back TiO
2Load quality per-cent reached 18%, and BET numerical value also significantly decreases, and nearly reduced about 25%, dropped to 590m from 744
2/ g.
(4) calcining of electrode
With the carbon aerogels of repeated impregnations butyl (tetra) titanate, place the tube furnace under the argon shield to be warming up to 800 ℃ and kept 2～4 hours respectively with the speed of 1.5～3.5 ℃/min.After 800 ℃ of calcinings, the diffraction peak of the XRD figure of material spectrum about 25.5 ° disappeared, and several peaks in addition exist, and intensity rises TiO to some extent
2Change into rutile crystal type fully.Obtain TiO after the cooling
2Charge capacity is 18%, specific surface area is 590m
2The CA/TiO that/g is above
2Electrode.
Embodiment 3:CA/TiO
2Be used for electro-adsorption fill-in light catalyzed degradation high chroma methylene blue waste water
The electro-adsorption device adopts: the CA/TiO that is connected with platinum filament
2As working electrode, platinized platinum is a counter electrode, and saturated calomel electrode adopts electrochemistry constant potential mode that required electric microfield is provided as reference electrode, carries out the experiment of electro-adsorption fill-in light catalyzed degradation under UV-irradiation.The simulated wastewater liquor capacity is 40～1000ml in the experiment, control constant potential voltage ± 200～± 600mV.
The starting point concentration of water sample be the 150mg/L methylene blue the H of 0.01mol/L
2SO
4In the supporting electrolyte, volume is 85ml, respectively as the CA/TiO of working electrode and counter electrode
2The area of electrode and platinum electrode is 3.5cm
2, constant potential voltage is-600mV.With independent photocatalysis is that simultaneous test is carried out effect relatively.Removing speed when adsorbing separately only is 2.62 * 10
-3Min
-1Removal speed significantly is increased to 9.88 * 10 after adopting the auxiliary photocatalytic Degradation of electro-adsorption
-3Min
-1, improved 3.8 times.
Embodiment 4:CA/TiO
2Be used for electro-adsorption fill-in light catalyzed degradation high chroma sodium alizarinsulfonate waste water
The electro-adsorption device adopts: the CA/TiO that is connected with platinum filament
2As working electrode, platinized platinum is a counter electrode, and saturated calomel electrode adopts electrochemistry constant potential mode that required electric microfield is provided as reference electrode, carries out the experiment of electro-adsorption fill-in light catalyzed degradation under UV-irradiation.The simulated wastewater liquor capacity is 40～1000ml in the experiment, control constant potential voltage ± 200～± 600mV.
The starting point concentration of water sample be the 400mg/L sodium alizarinsulfonate the NaOH supporting electrolyte of 0.01mol/L in, volume is 85ml, respectively as the CA/TiO of working electrode and counter electrode
2The area of electrode and platinum electrode is 5.5cm
2, constant potential voltage is 600mV.With independent photocatalytic Degradation be that simultaneous test is carried out effect relatively.Separately removing speed during photocatalytic Degradation only is 3.90 * 10
-3Min
-1Removal speed significantly is increased to 7.30 * 10 after adopting electro-adsorption fill-in light catalyzed degradation
-3Min
-1, improved 1.9 times.
In the large-scale treatment facility of practical application, particularly in the industrial dye waste water scavenging process, water pollutant concentration is generally higher, the colourity height of waste water, translucidus are poor, UV-light is difficult to reach photocatalyst surface when adopting Treatment by Photocatalysis Oxidation, and speed of reaction is low, and energy consumption is big.And simple electro-adsorption method is used in the processing low concentration wastewater more.So adopt the method for electro-adsorption fill-in light catalyzed degradation to be specially adapted to the processing of high-concentration high-chromaticity dye wastewater.
The required simulated wastewater liquor capacity of experiment is 30～1000ml in the reaction unit, control constant potential voltage ± 200～± 600mV.In industrial practicality,, can increase CA/TiO because pending waste water is more
2Electrode area (or adopts polylith CA/TiO
2The electrode parallel connection) mode increases electrode area, and wherein pending reactant comprises but the magnitude of voltage of control remains unchanged: the indicator pollutant of typical dye pollutent, high chroma characteristic specifically comprises methylene blue, sodium alizarinsulfonate.
The foregoing description proves: the change of preparation condition is to CA/TiO
2Character very big influence is arranged, for the top condition that obtains under the actual user mode can be optimized the CA/TiO that preparation condition obtains corresponding to actual needs
2Material.With CA/TiO
2As working electrode, electro-adsorption fill-in light catalyzed degradation typical dye waste water system methylene blue, sodium alizarinsulfonate etc. obtain good treatment effect.This technology is breakthrough and the development to existing green technology, can play the effect of protection water resources, meets the environmental consciousness that present country advocates, and has very wide application prospect and industry development concurrently and is worth.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (6)
1, a kind of preparation method of carbon aerogel load titanium dioxide electrodes is characterized in that concrete steps are as follows:
(1) be that 1: 2: 50～300: 17.5 mixed is even with Resorcinol, formaldehyde, catalyzer and water according to mol ratio, pour in the glass mold, the centre is cut apart with glass partition, the control spacing is 0.5～3cm, puts into encloses container then, standing and reacting, take out resultant resol aerogel, carry out solvent exchange with surface tension less than the organic reagent of 30mN/m again, the time is 5～7 days, and certain hour is changed organic reagent at interval; Resultant resol aerogel is positioned over carries out drying under the room temperature, the drying at room temperature time is sequence of control intensification in tube furnace after 5～7 days, be warmed up to 600 ℃～1200 ℃ and remain on and reacted under this temperature 3～5 hours with the speed of 1.5 ℃/min～3.5 ℃/min, be cooled to room temperature then at the same rate, obtain carbon aerogels;
(2) butyl (tetra) titanate, dehydrated alcohol, methyl ethyl diketone are mixed with the magnetic agitation instrument by 1: 3: 0.1～0.5 volume ratio, drip the mixing solutions of nitric acid, deionized water, dehydrated alcohol composition then, the volume ratio of nitric acid, deionized water and dehydrated alcohol is 1: 4: 20～30, continue to stir 2～4 hours, obtain the collosol and gel of butyl (tetra) titanate;
(3) carbon aerogels that step (1) is obtained is immersed in the butyl (tetra) titanate sol-gel solution that step (2) obtains, and kept 0.5～2 hour, take out then in 90 ℃ of baking ovens and placed 1～3 hour, repeat this step 2-6 time after cooling, obtain flooding the carbon silica aerogel electrode of butyl (tetra) titanate sol-gel;
(4) with the carbon silica aerogel electrode of the butyl (tetra) titanate sol-gel of step (3) gained, place the tube furnace under the argon shield to be warming up to 400 ℃～800 ℃ and kept 2～4 hours with the speed of 1.5～3.5 ℃/min, cooling promptly gets desired product then.
2, the preparation method of carbon aerogel load titanium dioxide electrodes according to claim 1, it is characterized in that the described catalyzer of step (1) be in yellow soda ash, sodium hydroxide or the potassium hydroxide any.
3, the preparation method of carbon aerogel load titanium dioxide electrodes according to claim 1, it is characterized in that time of repose is described in the step (1): 20～30 ℃ 20～30 hours down, 50～60 ℃ down 20～30 hours or 80～90 ℃ down in 60～90 hours any.
4, the preparation method of carbon aerogel load titanium dioxide electrodes according to claim 1 is characterized in that organic solvent is acetone or dehydrated alcohol described in the step (1).
5, the carbon aerogel load titanium dioxide electrodes that utilizes the inventive method to obtain is used for electro-adsorption fill-in light catalyzed degradation device.
6, the carbon aerogel load titanium dioxide electrodes that utilizes the inventive method to obtain is used for dye wastewater treatment using, comprises methylene blue or sodium alizarinsulfonate in this waste water from dyestuff.
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