CN102910767A - Method for removing arsenic by loading titanium dioxide with activated carbon fiber hydrothermal method by means of photoelectrocatalysis oxidation - Google Patents
Method for removing arsenic by loading titanium dioxide with activated carbon fiber hydrothermal method by means of photoelectrocatalysis oxidation Download PDFInfo
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Abstract
The invention discloses a method for removing arsenic by loading titanium dioxide with an activated carbon fiber hydrothermal method by means of photoelectrocatalysis oxidation. The method comprises the following steps of: oxidizing the trivalent arsenic, which is high in toxicity and difficult to treat, pentavalent arsenic which is easily treated by photoelectrocatalysis oxidation treatment, and completely removing the pentavalent arsenic by adsorbents which can strongly absorb the arsenic, namely titanium dioxide, iron oxide or activated aluminium oxide and the like. The method disclosed by the invention is simple in technology, convenient to operate, low in cost, and free from the generation of sludge residue, the arsenic in water can be effectively removed, an activated carbon fiber photoelectrode can run for a long term, and can be used at a large area and a large scale without changing, and the outlet water quality fulfills the national standard, so that the method is suitable for treating the drinking water and the high-arsenic waste water.
Description
Technical field
The present invention relates to the method that a kind of tap water removes arsenic.More particularly, the present invention relates to the method for a kind of activated carbon fiber hydrothermal method carried titanium dioxide photoelectrocatalysioxidization oxidization arsenic removal.
Background technology
The occurring in nature arsenic element extensively is present in the food chain of soil, rock, water body and animal and plant body.In 8 provinces, cities and regions, influenced population is more than 200 ten thousand people nearly at China's drinking water type distribution of endemic arsenism, and the arsenic element pollution can cause serious human health problems, and the high arsenic tap water of long-term drinking can cause black leg and skin carcinoma, and is dead because of cerebral palsy when serious.Up-to-date " drinking water sanitary standard " (GB5749-2006) has higher requirement to Urban water supply water quality, and arsenic content is reduced to 0.01mg/L by the 0.05mg/L of old standard.The method that arsenic contamination is processed arsenic contamination waste water at present mainly contains: absorption method, Coagulation Method, ion exchange method, biological process, electrocoagulation, pressure membrane driving method etc., yet limitation is separately arranged, such as titanium dioxide arsenic had preferably adsorptive power, stable chemical nature, acid and alkali-resistance is not to introducing by product and toxic substance after the polluted water processing.When titanium dioxide is subject to photon energy when irradiation that wavelength is less than or equal to 387.5nm, the transition of electron of valence band to conduction band, thereby produced light induced electron (e
-)-hole (h
+) right.The h that produces
+The OH of titanium dioxide surface will be adsorbed on
-And H
2O is oxidized to hydroxyl radical free radical; Electronics (e
-) with the oxygen molecule reaction on surface, finally may generate hydroxyl radical free radical, hydroxyl radical free radical has very strong oxidation capacity, As in the water (III) can be oxidized to As (V).U.S. Patent number US20090364505 adopts doping metals or nonmetallic titania powder As (III) in the photochemical catalytic oxidation water under radiation of visible light, the effect of arsenic removal is better, yet, the powder titanium dioxide particle is very little, the suspending phase catalyzer is difficult to be regained, cost is high, is not suitable for directly with powder titanium dioxide as oxidation As (III) catalyzer.
The toxicity of As (III) and transport property are greater than As (V), and As (III) is with neutral substance (H in most of natural water
3AsO
3) exist, and As (V) is with ionic species (H
2AsO
4 -Perhaps HAsO
4 2-) exist, than the easier removal of As (III), therefore most of Technology Needs are oxidized to pentavalent arsenic with trivalent arsenic to the As of ionic species (V) in advance by absorption or flocculation sediment.In addition, studies show that the toxicity of arsenide has very big-difference, the arsenide toxicity AsH of various forms
3As (III)〉As (V)〉MMA〉DMA.The As (III) that exists with arsenite exceeds 60 times than the toxicity of the As (V) that exists with the arsenate form.Therefore, As (III) is oxidized to As (V), both can have improved the clearance of arsenic, can reduce toxicity again.At present, the scholar is arranged take hypochlorite, oxygen, ozone, potassium permanganate etc. as oxygenant, adopt chemical oxidization method that arsenious oxidation is studied, adopt ozone that As (III) is oxidized to As (V) such as China Patent No. ZL02155224.X, but that the method need to successively pass into a large amount of ozone costs is higher; Granted publication CN101348296B adopts potassium permanganate as oxygenant, but uses this kind method to cause easily the secondary pollution of tap water, should not use in Drinking Water.Process Drinking Water and should avoid the use of chemical reagent as far as possible.Wei Zhigang etc. have announced the arsenic removal of platinum doped titanium dioxide photoelectrocatalysioxidization oxidization at Chinese patent bulletin CN101492199A, the effect of arsenic removal is better, but carrier uses gac, and contact resistance is larger between activated carbon granule and the particle, conductive capability is bad, must affect its catalytic effect; And having used noble metal platinum, cost is higher.Therefore, develop the effective arsenic removal technology of a kind of cheapness and become present research direction.
The present invention is with good conductivity, diameter is thin, and outer surface area is large, and the activated carbon fiber that can not cause secondary pollution is carrier, because the deadly defect of carbon-carbon composites is to be higher than under 500 ℃ the oxidizing atmosphere easily oxidizedly, therefore the physicals strength and modulus of charcoal filamentary material can weaken greatly.The physical vaporous depositions such as general carrying method such as atomic layer deposition method, sputtering method, laser assisted molecular beam sedimentation, ionization Cluster Method, chemical Vapor deposition process load temperature height and sol-gel method palpus high-temperature roasting crystallization must cause to a certain degree carrier active carbon fibrous physics physical strength and destroy.If the TiO that uses binding agent to prepare in advance
2Powder is loaded on the activated carbon fiber, can reduce to a certain extent TiO
2Activity, general binding agent is organism, easily produce slight crack after long-time the use even peel off, and slowly stripping causes secondary pollution to water body.
Adopt hydrothermal method to prepare at a lower temperature the high anatase-type nanometer titanium dioxide of photocatalytic activity, the hydrothermal method load only needs to place autoclave then to prepare the high anatase-type nanometer titanium dioxide of photocatalytic activity 200 ℃ of internal reaction for some time presoma and activated carbon fiber.Hydrothermal method need not can not destroy the original physical strength of activated carbon fiber through pyroprocessing.
Granular size directly affects photocatalytic activity, and particle diameter is less, and the specific surface area of photocatalyst is larger, and the probability that reacts on the unit surface increases, and more is conducive to improve photocatalysis efficiency.When grain diameter during at 1～10 nm, quantum size effect becomes obviously, and band gap broadens, thereby improves the oxidation-reduction ability in light induced electron and hole.So nano-TiO on surface
2Particle will be accepted photon catalyzed oxidation As (III) will be played an important role.
The photoelectrocatalysis technology is surface coverage TiO
2The conductor of film is as the light anode, and establishes in addition a noble electrode, and light induced electron can more effectively be separated with hole (current carrier) in the semi-conductor under the effect of extra electric field, and this electric field reinforcing effect has reduced simple composite significantly, uses TiO
2Optoelectronic pole can significantly improve the quantum yield of process.In addition, this photoelectrochemical system also has two other outstanding advantages, the one, the reduction process of conduction band electron is separated (comparing with semiconductive particles) with the oxidising process in valence band hole from the locus, the result has greatly increased the formation efficiency of semiconductor surface OH and has prevented intermediate oxidation product restoring on negative electrode.The 2nd, because conduction band electron is introduced to the H in the cathodic reduction water
+, therefore do not need in system, to blast the oxygen as the electron capture agent.Therefore, in containing the arsenic superstandard drinking water, first-selected photoelectrocatalysioxidization oxidization technology is rational.
Summary of the invention
The object of the invention is to solve in the prior art and can not effectively remove trivalent arsenic, the problem that the arsenic removal cost is high provides a kind of drinking water treatment method that has more using value, reaches the low-cost purpose that purifies high arsenic tap water.
Activated carbon fiber is compared with particulate state, powdered active carbon, activated carbon fiber has distinctive microvoid structure, higher outer surface area and specific surface area and multiple functional group, average pore diameter is also very little, reaches in fields such as waste water, off gas treatment, solution recovery, water purifications widely by modes such as physical adsorption, chemisorption and physical and chemical adsorption and uses.In the oxidation trivalent arsenic, be a kind of method of novel treatment Arsenic in Drinking Water with electrochemical applications.Utilize the various over-all properties of conduction, absorption and form of activated carbon fiber, it as a kind of novel photochemical catalyst electrode, is used for tap water removal arsenic and has broad prospects.
The carried titanium dioxide activated carbon fiber is as anode, and activated carbon fiber is as negative electrode, and impressed voltage is set to 0.1 ~ 1V; Large and unmanageable trivalent arsenic is oxidized to pentavalent arsenic with toxicity.At last, adopt high-efficient arsenic-removing sorbent that pentavalent arsenic is removed fully.
The method of a kind of activated carbon fiber hydrothermal method carried titanium dioxide photoelectrocatalysioxidization oxidization provided by the invention arsenic removal comprises the steps:
The treatment process of described activated carbon fiber is: commercially available activated carbon fiber is soaked down 30min 80 ℃ of 1mol/L sodium hydroxide solutions, water cleans up rear usefulness 68% nitric acid at 115 ℃ of lower constant temperature 4h, puts into 105 ℃ of dry 12h of baking oven after water cleans up.
Take by weighing the 10g tetrabutyl titanate in Erlenmeyer flask, add successively 45mL dehydrated alcohol and 20mL glacial acetic acid, magnetic agitation 30min is mixed into A liquid; Add 25mL dehydrated alcohol, 6.5mL redistilled water and 5mL glacial acetic acid in another Erlenmeyer flask, magnetic agitation 30min is mixed into B liquid; B liquid is splashed in the A liquid in the magnetic agitation with 1 drops/sec speed with separating funnel, and stirring velocity is 300r/min, drips off rear continuation and stirs 3h;
Measure the above solution of 60mL and activated carbon fiber and place the autoclave of inner liner polytetrafluoroethylene, described autoclave effective volume 100mL, pressure 10MPa, adopt hydrothermal method, prepare the carried titanium dioxide activated carbon fiber at 120 ~ 200 ℃ of lower reaction 1 ~ 5h, behind the ultrasonic cleaning 5min, in 105 ℃ of dry 12h, stand-by;
Photoelectrocatalysioxidization oxidization carries out under 4 ~ 1000W ultra violet lamp; Adopt the carried titanium dioxide activated carbon fiber as anode, activated carbon fiber is as negative electrode, and impressed voltage is set to 0.1 ~ 1V; Experimental water is redistilled water, because arsenic containing solution is As
2O
3Be dissolved in the NaOH solution and obtain, regulator solution pH is 6.5 ~ 8.5 before the catalysis.In arsenic containing solution, add sodium sulfate and be 100 ~ 1000 μ s/cm as ionogen regulator solution specific conductivity, close with the tap water specific conductivity; Place the dark whip attachment 3h of arsenic containing solution to make it reach adsorption equilibrium the carried titanium dioxide activated carbon fiber before the UV illumination, UV illumination 20 ~ 120min; Remove pentavalent arsenic with arsenic-removing adsorption agent after the illumination.Met " drinking water sanitary standard " tap water (GB5749-2006).
The mass ratio of described titanium dichloride load amount and activated carbon fiber is 0.2 ~ 1.0%.
The titanium dioxide of described load is nano titanium oxide.
Above-mentioned steps 3) used sorbent material comprises it being titanium dioxide, ferriferous oxide, iron hydroxide, Mn oxide, activated alumina or gac in.
Described carried titanium dioxide activated carbon fiber is reused.
Large and unmanageable trivalent arsenic is oxidized to pentavalent arsenic with toxicity in the present invention.At last, adopt high-efficient arsenic-removing sorbent that pentavalent arsenic is removed fully.
Beneficial effect of the present invention:
(1) the present invention is used in arsenic contamination drinking water treatment field with activated carbon fiber as electrode first.Highly toxic trivalent arsenic can be oxidized to pentavalent arsenic, and carry out active adsorption by the pentavalent arsenic of adsorption tower after to oxidation, reduce the consumption of sorbent material, reduce regeneration times, realize the low-cost high-efficiency arsenic removal.
(2) less energy-consumption of the present invention, only need apply 0.1 ~ 1V groove pressure is enough to effectively light induced electron be separated with the hole, this moment, water can be by electrolysis, low investment and low operational and administrative expenses, but large-scale application has environmental benefit and the social benefit of highly significant, simple to operate, operational management is convenient, and has reduced to greatest extent the exposure of pollutent in overall operation, and is environmentally friendly.
(3) the present invention does not produce sludge silt, does not need to carry out secondary treatment, and simple to the method for removing arsenic in the tap water, the very economical arsenic removal purpose that effectively reaches is conducive to the big area large-scale promotion.
Description of drawings
The TiO of Fig. 1 embodiment 1 preparation
2The transmission electron microscope picture.
The TiO of Fig. 2 embodiment 1 preparation
2The scanning electron microscope picture of/ACF.
Fig. 3 is activated carbon fiber photoelectrocatalysioxidization oxidization arsenic removing apparatus synoptic diagram of the present invention.
Wherein: 1. arsenic-containing water taphole 8. ultraviolet lamps 9. quartz socket tubes after arsenic-containing water solution entrance 5. sewage draining exits 6. arsenic-removing adsorption agents 7. of carried titanium dioxide activated carbon fiber 2. activated carbon fiber (ACF) before 3. voltage stabilized source 4. is processed are processed.
Embodiment
For a better understanding of the present invention, the invention will be further described below in conjunction with embodiment, but the scope of protection of present invention is not limited to the described scope of embodiment.
Take by weighing the 10g tetrabutyl titanate in Erlenmeyer flask, add successively 45mL dehydrated alcohol and 20mL glacial acetic acid, magnetic agitation 30min is called A liquid.Add 25mL dehydrated alcohol, 6.5mL redistilled water and 5mL glacial acetic acid in another Erlenmeyer flask, magnetic agitation 30min is called B liquid.B liquid is splashed in the A liquid in the magnetic agitation with 1 drops/sec speed with separating funnel, and stirring velocity is controlled to be 300r/min, drips off rear continuation and stirs 3h.
Measure the above solution of 60mL and activated carbon fiber and place autoclave (the effective volume 100mL of inner liner polytetrafluoroethylene, pressure 10MPa, compactedness 60%) in, 180 ℃ of lower reaction 3h prepare the carried titanium dioxide activated carbon fiber in baking oven, behind the ultrasonic cleaning 5min, in 105 ℃ of dry 12h.
Adopt as shown in Figure 3 reactor, the arsenic solution 250mL that in reactor, adds 2mg/L, regulate pH=7, adding sodium sulfate adjusting specific conductivity is 158 μ s/cm, and power is that the ultraviolet lamp of 9W places inside reactor, and it is anode that 0.25g carried titanium dioxide activated carbon fiber places inside reactor, take activated carbon fiber as negative electrode, applying groove is pressed 0.5V, and the dark 3h that places makes it reach adsorption equilibrium after the adding carried titanium dioxide activated carbon fiber, UV illumination 20 minutes.Sorbent material is the 0.25g titania powder.
Single voltage electro-adsorption and the Treatment by Photocatalysis Oxidation trivalent arsenic solution of applying, after measured, its clearance is respectively 6.7%, 66.7%, and the trivalent arsenic solution of processing through above-mentioned condition, after measured, its clearance is 86.7%, has preferably oxidation removal effect.
Adopt as shown in Figure 3 reactor, the arsenic solution 250mL that in reactor, adds 0.25mg/L, regulate pH=7, adding sodium sulfate adjusting specific conductivity is 158 μ s/cm, power is that the ultraviolet lamp of 100W places inside reactor, 0.25g it is anode that the carried titanium dioxide activated carbon fiber places inside reactor, take activated carbon fiber as negative electrode, applying groove is pressed 1V, the dark 3h of placement makes it reach adsorption equilibrium after adding the carried titanium dioxide activated carbon fiber, UV illumination 60 minutes, sorbent material are 0.03g active oxidation aluminium powder form.
Single voltage electro-adsorption and the Treatment by Photocatalysis Oxidation trivalent arsenic solution of applying, after measured, its clearance is respectively 6.7%, 91.3%, and the trivalent arsenic solution of processing through above-mentioned condition, after measured, its clearance is 99.7%, and arsenic concentration is lower than 0.01mg/L, reaches " drinking water sanitary standard ".
Claims (5)
1. the method for activated carbon fiber hydrothermal method carried titanium dioxide photoelectrocatalysioxidization oxidization arsenic removal is characterized in that comprising the steps:
(1) take by weighing the 10g tetrabutyl titanate in Erlenmeyer flask, add successively 45mL dehydrated alcohol and 20mL glacial acetic acid, magnetic agitation 30min is mixed into A liquid; Add 25mL dehydrated alcohol, 6.5mL redistilled water and 5mL glacial acetic acid in another Erlenmeyer flask, magnetic agitation 30min is mixed into B liquid; B liquid is splashed in the A liquid in the magnetic agitation with 1 drops/sec speed with separating funnel, and stirring velocity is 300r/min, drips off rear continuation and stirs 3h;
(2) measure the autoclave that the above solution of 60mL and activated carbon fiber place inner liner polytetrafluoroethylene, described autoclave effective volume 100mL, pressure 10MPa, adopt hydrothermal method, prepare the carried titanium dioxide activated carbon fiber at 120 ~ 200 ℃ of lower reaction 1 ~ 5h, behind the ultrasonic cleaning 5min, in 105 ℃ of dry 12h, stand-by;
(3) photoelectrocatalysioxidization oxidization carries out under 4 ~ 1000W ultra violet lamp; Adopt the carried titanium dioxide activated carbon fiber as anode, activated carbon fiber is as negative electrode, and impressed voltage is set to 0.1 ~ 1V; Because arsenic containing solution is As
2O
3Be dissolved in the NaOH solution and obtain, regulator solution pH is 6.5 ~ 8.5 before the catalysis; In arsenic containing solution, add sodium sulfate and be 100 ~ 1000 μ s/cm as ionogen regulator solution specific conductivity, close with the tap water specific conductivity; Place the dark whip attachment 3h of arsenic containing solution to make it reach adsorption equilibrium the carried titanium dioxide activated carbon fiber before the UV illumination, UV illumination 20 ~ 120min; Remove pentavalent arsenic with arsenic-removing adsorption agent after the illumination.
2. the method for claim 1, it is characterized in that: the mass ratio of described titanium dichloride load amount and activated carbon fiber is 0.2 ~ 1.0%.
3. the method for claim 1, it is characterized in that: the titanium dioxide of described load is nano titanium oxide.
4. the method for claim 1, it is characterized in that: used sorbent material comprises it being titanium dioxide, ferriferous oxide, iron hydroxide, Mn oxide, activated alumina or gac above-mentioned steps 3).
5. the method for claim 1, it is characterized in that: described carried titanium dioxide activated carbon fiber is reused.
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