CN102910767B - 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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- CN102910767B CN102910767B CN201210394589.9A CN201210394589A CN102910767B CN 102910767 B CN102910767 B CN 102910767B CN 201210394589 A CN201210394589 A CN 201210394589A CN 102910767 B CN102910767 B CN 102910767B
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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 a kind of method that 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
Occurring in nature arsenic element is extensively present in the food chain of soil, rock, water body and animal and plant body.At China's drinking water type distribution of endemic arsenism, in 8 provinces, cities and regions, influenced population is more than 200 ten thousand people nearly, and 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, when serious because cerebral palsy is dead.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.Arsenic pollutes the method for processing arsenic pollutant effluents at present and mainly contains: absorption method, Coagulation Method, ion exchange method, biological process, electrocoagulation, pressure membrane driving method etc., yet there is limitation separately, as titanium dioxide has good adsorptive power to arsenic, stable chemical nature, acid and alkali-resistance, can not introduce by product and toxic substance after polluted water is processed.When titanium dioxide is subject to photon energy that wavelength is less than or equal to 387.5nm and irradiates, the transition of electron of valence band to conduction band, thereby produced light induced electron (e
-)-hole (h
+) right.The h producing
+the OH of titanium dioxide surface will be adsorbed on
-and H
2o is oxidized to hydroxyl radical free radical; Electronics (e
-) react with surperficial oxygen molecule, finally may generate hydroxyl radical free radical, hydroxyl radical free radical has very strong oxidation capacity, As in water (III) can be oxidized to As (V).U.S. Patent number US20090364505 adopts doping metals or nonmetallic titania powder As (III) in photochemical catalytic oxidation water under radiation of visible light, the effect of arsenic removal is better, yet, powder titanium dioxide particle is very little, suspending phase catalyzer is difficult to be regained, cost is high, is not suitable for directly usining powder titanium dioxide as oxidation As (III) catalyzer.
The toxicity of As (III) and transport property are greater than As (V), and in most of natural water, As (III) is with neutral substance (H
3asO
3) exist, and As (V) is with ionic species (H
2asO
4 -or HAsO
4 2-) exist, the As of ionic species (V) more easily removes than As (III) by absorption or flocculation sediment, and therefore most of Technology Needs are oxidized to pentavalent arsenic by trivalent arsenic in advance.In addition, research shows that the toxicity of arsenide has very big-difference, the arsenide toxicity AsH of various forms
3>As (III) >As (V) >MMA>DMA.The As existing with arsenite (III) exceeds 60 times than the toxicity of the As (V) existing with arsenate form.Therefore, As (III) is oxidized to As (V), both can improves the clearance of arsenic, can reduce toxicity again.At present, having scholar to take hypochlorite, oxygen, ozone, potassium permanganate etc. is oxygenant, adopt chemical oxidization method to be studied arsenious oxidation, as China Patent No. ZL02155224.X adopts ozone, As (III) is oxidized to As (V), 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 of method easily to cause the secondary pollution of tap water, should not in Drinking Water, use.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 is used gac, and between activated carbon granule and particle, contact resistance is larger, 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 current 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 easily oxidized under the oxidizing atmosphere higher than 500 ℃, therefore the physicals strength and modulus of charcoal filamentary material can weaken greatly.General carrying method as the physical vaporous depositions such as atomic layer deposition method, sputtering method, laser assisted molecular beam sedimentation, ionization Cluster Method, chemical Vapor deposition process load temperature is high and sol-gel method must high-temperature roasting crystallization, must carrier active carbon fibrous physics physical strength be caused to a certain degree and be destroyed.If use binding agent by the TiO preparing in advance
2powder is loaded in activated carbon fiber, can reduce to a certain extent TiO
2activity, general binding agent is organism, after long-time use, easily produce slight crack and even peel off, and likely slowly stripping water body is caused to secondary pollution.
Adopt hydrothermal method to prepare at a lower temperature the anatase-type nanometer titanium dioxide that photocatalytic activity is high, hydrothermal method load only need be placed in presoma and activated carbon fiber autoclave and in 200 ℃, react for some time and prepare the anatase-type nanometer titanium dioxide that photocatalytic activity is high.Hydrothermal method is without not destroying 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 reacting in unit surface increases, and is more conducive to improve photocatalysis efficiency.When grain diameter is 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.
Photoelectrocatalysis technology is surface coverage TiO
2the conductor of film is as light anode, and separately establishes a noble electrode, and under the effect of extra electric field, in semi-conductor, light induced electron can be by more effectively separated with hole (current carrier), and this electric field reinforcing effect has reduced simple composite significantly, use 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 to (comparing with semiconductive particles) with the oxidising process in valence band hole from locus, 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 cathodic reduction water
+, therefore do not need to blast the oxygen as electron capture agent in system.Therefore,, in containing arsenic superstandard drinking water, first-selected photoelectrocatalysioxidization oxidization technology is rational.
Summary of the invention
The object of the invention is to solve in prior art and can not effectively remove trivalent arsenic, the problem that arsenic removal cost is high, provides a kind of drinking water treatment method that has more using value, reaches the low-cost object 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 application widely by modes such as physical adsorption, chemisorption and physical and chemical adsorption in fields such as waste water, off gas treatment, solution recovery, water purifications.By electrochemical applications, in oxidation trivalent arsenic, be a kind of method of novel treatment Arsenic in Drinking Water.Utilize the various over-all properties of conduction, absorption and form of activated carbon fiber, using it as a kind of novel photochemical catalyst electrode, for tap water, remove arsenic and have broad prospects.
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; By toxicity, large and unmanageable trivalent arsenic is oxidized to pentavalent arsenic.Finally, adopt high-efficient arsenic-removing sorbent that pentavalent arsenic is removed completely.
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 to 30min at 80 ℃ of 1mol/L sodium hydroxide solutions, water cleans up rear use 68% nitric acid constant temperature 4h at 115 ℃, puts into 105 ℃ of dry 12h of baking oven after water cleans up.
Take 10g tetrabutyl titanate in Erlenmeyer flask, add successively 45mL dehydrated alcohol and 20mL glacial acetic acid, magnetic agitation 30min, is mixed into A liquid; In another Erlenmeyer flask, add 25mL dehydrated alcohol, 6.5mL redistilled water and 5mL glacial acetic acid, magnetic agitation 30min, is mixed into B liquid; By B liquid, with separating funnel, the speed with 1 drop/sec splashes in the A liquid in magnetic agitation, and stirring velocity is 300r/min, drips off rear continuation and stirs 3h;
Measure the above solution of 60mL and activated carbon fiber and be placed in the autoclave of inner liner polytetrafluoroethylene, described autoclave effective volume 100mL, pressure 10MPa, adopt hydrothermal method, at 120 ~ 200 ℃, react 1 ~ 5h and prepare carried titanium dioxide activated carbon fiber, after ultrasonic cleaning 5min, in 105 ℃ of dry 12h, stand-by;
Photoelectrocatalysioxidization oxidization carries out under 4 ~ 1000W ultra violet lamp; Adopt 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 NaOH solution and obtain, before catalysis, regulator solution pH is 6.5 ~ 8.5.In arsenic containing solution, add sodium sulfate to be 100 ~ 1000 μ s/cm as ionogen regulator solution specific conductivity, close with tap water specific conductivity; Before UV illumination, carried titanium dioxide activated carbon fiber is placed in to the dark whip attachment 3h of arsenic containing solution and makes it reach adsorption equilibrium, UV illumination 20 ~ 120min; After illumination, with arsenic-removing adsorption agent, remove pentavalent arsenic.Obtain meeting the tap water of < < drinking water sanitary standard > > (GB5749-2006).
Described titanium dichloride load amount and the mass ratio of activated carbon fiber are 0.2 ~ 1.0%.
The titanium dioxide of described load is nano titanium oxide.
Above-mentioned steps 3) in, sorbent material used comprises it being titanium dioxide, ferriferous oxide, iron hydroxide, Mn oxide, activated alumina or gac.
Described carried titanium dioxide activated carbon fiber is reused.
By toxicity, large and unmanageable trivalent arsenic is oxidized to pentavalent arsenic in the present invention.Finally, adopt high-efficient arsenic-removing sorbent that pentavalent arsenic is removed completely.
beneficial effect of the present invention:
(1) the present invention is used in arsenic polluted drinking water process field first using activated carbon fiber as electrode.Highly toxic trivalent arsenic can be oxidized to pentavalent arsenic, and by adsorption tower, the pentavalent arsenic after being oxidized be carried out to active adsorption, reduce the consumption of sorbent material, reduce regeneration times, realize 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 that light induced electron is separated with hole, now water can be by electrolysis, low investment and low operational and administrative expenses, can large-scale application, has environmental benefit and the social benefit of highly significant, simple to operate, operational management is convenient, and in overall operation, has reduced to greatest extent the exposure of pollutent, environmentally friendly.
(3) the present invention does not produce sludge silt, does not need to carry out secondary treatment, and simple to removing the method for arsenic in tap water, the very economical arsenic removal object that effectively reaches, is conducive to big area large-scale promotion.
Accompanying drawing explanation
The TiO of Fig. 1 embodiment 1 preparation
2transmission 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 schematic diagram of the present invention.
Wherein: 1. 3. arsenic-containing water taphole 8. ultraviolet lamp 9. quartz socket tubes of voltage stabilized source 4. arsenic-containing water solution entrance 5. sewage draining exit 6. arsenic-removing adsorption agents 7. before processing after processing of carried titanium dioxide activated carbon fiber 2. activated carbon fiber (ACF).
Embodiment
For a better understanding of the present invention, below in conjunction with embodiment, the invention will be further described, but the scope of protection of present invention is not limited to the scope described in embodiment.
Take 10g tetrabutyl titanate in Erlenmeyer flask, add successively 45mL dehydrated alcohol and 20mL glacial acetic acid, magnetic agitation 30min, is called A liquid.In another Erlenmeyer flask, add 25mL dehydrated alcohol, 6.5mL redistilled water and 5mL glacial acetic acid, magnetic agitation 30min, is called B liquid.By B liquid, with separating funnel, the speed with 1 drop/sec splashes in the A liquid in magnetic agitation, and stirring velocity is controlled as 300r/min, drips off rear continuation and stirs 3h.
Measure the above solution of 60mL and activated carbon fiber and be placed in autoclave (the effective volume 100mL of inner liner polytetrafluoroethylene, pressure 10MPa, compactedness 60%) in, in baking oven, at 180 ℃, react 3h and prepare carried titanium dioxide activated carbon fiber, after ultrasonic cleaning 5min, in 105 ℃ of dry 12h.
embodiment 2
Adopt reactor as shown in Figure 3, the arsenic solution 250mL that adds 2mg/L in reactor, regulate pH=7, adding sodium sulfate to regulate specific conductivity is 158 μ s/cm, and the ultraviolet lamp that power is 9W is placed in inside reactor, and it is anode that 0.25g carried titanium dioxide activated carbon fiber is placed in inside reactor, take activated carbon fiber as negative electrode, applying groove is pressed 0.5V, add carried titanium dioxide activated carbon fiber after the dark 3h of placement make it reach adsorption equilibrium, UV illumination 20 minutes.Sorbent material is 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 good oxidation removal effect.
Adopt reactor as shown in Figure 3, the arsenic solution 250mL that adds 0.25mg/L in reactor, regulate pH=7, adding sodium sulfate to regulate specific conductivity is 158 μ s/cm, power is that the ultraviolet lamp of 100W is placed in inside reactor, it is anode that 0.25g carried titanium dioxide activated carbon fiber is placed in inside reactor, take activated carbon fiber as negative electrode, applying groove is pressed 1V, after adding carried titanium dioxide activated carbon fiber, the dark 3h of placement makes it reach adsorption equilibrium, UV illumination 60 minutes, sorbent material is 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%, arsenic concentration, lower than 0.01mg/L, reaches < < drinking water sanitary standard > >.
Claims (5)
1. a method for activated carbon fiber hydrothermal method carried titanium dioxide photoelectrocatalysioxidization oxidization arsenic removal, is characterized in that comprising the steps:
(1) take 10g tetrabutyl titanate in Erlenmeyer flask, add successively 45mL dehydrated alcohol and 20mL glacial acetic acid, magnetic agitation 30min, is mixed into A liquid; In another Erlenmeyer flask, add 25mL dehydrated alcohol, 6.5mL redistilled water and 5mL glacial acetic acid, magnetic agitation 30min, is mixed into B liquid; By B liquid, with separating funnel, the speed with 1 drop/sec splashes in the A liquid in magnetic agitation, 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 are placed in inner liner polytetrafluoroethylene, described autoclave effective volume 100mL, pressure 10MPa, adopt hydrothermal method, at 120 ~ 200 ℃, react 1 ~ 5h and prepare carried titanium dioxide activated carbon fiber, after ultrasonic cleaning 5min, in 105 ℃ of dry 12h, stand-by;
(3) photoelectrocatalysioxidization oxidization carries out under 4 ~ 1000W ultra violet lamp; Adopt 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 NaOH solution and obtain, before catalysis, regulator solution pH is 6.5 ~ 8.5; In arsenic containing solution, add sodium sulfate to be 100 ~ 1000 μ s/cm as ionogen regulator solution specific conductivity, close with tap water specific conductivity; Before UV illumination, carried titanium dioxide activated carbon fiber is placed in to the dark whip attachment 3h of arsenic containing solution and makes it reach adsorption equilibrium, UV illumination 20 ~ 120min; After illumination, with arsenic-removing adsorption agent, remove pentavalent arsenic.
2. the method for claim 1, is characterized in that: described titanium dichloride load amount and the mass ratio of activated carbon fiber are 0.2 ~ 1.0%.
3. the method for claim 1, is characterized in that: the titanium dioxide of described load is nano titanium oxide.
4. the method for claim 1, is characterized in that: above-mentioned steps 3), sorbent material used comprises it being titanium dioxide, ferriferous oxide, iron hydroxide, Mn oxide, activated alumina or gac.
5. the method for claim 1, is characterized in that: described carried titanium dioxide activated carbon fiber is reused.
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| CN113684679B (en) * | 2021-07-29 | 2023-11-03 | 超越者新材料科技河北有限公司 | Preparation method and application of carbon fiber-based nanocomposite |
| CN114162912B (en) * | 2021-11-04 | 2023-09-26 | 泉州南京大学环保产业研究院 | Preparation method of high {001} crystal face-loaded titanium dioxide particle electrode |
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