CN1830830A - Method of eliminating mitrogen in water by photo catalysis - Google Patents
Method of eliminating mitrogen in water by photo catalysis Download PDFInfo
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- CN1830830A CN1830830A CNA2006100461728A CN200610046172A CN1830830A CN 1830830 A CN1830830 A CN 1830830A CN A2006100461728 A CNA2006100461728 A CN A2006100461728A CN 200610046172 A CN200610046172 A CN 200610046172A CN 1830830 A CN1830830 A CN 1830830A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
A photocatalytic process for removing N from water and generating N2 features that the metal carried or N doped TiO2 catalyst is used, the photocatalytic oxidizing to NH3-N is combined with photocatalytic reducing to oxidized N, and the ferrous ions are added to increase the denitrifying efficiency by 40-100%.
Description
Technical field
The invention belongs to environment and technical field of chemical engineering.Relate to water body denitrification, specially refer to the method for photochemical catalysis water body denitrification.
Background technology
Water body denitrification often adopts biotechnology: microorganism finally is converted into nitrogen with the inorganic nitrogen composition, makes nitrogen content reduction in the water.Ammonia oxidation bacteria energy oxidation ammonia nitrogen forms nitrous acid nitrogen and nitric nitrogen.Denitrifying bacteria can produce nitrogen with nitric nitrogen/nitrite nitrogen reduction.The microorganism anammox bacterium that one class is special has special enzyme, can form nitrogen product simultaneously directly with ammonia nitrogen oxidation and the reduction of nitrous acid nitrogen under low dissolved axygen or anaerobic existence condition.Advantageous aspect nitric efficiency and system energy consumption.
The existing problems 1 of biological denitrificaion.The water of carrying out a biological disposal upon need be carried out advanced treatment as sterilization, clarification filtration, or, could obtain than higher water quality through membrane sepn, reverse-osmosis treated.2。The anaerobic oxidation technology of ammonia generally is applicable to the processing of high-concentration wastewater containing ammonia nitrogen.3。Can not handle the water decontamination cycle Treatment for Reuse during the sewage 4. space shuttle space flights that contain higher ammonia nitrogen and difficult degradation toxic organic compound simultaneously, should not adopt.In addition, water quality is relatively preferably in the micro-polluted water, and the nitrogenous source pollutant load may be lower, exist with multi-form, as ammonia nitrogen or nitrous acid nitrogen, nitric nitrogen etc.Though these composition content are low, and are very harmful to HUMAN HEALTH especially infant.Only the place to go treatment process with regard to ammonia nitrogen has zeolite adsorption, methods such as stripping, but these methods have zeolite regeneration and secondary pollution problem [Zhang Linsheng chief editor, the advanced treatment of water and reuse technology, Chemical Industry Press, 2004 Beijing p207].Micro-polluted water matter, especially tap water is suitable for adopting chemical process: remove nitrous acid nitrogen, nitrate nitrogen as the catalytic hydrogenating reduction technology; And senior catalyzed oxidation technology one ozone oxidation, electrolysis, photochemical catalysis are handled.The technology of suitable denitrogenation is a photocatalysis technology.Utilize the light-catalyzed reaction of metal-doped catalyst, oxidative deamination nitrogen [Jae SangLee, et al.Selective photocatalytic oxidation of NH as the investigator of Korea S
3To N
2On platinzedTiO
2In water[J] .J.Environ.Sci.Technol, 2002,36 (24): 5462-5468].Photochemical catalysis not only can oxidation process denitrification, can also carry out photo catalytic reduction with organic oxidation coupling, transforms and removes nitric nitrogen and nitrite nitrogen.Utilize metatitanic acid hydrate/Cadmium Sulfide catalyzer as the Japanology person, the catalysis nitro-reduction reaction forms nitrogen or ammonia [sato in the presence of methyl alcohol, tsugio, et al, journal ofchemical technology and biotechnology 1996,67 (4), 345 ~ 349, and journalof material science letters, 1996,15 (10), 874 ~ 877].Nickel/zinc sulphide is nitro, nitroso-group light-catalyzed reaction meeting formation hydrogen, nitrogen, ammonia and nitroso-group product [Kato H when methyl alcohol exists and under the visible light photograph, Kudo A, physical chemistry chemical physics, 2002,4 (12), 2833 ~ 2838, Mori T, suzuki, journal of sol-gel science and technology 2000,19 (1`3), 505 ~ 501].But in the system of opening with atmosphere communicates, removing nitro with titanium dioxide and high voltage mercury lamp photochemical catalysis needs for a long time, and seventy or eighty hours can transform about 30%.[Bems?B，JentoftF?C，Schlogl?R，applied?catalysis?B，environmental，1999，20(2)，155-163]。
Except the photochemical catalysis denitrification reaction, the metal catalytic hydrogenation reaction is used to handle/reduce the water that contains nitric nitrogen, at this moment needs to feed in water hydrogen [Gao wenliang et al, catalysis letter, 2003,91 (1 ~ 2) 25 ~ 30 and 345 ~ 349].
The photochemical catalysis ammonia nitrogen removal forms more oxidation state nitrogen compound under the general condition, and it is higher that especially over oxidation forms oxidation state nitrogen-containing products ratio, and the selectivity that forms nitrogen is not high, thus nitric efficiency and the denitrogenation degree is not really high, inadequately fully, thorough inadequately.And the photocatalytic degradation of itrogenous organic substance can form ammonia nitrogen or nitric nitrogen mineral products in the water body.Such water quality needs further to handle.Water body denitrification usually will face ammonia nitrogen and oxidation state nitrogen while coexisting state.
Photo catalytic reduction removal nitric nitrogen obtains nitrite nitrogen needs the time longer, and speed is slower.Denitrogenation is not thorough, and more water-soluble products is arranged, and extra catalyst formation component is many, preparation is complicated.The safety of water quality transforms and the water body recycle, should reach higher water quality requirement, but lacks such effective means now.
Summary of the invention
The present invention seeks to by light-catalyzed reaction, realize the efficient and denitrogenation comparatively completely of water body.The oxidizing reaction of photochemical catalysis ammonia nitrogen and the reduction reaction of oxidation state nitrogen being coupled together,, reducing the formation of other by product, realize in the water efficiently, denitrogenation comparatively completely by improve forming the selectivity of nitrogen product.Improve denitrogenation processing efficient and effect.
Technical solution of the present invention is to adopt photocatalysis method, feed nitrogen or argon gas, to remove or to reduce the oxygen in water level, in immobilization film catalyst reactor or outstanding slurry reactor, utilize the titanium dioxide composite catalyst of metal load nano titania catalyzer or nitrating.Under UV-light or visible light radiation, the hole/electron pair that utilizes photochemical catalysis to produce with oxidation/reductive action, and follow-up generation have an oxygenizement hydroxyl radical free radical, acts on ammonia nitrogen and high price/oxidation state nitrogen (nitro, nitroso-group) in the water.Transform ammonia-state nitrogen and the nitric nitrogen/nitrous acid nitrogen that removes in the water simultaneously.Light source can be sunlight, indoor light source or ultraviolet source, and used photocatalyst can be: nitrating titanium dioxide; Metal-doped titanium dioxide etc.In liquid, add the removal effect that ferrous ion can effectively improve various nitrogen.
The reactor types that this invention is used can be various photo catalysis reactors.As: 1. ring-type crystal reaction tube, ultraviolet lamp is placed in the reaction tubes.2. catalyzer can be compounded on flat board or the mesopore filter membrane, sinks in the water, stirs by feeding gas.3. catalyzer is suspended in the reactor, and water outlet is through filter membrane and catalyst separating.
Noble metal support/photocatalysis coupled redox denitrogenation adds ferrous ion, improves the effect catalyzed oxidation of coupling light catalyzed oxidation and reduction denitrogenation and the effect of reduction denitrogenation, and this is that a kind of catalyst action causes the " original position " coupling of reaction.Utilize the TiO that carries argent of photo catalytic reduction method preparation
2Catalyzer, uviolizing, the test of ring-type quartz reactor: proved photochemical catalytic oxidation reduction coupling reaction denitrification activity.With the variation of silver carrying amount, the photochemical catalysis denitrification effect presents an optimum value, and the charge capacity scope that obtains denitrification activity optimum value silver is in 0.1～2.9%; Nitrogen for the condition of protection gas under the transformation efficiency of total nitrogen, ammonia nitrogen, nitrous acid nitrogen all apparently higher than make the effect that stirs gas and drive carrier of oxygen of argon gas; In reaction system, add Fe
2+The carrying out that helps photochemical catalytic oxidation and reduction reaction improved the clearance of total nitrogen greatly.
The acid-alkali accommodation method, emphasis transforms oxidation state nitrogen emphasis conversion removal ammonia-state nitrogen under alkaline condition then under acidic conditions earlier.It is the photocatalysis coupled denitrogenation on a kind of time series.
Nitrating titanium dioxide composite catalyst catalysis ammonia nitrogen under visible light/daylight efficiently is converted into nitrogen product, has avoided over oxidation to form oxidation state nitrogen, belongs to " gentleness " oxidation, " efficiently " practical denitride technology.
Effect of the present invention and benefit are because the photocatalysis oxidation reaction of ammonia nitrogen and the photo catalytic reduction effect reduction reaction to oxidation state nitrogen that has been coupled, improved the ratio of photochemical catalysis formation nitrogen product, avoid the mutual conversion between the water-soluble nitrogenous mineral compound of different valence state in the light-catalyzed reaction process, thereby improved the effect of photochemical catalysis denitrogenation.This method can be used for the nitrogenous purification of water quality of little contamination type, nitrogenous middle water treatment or contains the sewage disposal of low concentration micro quantity organic pollutant, ammonia nitrogen or mixed valence inorganic nitrogen.
Embodiment
Be described in detail most preferred embodiment of the present invention below in conjunction with technical scheme.
Photochemical catalysis denitrification reaction embodiment:
Embodiment one
Noble metal support/photocatalysis coupled redox denitrogenation adds ferrous ion, improves the effect catalyzed oxidation of coupling light catalyzed oxidation and reduction denitrogenation and the effect of reduction denitrogenation, and this is that a kind of catalyst action causes the " original position " coupling of reaction.
Catalyst levels 1g/L, ultraviolet germicidal (20 watts) feed nitrogen for protection gas, shine 2～4 hours, utilize Ag/TiO2, Ag charge capacity 0.2～2.5%; PH=9～10.21), when water body contained ammonia nitrogen～25mg/l and nitrous acid nitrogen～25mg/L, the photochemical catalysis denitrification effect is: total nitrogen was removed 38% (ammonia nitrogen, nitrous acid nitrogen reach 48%, 27% respectively).(5～50mg/l), nitrogen removal rate can reach 64% to add ferrous ion.(ammonia nitrogen, nitrous acid nitrogen reach 88%, 43% respectively)
Adding Fe
2+Reaction in, detect the generation of a spot of nitrate nitrogen, but do not influence total nitrogen removal effect, i.e. Fe
2+To Ag/TiO
2The activity of photocatalyst has significant promotion.
If utilize argon gas to do protection gas, stir and remove dissolved oxygen, under the similarity condition, 1～4 hour total nitrogen is removed has only 10～50%, ammonia nitrogen removal frank 40%, nitrous acid nitrogen 12%.Do microgas with nitrogen under the similarity condition, ammonia nitrogen removal frank can reach 82%.Nitrogen removal rate also reaches 62%.
Embodiment two
The acid-alkali accommodation method, emphasis transforms oxidation state nitrogen emphasis conversion removal ammonia-state nitrogen under alkaline condition then under acidic conditions earlier.It is the photocatalysis coupled denitrogenation on a kind of time series.
Adopt immobilized supportedly at titanium dioxide on glass (2cm*4cm), feeding under the condition of nitrogen, (total nitrogen 50mg/l, ammonia nitrogen and nitrous acid nitrogen respectively account for half) the nitrogenous water body with in the ultra violet lamp silica tube carries out light-catalyzed reaction.Add carbon source such as formic acid regulator solution pH, photochemical catalysis removes nitrous acid nitrogen under acid pH 2～4 conditions earlier, and major part can be converted into nitrogen.If react 1～4 hour, can remove 88% nitrous acid nitrogen.If regulate pH2～5 then when transforming nitrous acid nitrogen, form some ammonia nitrogens.Reacted 0.25～2 hour if make to be reflected under the acidic conditions, with being transferred to alkaline range on the pH as＞9.6, proceed light-catalyzed reaction then, then total nitrogen and nitrous acid nitrogen, ammonia-N removal rate all can reach 60% after 2～4 hours total reaction times.
The photochemical catalysis denitrogenation of embodiment three nitrating photocatalysts under the visible light condition
Nitrating catalyzer catalysis ammonia nitrogen under visible light efficiently is converted into nitrogen product, has avoided over oxidation to form oxidation state nitrogen, belongs to " gentleness " oxidation, " " is practical denitride technology efficiently.
Light-catalyzed reaction is 250ml at volume, and diameter is to carry out in the silica tube of 32mm.Used ultraviolet source be emission wavelength be 254nm and with reactor at a distance of the 20W UV-lamp of the parallel placement of 6cm, daylight photochemical catalysis test is light source (Dalian December, sunny noon) with the sunlight.The reactive behavior of photocatalyst is estimated by the ammonia nitrogen of mensuration ammoniacal liquor and the clearance of total nitrogen.Add 100ml concentration during reaction in the system and be the ammoniacal liquor of 85mg/L and the catalyst fines of 0.1g (ACF makes template, by the tetrabutyl titanate raw material through Prepared by Sol Gel Method, the atomic ratio that obtains Ti and N is 1: 0.19), guarantee O in the reaction system by blasting air (flow is 100ml/min)
2Concentration and reaction solution in catalyzer be in suspended state. the sample of taking a sample at regular intervals filters through filter membrane (aperture 0.22 μ m).Total nitrogen is measured with Tianjin, island TOC-VCPH-TNM-1 determination of total nitrogen content instrument.The nessler reagent metric measurement is adopted in the ammonia nitrogen analysis
[14]752 ultraviolet-visible pectrophotometers of using sea light spectrometer company limited are measured the filtrate absorbancy and converted according to typical curve under λ=420nm become corresponding concentration.
Ultraviolet lighting reaction 1～5 hour, ammonia nitrogen removal frank can reach 60%, and nitrogen removal rate can reach 45%.Reacted under the sun exposure condition 1～5 hour, ammonia nitrogen, nitrogen removal rate reach respectively: 45% and 30%.
If catalyzer total nitrogen content height, then speed of response is fast; If total nitrogen content is low, speed of response is slow.1: 1-NH4-N: NO2-N, 50～60mg/L, UV-light reaction 1～6 hour, nitrogen removal rate can reach 68%.If nitrogen concentration improves in the water body, speed of reaction also improves.
Under the similarity condition, if do not use the nitrating catalyzer, the oxidation of ammonia nitrogen, the removal effect of total nitrogen are all relatively poor, and for the titanium dioxide composite catalyst of nitrating, ammonia nitrogen removal and changing effect descend 10 ~ 40%.
Claims (3)
1. a photochemical catalysis removes the method for nitrogen in the water, it is characterized in that feeding nitrogen, under nitrogen atmosphere and under metal load or the effect of nitrating composite titanium dioxide photocatalyst, carry out light-catalyzed reaction, by the oxidizing reaction removal of ammonia and nitrogen, react nitric nitrogen and the nitrite nitrogen that removes oxidation state by photo catalytic reduction, the coupling of two reactions can take place simultaneously; The ratio of the ammonia nitrogen in the removal water and the inorganic nitrogen of oxidation state 1: 1～2: 1; The photocatalysis coupled denitrification reaction of water body is when adding ferrous ion, and nitric efficiency and degree increase by 40% ~ 100%; Utilize the adulterated titanium deoxide catalyst of nitrogen to expand the scope that catalyzer utilizes visible light, oxidation ammonia nitrogen and denitrification effect exceed not nitrating titanium dioxide composite catalyst 10 ~ 40% under ultraviolet lighting or sun exposure.
2. 1 described a kind of photochemical catalysis removes the method for nitrogen in the water according to right, it is characterized in that if contain organic carbon in the water, photochemical catalytic oxidation/mineralising organism and water photochemical catalysis denitrification reaction carry out simultaneously, and organic having is beneficial to photo catalytic reduction removal nitric nitrogen and nitrite nitrogen; But nitric nitrogen/nitrite nitrogen content exceeds 1 times of ammonia-nitrogen content or more for a long time, Xiang Shuizhong adds organic carbon source, and light-catalysed oxidizing reaction and reduction reaction are removed organic carbon and oxidation state nitrogen respectively; Proceed coupling light catalysis denitrification reaction according to the new ratio that forms ammonia nitrogen and oxidation state nitrogen then.
3. 1 described a kind of photochemical catalysis removes the method for nitrogen in the water according to right, it is characterized in that pH value of solution is regulated, and carries out earlier the reduction of nitric nitrogen and nitrite nitrogen under acidic conditions, forms nitrogen or ammonia; The oxidation of ammonia is carried out in the back under alkaline condition; Be the photo catalytic reduction reaction on the time sequence and the coupling of photocatalysis oxidation reaction.
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| CN106315755A (en) * | 2016-10-13 | 2017-01-11 | 天津工业大学 | Method for removing nitrate nitrogen from water by photocatalytic reduction |
| CN107051337B (en) * | 2017-06-16 | 2023-01-31 | 云南大学 | Non-equilibrium state photocatalytic reaction device and application thereof |
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| CN108975507A (en) * | 2018-07-31 | 2018-12-11 | 苏州科技大学 | The method that zinc ferrite-fullerene photochemical catalyst removes nitrite and ammonia nitrogen simultaneously |
| CN108975506B (en) * | 2018-07-31 | 2021-08-06 | 苏州科技大学 | Method for removing nitrite and ammonia nitrogen by zinc ferrite-activated carbon photocatalysis |
| CN108975507B (en) * | 2018-07-31 | 2021-08-13 | 苏州科技大学 | Method for simultaneously removing nitrite and ammonia nitrogen by using zinc ferrite-fullerene photocatalyst |
| CN110803736A (en) * | 2019-11-14 | 2020-02-18 | 天津理工大学 | Bionic denitrification method for wastewater containing low-concentration nitrate and/or nitrite |
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