CN104289708A - Aluminum iron alloy powder material and method for reducing and degrading nitrate or chlorine disinfection by-products in water with same - Google Patents
Aluminum iron alloy powder material and method for reducing and degrading nitrate or chlorine disinfection by-products in water with same Download PDFInfo
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- CN104289708A CN104289708A CN201410482530.4A CN201410482530A CN104289708A CN 104289708 A CN104289708 A CN 104289708A CN 201410482530 A CN201410482530 A CN 201410482530A CN 104289708 A CN104289708 A CN 104289708A
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Abstract
The invention discloses an aluminum iron alloy powder material for reducing and degrading nitrate or chlorine disinfection by-products in water. The aluminum iron alloy powder material is prepared through the following steps that (a) iron ingots and pure aluminum are heated and melted for one to two hours at the temperature ranging from 1000 DEG C to 1800 DEG C; (b) the melted aluminum iron alloy is cooled and smashed to obtain the aluminum iron alloy powder material. The invention further discloses a method for reducing and degrading the nitrate or the chlorine disinfection by-products in water. Water, containing the degrading nitrate or the chlorine disinfection by-products, to be treated is made to pass through a filter column filled with the aluminum iron alloy powder material. The method for reducing and degrading the nitrate or the chlorine disinfection by-products in the water has the advantages that the method is economical and efficient, and operation is easy, and the aluminum iron alloy powder material and the method have good economic and environmental benefits.
Description
Technical field
The invention belongs to water treatment field, be specifically related to new material and the method for nitrate and chlorine disinfection by-product in a kind of deoxidization, degradation process water.
Background technology
Along with improving constantly of industrialized level, the existing water body more than 25% in the whole world is contaminated, how to process polluted water body and makes it be converted into safe drinking water, become we mankind have to faced by a significant task.
After former water enters water factory while disinfectant carries out sterilizing in use, the substance reactions such as natural organic matter, humic acid and man-made pollutant in disinfectant chlorine and former water produce DBPs----carbon tetrachloride, chloroform, trichloroacetic acid etc. to human health.These chlorine disinfection by-products harm Environmental security, with healthy, cause damage to the nervous system of human or animal, liver or kidney etc. and has " three cause " effect (carcinogenic, teratogenesis, mutagenesis).According to national drinking water standard, the content of carbon tetrachloride in water body must not more than 2 μ g/L, and the content of chloroform in water body must not more than 60 μ g/L, and the content of trichloroacetic acid in water body must not more than 100 μ g/L.
In water, azotate pollution produces primarily of human being's production and life, and agricultural fertilizer, sanitary sewage, industrial wastewater etc. enter body of groundwater after oozing under leaching.Drinking the underground water after by azotate pollution can serious harm health.Nitrate is reduced to nitrite under nitrate reduction bacterium and metabolism in people's enteron aisle, can cause " blue baby is sick "; In addition, nitrate also easy induced tumor disease.World Health Organization's regulation Nitrate In Drinking Water content should be no more than 50mg/L, and content of nitrite is no more than 3mg/L, and (nitrate concentration/50+ nitrite concentration/3)≤1mg/L.Environmental Protection Agency and the most ceiling value of Canadian environmental organization regulation nitrate are 10mg-N/L, and the most ceiling value of nitrite is 1mg-N/L.
In domestic and international removal water, the main method of DBPs has physical method and the electronation edman degradation Edmans such as vaporizing extract process, extraction, absorption method.Chemical reduction method commonly utilizes the reproducibility of metal self to degrade organic chlorine-containing compound, thus is removed one by one by the chlorine element in organic chlorine-containing compound, makes it become nontoxic chlorion and hydro carbons.Simple substance iron powder is cheap, has stronger reproducibility, is widely used in the chlorine organic in deoxidization, degradation water body.The people such as Helland use fe powder body material to remove the carbon tetrachloride of in water 1.5-5.5 μM, and find under anaerobic, it can remove by Zero-valent Iron fast, and wherein 49% is converted into chloroform.But particle diameter is that the Zero-valent Iron of micron or millimeter is lower to some chlorinated organics reactivity, degraded not exclusively, have a large amount of iron ions to generate, and its surface can form passivation layer, thus cause the decline of degradation rate in the process of degraded.Pure aluminum light weight, reproducibility is strong, but the aluminum oxide film passivation of its surface compact reactivity of aluminium, application is extremely restricted.There is scholar will obtain the degraded of Fe-Al bimetallic material using aluminium as inner layer metal and remove carbon tetrachloride in water, this material prevents the corrosion product of material surface iron from depositing thus keeping ironing surface more new state using Al as electron donor, but obtained Fe-Al bimetallic material is the surface of deposition of iron at alumina particles, easily come off in course of reaction, cause treatment effect unstable.In addition, nano material and being separated in engineer applied of water body are stubborn problems, and the impact of the secondary pollution of the water body nano material that it causes can not be ignored.
In water, the minimizing technology of nitrate mainly contains physical-chemical process, biological denitrification method and chemical reduction method at present.In metal deoxidization removal water, nitrate is swift in response compared with bioanalysis, technique is simple, be suitable for small-sized and dispersion treatment.Zero-valent metal, as Zero-valent Iron, aluminium etc., can effectively remove nitrate in water.Aluminium can effectively remove nitrate in water in the basic conditions.Under weak basic condition (pH=8), alumina particles Surface Creation protective sull, covers metal surface.Along with pH raises, metal surface protection film dissolves gradually, and the metallic aluminium exposed can remove nitrate in water.When pH=10.25, aluminium optionally removes nitrate in water, can reach 70% to nitrate clearance in 10min of 100mg/L.The permeable reactive wall technology that groundwater remediation adopts often, namely inserts Zero-valent Iron as reducing agent in body of wall in contaminated underground water body.When Zero-valent Iron removes nitrate in water, metallic iron surface can form one deck ferriferous oxide or hydroxide passivating layer gradually, thus reduction even stops iron to the further reduction of nitrate.Zero-valent Iron is applied to the removal of nitrate in water usually when low pH.Metallic iron removes nitrate in water, have many problems demand to solve, comprising reaction must carry out in acid condition, and the nitrogen selective of product is not high, iron stripping causes colourity in water outlet to exceed standard, and the generation of oxidation on metal surface thing and hydroxide stops reacts problems such as carrying out further.
The US Patent No. 5,069,800 of Murphy discloses a kind of to the chemical method of denitrogenation of water, nitrate in alternative removal water when the method has sulfate and chlorion to coexist in alkaline solution, and aluminium and water react the material consumed and can almost ignore; Needed for solution reaction, pH value is higher, is applied to water factory's process pH value and is restricted when being the former water of neutral range.The Chinese patent CN102744041A of the people such as Li Fulin discloses permeable reactive barrier packing material removing nitrate and preparation method thereof, reacting packing material is within the walls iron powder, active carbon and the coarse sand that the pretreatment of volume ratio 3:1:6 is arrived, for the repairing and treating of high concentration nitrate IA.The Chinese patent CN 103570114A of the people such as Lu Yongsheng discloses the method for nitrate in a kind of reduction treatment water, reacting, removing the nitrate of more than 95% in 4h containing dropping into patina class material in nitrate wastewater; Nitrogen removal rate 35%.
It is that material surface easily generates metal oxide or hydroxide stops reaction to be carried out further that current employing aluminium or iron simple substance remove main Problems existing in pollutant process; Therefore, pure aluminum and fe need to carry out under specific pH value (alkalescence or acid) usually, to avoid the problem of passivation of metal surfaces as far as possible, and need the work a large amount of pending waste water being carried out to adjust ph in practice, waste time and energy, cost improves.In addition, during with pure aluminum or fe reduction nitrate, in nitrate reduction product, ammonia nitrogen proportion is higher, and the nitrate transformation even more than 90% is ammonia nitrogen; DBPs deoxidization, degradation speed is slower.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, the materials and methods of nitrate and chlorine disinfection by-product in a kind of deoxidization, degradation water is provided.Utilize the reproducibility of alfer in the present invention, reduce under near-neutral sulfite deinking to nitrate, process is by the water body of azotate pollution; Under condition of different pH, deoxidization, degradation is carried out to chlorine disinfection by-product, the water body that process is polluted by chlorine disinfection by-product.
One aspect of the present invention relates to the alfer powder body material of nitrate and chlorine disinfection by-product in a kind of deoxidization, degradation water, and it is prepared by following steps:
A. the heating and melting 1-2h at 1000 ~ 1800 DEG C by ingot iron and fine aluminium;
B. cool the ferroaluminium of melting and by its fragmentation, obtain alfer particle.
Described melting process can carry out in electric furnace, and whole preparation process can be carried out under air atmosphere.
In preferred embodiments, in described material, the mass ratio of total aluminium and total iron is (40% ~ 90%): (60% ~ 10%).
In preferred embodiments, described alfer has ferromagnetism.
In preferred embodiments, the density of described alfer is 1.9 ~ 4.7g/cm
3.
In preferred embodiments, can sieve after fragmentation.Such as, the particle diameter of described alfer powder body material can be 0.3 ~ 3.0mm.
Second aspect present invention relates to a kind of method of nitrate or chlorine disinfection by-product in deoxidization, degradation water, it comprises and being contacted by the alfer powder body material of the water containing nitrate or chlorine disinfection by-product with nitrate in above-mentioned deoxidization, degradation water or chlorine disinfection by-product, comes nitrate described in deoxidization, degradation or DBPs.
In preferred embodiments, described chlorine disinfection by-product comprises chloroform, carbon tetrachloride or trichloroacetic acid.
Wherein when described method is used for the nitrate in deoxidization, degradation water, by the water containing nitrate in a looping fashion, such as flow through by peristaltic pump the reaction column that described alfer powder body material is housed: wherein the initial concentration of nitrate in nitrogen within the scope of 10 ~ 100mg/L; Be react under the near-neutral sulfite deinking of 6.5 ~ 8.0 at pH; The dosage of alfer is 100 ~ 400g/L.Flow velocity can be 2.5 ~ 3.5ml/s.
Wherein when described method is used for the trichloroacetic acid DBPs in deoxidization, degradation water, by the water containing DBPs trichloroacetic acid in a looping fashion, such as flow through by peristaltic pump the reaction column that described alfer powder body material is housed: wherein the initial concentration of trichloroacetic acid is within the scope of 1 ~ 20mg/L; The initial pH of solution is not regulated to react; The dosage of alfer is 100 ~ 400g/L.Flow velocity can be 2.5 ~ 3.5ml/s
Wherein when described method is used for the Small molecular DBPs in deoxidization, degradation water, water containing Small molecular DBPs is flowed through in the disposable mode crossing post the reaction column that described alfer powder body material is housed: wherein the initial concentration of carbon tetrachloride is less than 20 μ g/L, and the initial concentration of chloroform is less than 200 μ g/L; The initial pH of solution is not regulated to react; The dosage of alfer is 100 ~ 400g/L.Wherein, described Small molecular DBPs comprises carbon tetrachloride or chloroform.Flow velocity can be 1 ~ 1.5ml/s
In the present invention, the water body containing nitrate or DBPs with certain flow velocity by Filter column or filtering ponds that alfer powder body material is housed time, in water, nitrate and DBPs are removed by alloy powder material deoxidization, degradation.In deoxidization, degradation process, be nitrogen, nitrite and ammonia nitrogen by nitrate transformation, the chlorine that DBPs contains as chloroform, carbon tetrachloride and trichloroacetic acid etc. is removed successively.When the logical in a looping fashion Filter column of water body or filter tank flow velocity are 2.5 ~ 3.5ml/s, can remove the nitrate of more than 99% in 1h, nitrogen removal rate reaches more than 45%, and trichloroacetic acid clearance can reach 70%; When the disposable logical Filter column of water body, during <2min time of contact, carbon tetrachloride clearance can reach more than 50%, and chloroform clearance can reach 23%.
Wherein, nitrogen removal rate computing formula is as follows:
Nitrogen total amount after nitrogen removal rate=1-reaction in solution in the front nitrate of the total amount/reaction of various nitrogen forms.
From this formula, nitrogen removal rate is higher, and the nitrate being converted into nitrogen is more.
By the shortcoming that materials A l existing in prior art, Fe and Al-Fe bimetallic nano exist, and compared with prior art beneficial effect of the present invention is listed in table 1:
Table 1
The present invention utilizes the corrosion resistance of alfer material high, considerably reduce the corrosion rate using traditional fe powder as reduction filtering material, the aluminium ion produced because of the micro-stripping of aluminium in alloy material and iron in water body and iron ion meet the national standard of correlation water.And alfer powder body material of the present invention, no matter be reduction nitrate or reduction chlorine disinfection by-product, can both play a role under near-neutral sulfite deinking, therefore without the need to carrying out preconditioning pH step to pending waste water.In addition, alfer material of the present invention can reduce and remove nearly all nitrate, and in reduzate, ammonia nitrogen ratio reduces greatly.Therefore, the present invention is a kind of economical and efficient, simple to operate, has the method for nitrate or chlorine disinfection by-product in the removal water of good economy and environment benefit.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, but should not be construed as limitation of the present invention.
Embodiment 1
Cast iron and aluminium ingot are compared for 40%:60% adds in smelting furnace according to total aluminium and total weight of iron, heating and melting at 1500 DEG C.Come out of the stove after cooling, sieve after the alloy breaks down obtained, obtain the Al-Fe alloy powder material of particle diameter 10-20 order (0.3mm-3mm).Deionized water is used to soak with activated metal material surface Al-Fe alloy material.After filtration, Al-Fe alloy powder material is inserted in the lucite post of internal diameter 40mm as filtrate.
Under room temperature, measuring 200ml nitrate concentration is that the aqueous solution of 100mg/L is placed in conical flask, and pH is adjusted to 7.8 ± 0.1.Peristaltic pump is used to be circulated through the pillar that Al-Fe alloy material filtrate is housed with the flow velocity of 3.0ml/s.Initial reaction stage interval 5min extracts water sample, and after 30min, interval 10min extracts water sample.Each water sample, by after 0.22 μm of filter membrane, is analyzed nitrate, nitrite, ammonia nitrogen, aluminium ion and iron concentration in water.Result shows, reaction only carries out 4min, and in water, the clearance of nitrate reaches 31%, and nitrogen removal rate reaches 31%; After 1h, in water, the clearance of nitrate reaches 100%, and nitrogen removal rate reaches 45%, and in water body, metal ion aluminium ion, iron concentration detect through ICP-MS, concentration <0.1mg/L.
Embodiment 2
Cast iron and aluminium ingot are compared for 80%:20% adds in smelting furnace according to total aluminium and total weight of iron, heating and melting at 1300 DEG C.Come out of the stove after cooling, sieve after the alloy breaks down obtained, obtain the Al-Fe alloy powder material of particle diameter 10-20 order (0.3mm-3mm).Deionized water is used to soak with activated metal material surface Al-Fe alloy material.After filtration, Al-Fe alloy powder material is inserted in the tool core glass column of internal diameter 35mm as filtrate.
Under room temperature, measure the solution that 100ml Carbon Tetrachloride Concentration is 10 μ g/L, flow through the filtrate of thickness 7cm in the disposable mode crossing post.After solution passes through completely, measure 5ml water sample and add in 25ml cillin bottle, after sealing of jumping a queue, in 45 DEG C of water-baths, keep 1h, extract upper gas 20 μ L and carry out gas chromatographic detection.Result shows, after solution crosses post completely, carbon tetrachloride clearance is 38.5%; Metal ion in solution aluminium ion, iron concentration detects through ICP-MS, concentration <0.1mg/L.
Embodiment 3
Cast iron and aluminium ingot are compared for 90%:10% adds in smelting furnace according to total aluminium and total weight of iron, heating and melting at 1000 DEG C.Come out of the stove after cooling, sieve after the alloy breaks down obtained, obtain the Al-Fe alloy powder material of particle diameter 10-20 order (0.3mm-3mm).Deionized water is used to soak with activated metal material surface Al-Fe alloy material.After filtration, Al-Fe alloy powder material is inserted in the tool core glass column of internal diameter 35mm as filtrate.
Under room temperature, measure the solution that 100ml chloroform concentration is 100 μ g/L, flow through the filtrate of thickness 7cm in the disposable mode crossing post.After solution passes through completely, measure 5ml water sample and add in 25ml cillin bottle, after sealing of jumping a queue, in 45 DEG C of water-baths, keep 1h, extract upper gas 20 μ L and carry out gas chromatographic detection.Result shows, after solution crosses post completely, chloroform clearance is 23%; Metal ion in solution aluminium ion, iron concentration detects through ICP-MS, concentration <0.1mg/L.
Embodiment 4
Cast iron and aluminium ingot are compared for 90%:10% adds in smelting furnace according to total aluminium and total weight of iron, heating and melting at 1000 DEG C.Come out of the stove after cooling, sieve after the alloy breaks down obtained, obtain the Al-Fe alloy powder material of particle diameter 10-20 order (0.3mm-3mm).Deionized water is used to soak with activated metal material surface Al-Fe alloy material.After filtration, Al-Fe alloy powder material is inserted in the lucite post of internal diameter 40mm as filtrate.
Under room temperature, measuring 250ml concentration is that the solution of trichloroacetic acid of 20mg/L is placed in conical flask, does not regulate solution initial pH value.Peristaltic pump is used to be circulated through the pillar that Al-Fe alloy powder material is housed with the flow velocity of 3.5ml/s.Initial reaction stage interval 5min extracts water sample, and after 30min, interval 10min extracts water sample.Water sample, by after 0.22 μm of filter membrane, is analyzed trichloroacetic acid, aluminium ion and iron concentration in water.Result shows, after 1h, in water, the clearance of trichloroacetic acid reaches 70%, and in water body, metal ion aluminium ion, iron concentration detect through ICP-MS, concentration <0.1mg/L.
From embodiment, alfer powder body material of the present invention for nitrate in water and chlorine disinfection by-product removal effect good, and in use in alfer metal dissolving little, corrosion resistance is strong, therefore, the present invention is a kind of economical and efficient, simple to operate, has the method for nitrate or chlorine disinfection by-product in the removal water of good economy and environment benefit.
Claims (10)
1., for an alfer powder body material for nitrate or chlorine disinfection by-product in deoxidization, degradation water, it is prepared by following steps:
A. the heating and melting 1-2h at 1000 ~ 1800 DEG C by ingot iron and fine aluminium;
B. cool the ferroaluminium of melting and by its fragmentation, screening, obtain alfer powder body material.
2. material according to claim 1, wherein the mass ratio of total aluminium and total iron is (40% ~ 90%): (60% ~ 10%).
3. material according to claim 1, it has ferromagnetism.
4. material according to claim 1, the density of wherein said alfer powder body material is 1.9 ~ 4.7g/cm
3.
5. material according to claim 1, the particle diameter of wherein said alfer powder body material is 0.3 ~ 3.0mm.
6. the method for nitrate or chlorine disinfection by-product in deoxidization, degradation water, it comprises and being contacted with the alfer powder body material described in claim 1 by the water containing nitrate or chlorine disinfection by-product.
7. method according to claim 6, wherein said chlorine disinfection by-product comprises chloroform, carbon tetrachloride or trichloroacetic acid.
8. method according to claim 6, when being wherein used for the nitrate in deoxidization, degradation water when described method, the water containing nitrate is flowed through in a looping fashion the reaction column that described alfer powder body material is housed: wherein the initial concentration of nitrate in nitrogen within the scope of 10 ~ 100mg/L; Be react under the near-neutral sulfite deinking of 6.5 ~ 8.0 at pH; The dosage of alfer is 100 ~ 400g/L.
9. method according to claim 6, wherein when described method is used for the trichloroacetic acid DBPs in deoxidization, degradation water, the water containing DBPs trichloroacetic acid is flowed through in a looping fashion the reaction column that described alfer powder body material is housed: wherein the initial concentration of trichloroacetic acid is within the scope of 1 ~ 20mg/L; The initial pH of solution is not regulated to react; The dosage of alfer is 100 ~ 400g/L.
10. method according to claim 6, wherein when described method be used in deoxidization, degradation water comprise the Small molecular DBPs of carbon tetrachloride or chloroform time, water containing Small molecular DBPs is flowed through in the disposable mode crossing post the reaction column that described alfer powder body material is housed: wherein the initial concentration of carbon tetrachloride is less than 20 μ g/L, and the initial concentration of chloroform is less than 200 μ g/L; The initial pH of solution is not regulated to react; The dosage of alfer is 100 ~ 400g/L.
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| CN201410482530.4A CN104289708B (en) | 2014-09-19 | Nitrate or the method for chlorine disinfection by-product in a kind of deoxidization, degradation water |
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| CN201410482530.4A CN104289708B (en) | 2014-09-19 | Nitrate or the method for chlorine disinfection by-product in a kind of deoxidization, degradation water |
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| CN104289708B CN104289708B (en) | 2017-01-04 |
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| CN106365261A (en) * | 2016-11-18 | 2017-02-01 | 北京化工大学 | Electrode for synchronously removing nitrate and tetrachloromethane from water and preparation method and use method thereof |
| CN106365291A (en) * | 2016-11-18 | 2017-02-01 | 北京化工大学 | Material for removing nitrate from water as well as preparation and using methods of material |
| CN108355659A (en) * | 2018-03-14 | 2018-08-03 | 兰州交通大学 | A kind of metal carrier material and preparation method thereof based on the catalysis of iron aluminium |
| WO2021208289A1 (en) * | 2020-04-15 | 2021-10-21 | 北京化工大学 | Composite material and method for removing pollutant from polluted water |
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| CN108355659A (en) * | 2018-03-14 | 2018-08-03 | 兰州交通大学 | A kind of metal carrier material and preparation method thereof based on the catalysis of iron aluminium |
| WO2021208289A1 (en) * | 2020-04-15 | 2021-10-21 | 北京化工大学 | Composite material and method for removing pollutant from polluted water |
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