CN105540954B - A kind of method that chemical denitrification removes nitrate nitrogen in water removal - Google Patents
A kind of method that chemical denitrification removes nitrate nitrogen in water removal Download PDFInfo
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- CN105540954B CN105540954B CN201610010039.0A CN201610010039A CN105540954B CN 105540954 B CN105540954 B CN 105540954B CN 201610010039 A CN201610010039 A CN 201610010039A CN 105540954 B CN105540954 B CN 105540954B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46176—Galvanic cells
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4676—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction
- C02F1/4678—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction of metals
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/163—Nitrates
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a kind of method that chemical denitrification removes nitrate nitrogen in water removal, zinc-silver bimetallic fragment and disodium ethylene diamine tetraacetate are added in waste water, the pH value for adjusting waste water stirs generation nitrosation reduction reaction under conditions of air is completely cut off, and filtrate is collected by filtration；Urea is added after adjusting the pH value of filtrate, the denitration under conditions of air is completely cut off.The galvanic couple galvanic cell and urea coupling denitrification method that the present invention uses improve selectivity of the reduction final product for nitrogen；Low in raw material price that the present invention uses, being compatible with the environment property be good, denitrifying final product based on non-harmful nitrogen, therefore, the present invention has the advantages of green, environmentally friendly；Present invention process is simple and convenient to operate, reaction condition is gentle, cost is low, is mass produced suitable for industrialization.
Description
Technical field
The invention belongs to Environmental Chemistry technical field, and in particular to a kind of chemical denitrification goes to the side of nitrate nitrogen in water removal
Method.
Background technology
Excess nitrate intake body can cause the generation of a variety of diseases such as to cause high ferro hemalbumin disease and induce cancer.
To protect health, the World Health Organization provides the nitrate nitrogen ＜ 10mg/L in drinking water, and the standard in China is still
20mg/L .It is the important way for ensureing drinking water quality safety that the waste water high to nitrate content and underground water, which are effectively treated,
Footpath, it is this《China's urban wastewater treatment firm pollutant emission standard》GB18918-2002、《Household refuse landfill sites contamination control
Standard》The emission limit of total nitrogen is provided in the standards such as GB16889-2008.There is more the minimizing technology of nitrate in water
Kind, wherein practical application has been put into biological denitrification, ion exchange and reverse osmosis process.Although ion exchange and counter-infiltration work
The physical chemistry methods such as skill can separate nitrate from waste water or underground water, but the nitrate isolated also faces solution
The problem of final outlet.Manual type is taken to promote nitrogen to be released into air in the form of nitrogen to recover nature Nitrogen Cycling
Balance is the fundamental solution for solving azotate pollution.
Biological denitrification and chemical denitrification are two kinds of main methods that nitrate nitrogen in water is reduced to nitrogen.It is although raw
Thing denitrification method obtains practical application in the waste water of easily biological-degradable, but still suffer from complex process, operational management requirement it is high,
The shortcomings of denitrification speed is slow, required reactor volume is huge, it is especially poor to the high water treatment effect containing bio-toxicity.
Compared with biological denitrification, chemical denitrification method has that denitration speed is fast, and technique is simple, and the requirement to operational management is low, fits
For waste water quality scope it is wide the advantages that.Chemical denitrification method is by using reducing agent (energy) or reduction mode, by nitric acid
Salt is reduced to the nitrogen-containing compound of lower valency, so as to reach the purpose for removing nitrate nitrogen in waste water.In chemical denitrification process
In, the selection of the selection of reducing agent on the clearance and reduzate of nitrate nitrogen influence it is very big, therefore, people have developed use
Several reducing agents such as hydrogen, active metal and formic acid, methanol.Wherein, the work using metal simple-substances such as iron, aluminium, zinc as reducing agent
Metal deoxidization is sprinkled to be paid close attention to by some researchers due to the reason such as reducing agent is cheap, reaction speed is fast.But individually
The denitrifying primary product of metal simple-substance be ammonia nitrogen, and need more strictly control pH values.Although people construct
Bimetallic system solves the problems, such as that the control of pH values is difficult to a certain extent, makes denitrification can be with wider pH value range
There is higher activity, but also only be difficult to make the product of reaction by the single reduction process of bimetallic system with harmless nitrogen
Based on.How to efficiently control the reduction process of nitrate nitrogen, both played the advantage of bimetallic system, and can make reaction product with
It is current active metal denitrification method urgent problem based on nitrogen.
The content of the invention
The shortcomings that it is an object of the invention to overcome prior art, there is provided a kind of chemical denitrification removes nitrate nitrogen in water removal
Method.
The purpose of the present invention is achieved through the following technical solutions：A kind of chemical denitrification goes to the side of nitrate nitrogen in water removal
Method, it comprises the following steps：
S1. nitrosation reduces：Zinc-silver bimetallic fragment and disodium ethylene diamine tetraacetate are added in waste water（EDTA-2Na）,
The pH value of waste water is adjusted, stirring generation nitrosation reduction reaction, filtering, collects filtrate under conditions of air is completely cut off；
S2. denitration：The pH value of filtrate is adjusted, urea is added, stirs denitration under conditions of air is completely cut off, as remove
The water of nitrate nitrogen.
Further, zinc-silver bimetallic fragment described in step S1 be with silver ion on zinc metal sheet by replacing reactive deposition
Form, in the zinc-silver bimetallic fragment silver-colored content be 0.005~0.01%, a length of 2~4mm of fragment, a width of 0.5~
2mm, thickness 0.1mm.
Further, the mass ratio of nitrate nitrogen is in the dosage and waste water of zinc-silver bimetallic fragment described in step S1
600：1~1000：1.
Further, the mass ratio of nitrate nitrogen is 10 in EDTA-2Na addition described in step S1 and waste water:1~
40:1。
Further, in step S1 using the pH value of formic acid regulation waste water to 2~5.
Further, the reaction temperature of nitrosation reduction is 15~40 DEG C, and the reaction time is 1~4h, mixing speed
For 100~200r/min.
Further, the mass ratio of nitrate nitrogen is 1 in the addition of urea described in step S2 and waste water:1~10:1.
Further, the temperature of denitration reaction is 50~80 DEG C, and the time be 10~60min, mixing speed for 100~
200r/min。
Further, in step S2 using the pH value of hydrochloric acid regulation filtrate to 1~3.
The present invention principle be：Zinc and the silver metal that to be two kinds of electrode potentials different, they are in the solution containing nitrate nitrogen
Galvanic couple galvanic cell can be formed during middle contact, under neutral and solutions of weak acidity, the higher zinc of electrode potential discharges electronics, from
And accelerate the reduction of nitrate nitrogen in solution, while provide reaction interface, nitric acid as the silver of negative electrode for the reduction of nitrate nitrogen
Salt nitrogen can directly obtain electronics on its surface and be reduced.In reduction process, EDTA-2Na effect is added：First, production can be made
With it corrosion of the complex reaction so as to accelerating anode zinc occurs for raw divalent zinc ion, accelerates the generation of electronics；Second, anode is rotten
After zinc ion caused by erosion and EDTA form complex compound, change Zn/Zn () electrode potential so that the former electricity of whole galvanic couple
The control of Electric potentials in pond makes the reduction of nitrate nitrogen control in the nitrite nitrogen stage in optimum range.By selecting silver to be used as catalysis
Reduce negative electrode and control reaction condition（Time, temperature, pH etc.）The reduction process of nitrate nitrogen can also be made to control in nitrous
The state nitrogen stage.When urea is added into the solution after nitrosation reaction, in certain reaction condition（Time, temperature, pH etc.）Under,
Urea can react with nitrite nitrogen, be reduced to nitrogen, reach the purpose for thoroughly removing pollution of nitrate nitrogen.In reduction process
Main reaction equation is as follows：
The anode reaction of galvanic couple galvanic cell：Zn→Zn2++2e-, Zn2++ EDTA-2Na→EDTA-Zn() +2Na+
The cathode reaction of galvanic couple galvanic cell：NO3 -+2e-→NO2 -
The reduction reaction of urea：CO(NH2)2+2NO2 -+2H+=CO2↑+2N2↑+3H2O
The present invention has advantages below：
（1）The present invention makees reducing agent using galvanic couple galvanic cell and urea, is reacted by two-stage reductive, makes nitrate in waste water
Nitrogen is first reduced to nitrite nitrogen, then is reduced into nitrogen, relative to single active metal and the single anti-nitre of galvanic couple galvanic cell
Change method, the galvanic couple galvanic cell and urea coupling denitrification method that the present invention uses improve selection of the reduction final product for nitrogen
Property；
（2）The present invention, as galvanic couple galvanic cell, passes through the difference in Electrode Potential of zinc-silver, and EDTA- using zinc-silver bimetallic
The 2Na control for adding, reacting the conditions such as pH and time, makes nitrate nitrogen first be reduced to nitrite nitrogen, avoids the production of ammonia nitrogen
It is raw, its drastic reduction is provided into guarantee for nitrogen for urea；
（3）Low in raw material price that the present invention uses, being compatible with the environment property be good, denitrifying final product is with non-harmful
Based on nitrogen, therefore, the present invention has the advantages of green, environmentally friendly；
（4）Present invention process is simple and convenient to operate, reaction condition is gentle, cost is low, extensive raw suitable for industrializing
Production.
Embodiment
With reference to embodiment, the present invention will be further described, and protection scope of the present invention is not limited to following institute
State.
Embodiment 1：A kind of method that chemical denitrification removes nitrate nitrogen in water removal, it comprises the following steps：
S1. nitrosation reduces：Zinc-silver bimetallic fragment and EDTA-2Na are added in waste water, formic acid adjusts the pH value of waste water
To 2, completely cut off stirring generation nitrosation reduction reaction 1h under conditions of air, reaction temperature is 15 DEG C, mixing speed 100r/
Min, filtering, collect filtrate；The mass ratio of nitrate nitrogen is 600 in the dosage and waste water of the zinc-silver bimetallic fragment:1；
The mass ratio of nitrate nitrogen is 10 in EDTA-2Na addition and waste water:1；Zinc-silver bimetallic fragment is in zinc metal sheet with silver ion
On formed by replacing reactive deposition, silver-colored content is 0.005%, a length of 2mm of fragment in the zinc-silver bimetallic fragment, wide
For 0.5mm, thickness 0.1mm；
S2. denitration：The pH value of hydrochloric acid regulation filtrate adds urea to 1, nitrate nitrogen in the addition and waste water of urea
Mass ratio be 1：1,10min is stirred under conditions of air is completely cut off, the temperature of reaction is 50 DEG C, mixing speed 100r/
Min, as remove the water of nitrate nitrogen.
Embodiment 2：A kind of method that chemical denitrification removes nitrate nitrogen in water removal, it comprises the following steps：
S1. nitrosation reduces：Zinc-silver bimetallic fragment and EDTA-2Na are added in waste water, formic acid adjusts the pH value of waste water
To 5, completely cut off stirring generation nitrosation reduction reaction 4h under conditions of air, reaction temperature is 40 DEG C, mixing speed 200r/
Min, filtering, collect filtrate；The mass ratio of nitrate nitrogen is 1000 in the dosage and waste water of the zinc-silver bimetallic fragment:1；
The mass ratio of nitrate nitrogen is 40 in EDTA-2Na addition and waste water:1；Zinc-silver bimetallic fragment is in zinc metal sheet with silver ion
On formed by replacing reactive deposition, silver-colored content is 0.01%, a length of 4mm of fragment in the zinc-silver bimetallic fragment, a width of
2mm, thickness 0.1mm；
S2. denitration：The pH value of hydrochloric acid regulation filtrate adds urea to 3, nitrate nitrogen in the addition and waste water of urea
Mass ratio be 10:1,60min is stirred under conditions of air is completely cut off, the temperature of reaction is 80 DEG C, mixing speed 200r/
Min, as remove the water of nitrate nitrogen.
Embodiment 3：A kind of method that chemical denitrification removes nitrate nitrogen in water removal, it comprises the following steps：
S1. nitrosation reduces：Zinc-silver bimetallic fragment and EDTA-2Na are added in waste water, formic acid adjusts the pH value of waste water
To 3, completely cut off stirring generation nitrosation reduction reaction 2h under conditions of air, reaction temperature is 22 DEG C, mixing speed 135r/
Min, filtering, collect filtrate；The mass ratio of nitrate nitrogen is 720 in the dosage and waste water of the zinc-silver bimetallic fragment:1；
The mass ratio of nitrate nitrogen is 23 in EDTA-2Na addition and waste water:1；Zinc-silver bimetallic fragment is in zinc metal sheet with silver ion
On formed by replacing reactive deposition, silver-colored content is 0.007%, a length of 3mm of fragment in the zinc-silver bimetallic fragment, wide
For 1mm, thickness 0.1mm；
S2. denitration：The pH value of hydrochloric acid regulation filtrate adds urea to 1.5, nitrate in the addition and waste water of urea
The mass ratio of nitrogen is 4:1,35min is stirred under conditions of air is completely cut off, the temperature of reaction is 62 DEG C, mixing speed 130r/
Min, as remove the water of nitrate nitrogen.
Embodiment 4：A kind of method that chemical denitrification removes nitrate nitrogen in water removal, it comprises the following steps：
S1. nitrosation reduces：Zinc-silver bimetallic fragment and EDTA-2Na are added in waste water, formic acid adjusts the pH value of waste water
To 4, completely cut off stirring generation nitrosation reduction reaction 3h under conditions of air, reaction temperature is 32 DEG C, mixing speed 180r/
Min, filtering, collect filtrate；The mass ratio of nitrate nitrogen is 850 in the dosage and waste water of the zinc-silver bimetallic fragment:1；
The mass ratio of nitrate nitrogen is 18 in EDTA-2Na addition and waste water:1；Zinc-silver bimetallic fragment is in zinc metal sheet with silver ion
On formed by replacing reactive deposition, silver-colored content is 0.009%, a length of 4mm of fragment in the zinc-silver bimetallic fragment, wide
For 1.5mm, thickness 0.1mm.
S2. denitration：The pH value of hydrochloric acid regulation filtrate adds urea to 2.5, nitrate in the addition and waste water of urea
The mass ratio of nitrogen is 8:1,50min is stirred under conditions of air is completely cut off, the temperature of reaction is 72 DEG C, mixing speed 170r/
Min, as remove the water of nitrate nitrogen.
Experimental example 1：
Certain percolate film-filter concentration liquid, nitrate nitrogen, nitrite nitrogen, ammonia-nitrogen content are respectively 40mg/ in raw water
L, 200mg/L, 182mg/L, raw sewage pre-process nitrate nitrogen, nitrite nitrogen, ammonia in water outlet after wet oxidation pre-processes
Nitrogen content is respectively 60mg/L, 0.17mg/L, 1.6mg/L, and this pretreatment water outlet 1L is collected in the container 1 of 2L acid and alkali-resistances,
The zinc-silver bimetallic chip that silver content is 0.006% is added into container 1（A length of 2mm of chip, a width of 1mm, thickness are
0.1mm）43.3 g, the ml of EDTA-2Na solution 8 that mass fraction is 11% is added, with the pH to 3 of first acid-conditioning solution, 20
Nitrosation reduction reaction 180min is carried out at DEG C, nitrosation reduction reaction water outlet is collected to volume as 2L and the container of acid and alkali-resistance
In 2,0.176g urea is added into container 2, with the pH to 3 of hydrochloric acid conditioning solution, depth denitration reaction is carried out at 75 DEG C
40min, content difference 0mg/L, 0mg/L, 2.8 mg/L, the nitre of nitrate nitrogen, nitrite nitrogen, ammonia nitrogen in measure processing water outlet
The clearance of hydrochlorate nitrogen reaches 100%, and the selection rate of non-ammonia nitrogen reaches more than 95% in chemical denitrification final product.
Experimental example 2：
Certain underground water, nitrate nitrogen content are 18.7mg/L, pH 6.5, and this waste water 5L is collected to 10L acid and alkali-resistance
In container 1, the zinc-silver bimetallic chip that silver content is 0.009% is added into container 1（A length of 3mm of chip, a width of 0.5mm,
Thickness is 0.1mm）75g, the EDTA-2Na solution 20ml that mass fraction is 11% are added, with the pH to 4.5 of first acid-conditioning solution,
Nitrosation reduction reaction 60min is carried out at 35 DEG C, nitrosation reduction reaction water outlet is collected to volume as 10L and acid and alkali-resistance
In container 2,0.4g urea is added into container 2, adjusts the pH to 2 of solution, depth denitration reaction 30min is carried out at 65 DEG C,
Content difference 0mg/L, the 0.3mg/L of nitrate nitrogen, nitrite nitrogen, ammonia nitrogen, 1.88mg/L, nitrate in measure processing water outlet
The clearance of nitrogen reaches 100%, and the selection rate of non-ammonia nitrogen reaches more than 90% in chemical denitrification final product.
Claims (4)
1. a kind of method that chemical denitrification removes nitrate nitrogen in water removal, it is characterised in that it comprises the following steps：
S1. nitrosation reduces：Zinc-silver bimetallic fragment and disodium ethylene diamine tetraacetate are added in waste water, adjusts the pH value of waste water,
Nitrosation reduction reaction occurs for stirring under conditions of air is completely cut off, and filtering, collects filtrate；
S2. denitration：Using the pH value of hydrochloric acid regulation filtrate to 1~3, urea is added, is stirred under conditions of air is completely cut off de-
Nitre, as remove the water of nitrate nitrogen；The temperature of denitration reaction is 50~80 DEG C, and the time is 10~60min, and mixing speed is
100~200r/min；
Wherein, zinc-silver bimetallic fragment described in step S1 is to be formed with silver ion on zinc metal sheet by replacing reactive deposition, institute
It is 0.005~0.01% to state content silver-colored in zinc-silver bimetallic fragment, a length of 2~4mm of fragment, a width of 0.5~2mm, and thickness is
0.1mm；
Using the pH value of formic acid regulation waste water to 2~5 in step S1；The reaction temperature of the nitrosation reduction is 15~40 DEG C,
Reaction time is 1~4h, and mixing speed is 100~200r/min.
2. the method that a kind of chemical denitrification as claimed in claim 1 removes nitrate nitrogen in water removal, it is characterised in that step S1
Described in zinc-silver bimetallic fragment dosage and waste water in nitrate nitrogen mass ratio be 600:1~1000:1.
3. the method that a kind of chemical denitrification as claimed in claim 1 removes nitrate nitrogen in water removal, it is characterised in that step S1
Described in the addition of disodium ethylene diamine tetraacetate and the mass ratio of nitrate nitrogen in waste water be 10:1~20:1.
4. the method that a kind of chemical denitrification as claimed in claim 1 removes nitrate nitrogen in water removal, it is characterised in that step S2
Described in the addition of urea and the mass ratio of nitrate nitrogen in waste water be 1:1~10:1.
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| CN111484117B (en) * | 2020-04-17 | 2022-06-28 | 无锡中天固废处置有限公司 | Method and device for reducing nitrate radical in acid solution |
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| CN103964550A (en) * | 2014-05-24 | 2014-08-06 | 长安大学 | Method for removing nitrate nitrogen in water body |
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Effective date of registration: 20181205 Address after: 610041, 24th Floor, New Hope International C Block, No. 8, Jitai No. 3 Road, Chengdu High-tech Zone, Sichuan Province (1-8) Patentee after: Deepblue Environmental Protection Technologies Co., Ltd. Address before: 610068 No. 5 Jing'an Road, Jinjiang District, Chengdu City, Sichuan Province Patentee before: Sichuan Normal University |