CN104230061A - Catalytic oxidation treatment method of ammonia nitrogen wastewater - Google Patents
Catalytic oxidation treatment method of ammonia nitrogen wastewater Download PDFInfo
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- CN104230061A CN104230061A CN201410455338.6A CN201410455338A CN104230061A CN 104230061 A CN104230061 A CN 104230061A CN 201410455338 A CN201410455338 A CN 201410455338A CN 104230061 A CN104230061 A CN 104230061A
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Abstract
The invention provides a catalytic oxidation treatment method of ammonia nitrogen wastewater. The catalytic oxidation treatment method comprises the following steps: catalytic oxidation: adding a catalytic oxidizing agent into the ammonia nitrogen wastewater and performing a catalytic oxidation reaction under the condition that the pH value is 5-10 to obtain outlet water and denitrified outlet water; and electrolysis: supplementing a chlorine salt into the denitrified outlet water, then performing electrolysis to obtain the catalytic oxidizing agent, and refluxing the catalytic oxidizing agent into the catalytic oxidation step to be used as the catalytic oxidizing agent, wherein the amount of the denitrified outlet water and the water inlet of the ammonia nitrogen wastewater are calculated according to WC1*Qe=(7.6-8.0) WN*Qi, wherein Qe is the flow rate of the denitrified outlet water, Qi is the flow rate of the ammonia nitrogen wastewater, WC1 is the mass concentration of chlorine in an electrolyte in the electrolysis step, and WN is the mass concentration of ammonia nitrogen in the ammonia nitrogen wastewater. By adopting the method provided by the invention, the secondary pollution of an environment can be avoided.
Description
Technical field
The present invention relates to ammonia nitrogen waste water process field, especially, relate to a kind of ammonia nitrogen waste water treatment by catalytic oxidation.
Background technology
Ammonia nitrogen waste water wide material sources are one of main water pollutants, and in water body, ammonia nitrogen exceeds standard and can cause algae and other microorganism amount reproduction, causes body eutrophication, accelerates the consumption of Dissolved Oxygen in Water, cause aquatic organism dead.
Existing catalytic oxidation treatment ammonia nitrogen waste water method focuses mostly on the research of in the catalytic oxidation process such as conventional parameter such as current density, spread of electrodes, to obtain processing parameter ammonia nitrogen waste water to better treatment effect.But the adjustment of these parameters is difficult to the real-time monitoring realizing reacting to waste water in treating processes.Thus often can produce the hazardous and noxious substances such as nitrite, nitrogen trichloride in reaction process, cause reaction uncontrollable.Disclosed in CN102701334A, utilize the ammonia nitrogen in catalytic oxidation process gold smelting waste water, after process, water outlet ammonia nitrogen concentration is stable lower than 10mg/L.Although this technique achieves efficient, the stable of ammonia nitrogen in waste water and removes, in electrolytic process, easily produce nitrite, secondary pollution is caused to environment.
Summary of the invention
The object of the invention is to provide a kind of ammonia nitrogen waste water treatment by catalytic oxidation, to solve the technical problem producing the secondary pollutions such as nitrite in prior art in catalytic oxidation process ammonia nitrogen waste water reaction process.
For achieving the above object, the invention provides a kind of ammonia nitrogen waste water treatment by catalytic oxidation, comprise the following steps: catalyzed oxidation: in ammonia nitrogen waste water, add catalytic oxidant, under pH value 5 ~ 10 condition, carry out catalytic oxidation, obtain water outlet and denitrogenation water outlet; Electrolysis: carry out electrolysis after denitrogenation water outlet supplements villaumite, obtain catalytic oxidant, catalytic oxidant passes back in catalytic oxidation stage, uses as catalytic oxidant; Wherein W pressed by the water yield of denitrogenation water outlet and the flooding quantity of ammonia nitrogen waste water
c1× Q
e=(7.6 ~ 8.0) W
n× Q
icalculate, wherein Q
efor the flow of denitrogenation water outlet, Q
ifor the flow of ammonia nitrogen waste water, W
c1for the mass concentration of the chlorine of electrolytic solution in electrolysis step, W
nfor the mass concentration of ammonia nitrogen in ammonia nitrogen waste water.
Further, the pH value in catalytic oxidation treatment step is 7 ~ 9.
Further, in catalytic oxidation process, redox potential is 400 ~ 1000mV.
Further, the redox potential in catalytic oxidation treatment step is 600 ~ 800mV.
Further, during electrolysis, the chlorine ion concentration of electrolytic solution is 5 ~ 40g/L; Preferred villaumite is sodium-chlor or Repone K.
Further, during electrolysis, the chlorine ion concentration of electrolytic solution is 20 ~ 30g/L.
Further, the reference electrode measuring redox potential is Hg and HgCl
2.
Further, in ammonia nitrogen waste water, ammonia nitrogen concentration is 20 ~ 400mg/L.
The present invention has following beneficial effect:
Method provided by the invention, by controlling the water yield of the pH value of the reaction solution in catalytic oxidation process, ammonia nitrogen waste water flooding quantity and denitrogenation water outlet simultaneously, realizes ammonia nitrogen in whole treating processes and all reacts in the mode of indirect oxidation.Reduce the generation of nitrite or nitrogen trichloride, avoid the secondary pollution to environment.By recycling the hypochlorite in denitrogenation water outlet, improving the utilization ratio of villaumite, saving electrolysis energy consumption and cost.
Except object described above, feature and advantage, the present invention also has other object, feature and advantage.Below with reference to figure, the present invention is further detailed explanation.
Accompanying drawing explanation
The accompanying drawing forming a application's part is used to provide a further understanding of the present invention, and schematic description and description of the present invention, for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 is the process flow diagram of the preferred embodiment of the present invention; And
Fig. 2 is the equipment flowsheet schematic diagram of the preferred embodiment of the present invention.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are described in detail, but the multitude of different ways that the present invention can be defined by the claims and cover is implemented.
Catalytic oxidation process ammonia nitrogen waste water comprises direct oxidation and indirect oxidation, and reaction formula is as follows:
Mainly there is following reaction equation in direct oxidation:
2NH
3+6OH
--6e
-＝N
2↑+6H
2O (1)
NH
3+7OH
--6e
-＝NO
2 -+5H
2O (2)
Mainly there is following reaction equation in indirect oxidation:
2Cl
-＝Cl
2+2e
- (3)
Cl
2+H
2O＝HClO+HCl (4)
2NH
3+3HClO＝N
2↑+3HCl+3H
2O (5)
2NH
4 ++2OH
-+3HClO＝N
2↑+3HCl+5H
2O (6)
NH
3+3HClO＝NCl
3↑+3H
2O (7)
NH
4 ++3HClO＝NCl
3↑+3H
++3H
2O (8)
Direct oxidation mainly relies on transfer transport in electrolytic process, and by the ammonia nitrogen removal in waste water, the product after ammonia nitrogen direct oxidation is nitrogen (N
2) or nitrite (NO
2-).Due to formula (1) and formula (2) reaction conditions close, be thus difficult to stability contorting by Controlling Technology condition, thus gained water outlet nitrite is too high.
Indirect oxidation mainly relies on the hypochlorite produced in electrolytic process, by ammonia or ammonium radical ion oxidation removal.Product after ammonia nitrogen indirect oxidation is nitrogen or nitrogen trichloride.Main generating polynomial (5), (6), (7), (8) in indirect oxidation process, when generating polynomial (7) and (8) can produce nitrogen trichloride often.Nitrogen trichloride can produce foul gas and be decomposed into ammonia and hypochlorous acid, causes secondary pollution to environment.Need in prior art simultaneously in control ph, electrolyzer the parameter such as electrode used therein distance, current density to the generation preventing formula (7), (8) react.And these parameters are real-time change in reaction process, in reaction process, be thus difficult to the generation avoiding formula (7) completely, (8) react.
See Fig. 1, catalytic oxidation process ammonia nitrogen waste water provided by the invention is 5 ~ 10 by controlling the pH value of ammonia nitrogen waste water, the water yield of denitrogenation water outlet and the flooding quantity of ammonia nitrogen waste water, makes formula (3) ~ (6) only occurred in catalytic oxidation process in indirect oxidation reaction process.And without the need to controlling other parameters in catalyzed oxidation groove.Other parameters are carried out according to a conventional method.Preferable ph is 7 ~ 9 can ensure the carrying out that catalytic oxidation is quick, stable.The present invention carries out electrolysis to denitrogenation water outlet, when avoiding Direct Electrolysis ammonia nitrogen waste water, because in waste water, ammonia nitrogen concentration is too high, causes the problem producing nitrite in electrolytic process.
In electrolytic process, electrolytic solution used is the solution that gained after villaumite is added in denitrogenation water outlet.This ammonia nitrogen in solution concentration is very low and containing a large amount of hypochlorite, thus can avoid generating polynomial (1) and formula (2).
Ammonia nitrogen waste water through catalytic oxidation treatment is made up of two portions.A part is water outlet, and this part water outlet can directly be discharged.Another part is denitrogenation water outlet, and this part denitrogenation water outlet enters in follow-up electrolysis step.After electrolysis, products therefrom uses as the catalytic oxidant in catalytic oxidation stage.The flooding quantity of ammonia nitrogen waste water and the water yield of denitrogenation water outlet can according to following formula: W
c1× Q
e=(7.6 ~ 8.0) W
n× Q
icalculate, wherein Q
efor the flow of denitrogenation water outlet, Q
ifor the flow of ammonia nitrogen waste water, W
c1for the mass concentration of the chlorine of electrolytic solution in electrolysis step, W
nfor the mass concentration of ammonia nitrogen in ammonia nitrogen waste water.The electrolysis amount of the denitrogenation water outlet obtained by this formulae discovery, the flooding quantity of ammonia nitrogen waste water and pH value act synergistically and avoid the generation of nitrogen trichloride.Waste water is after catalytic oxidation treatment, and denitrogenation water outlet enters in electrolyzer carries out electrolysis, and in denitrogenation water outlet, remaining hypochlorite can as oxygenant reuse.Calculate reuse denitrogenation water outlet by this formula and the rate of recovery of chlorine can be increased to 50%.Improve chlorine utilization in waste water.If carry out reuse not according to this, the reaction of only generating polynomial (3) ~ (6) cannot be ensured.Q simultaneously
ewith Q
ithan too low, chlorine utilization ratio can be caused too low; Q
ewith Q
ithan too high, ammonia nitrogen waste water processing power can be caused too low, electrical catalyze reduction efficiency reduces, and in gained discharge water, ammonia nitrogen concentration is high.
In preferred control catalytic oxidation process, redox potential is 400 ~ 1000mV.ORP current potential is lower than 400mV, then ammonia nitrogen removal efficiency is lower; ORP current potential is higher than 1000mv, then catalytic oxidant add-on is excessive causes waste.From formula (5) ~ (6), the indirect oxidation process of ammonia nitrogen is carried out mainly through redox reaction.Therefore selective redox current potential is as the main control parameters of oxidising process, can reflect the ratio of ammonia nitrogen waste water and catalytic oxidant add-on.Can only generating polynomial (3) ~ (6) in more effective guarantee treating processes by control ORP.The acquisition comparatively simple, intuitive of redox potential (ORP), only needing reference electrode is Hg and HgCl
2can directly to read in insertion reaction liquid, but when redox potential value exceedes this scope, also by simply adding catalytic oxidant or ammonia nitrogen waste water can realize regulation and control.When preferred redox potential is 600 ~ 800mV, in gained final outflow water, ammonia nitrogen concentration is lower, and the reaction simultaneously producing hazardous and noxious substances less occurs.
The energy consumption of electrolytic process is relevant with the villaumite concentration of solution in electrolyzer.Villaumite concentration is lower, and electrolysis energy consumption is larger, and villaumite is too high, causes the waste of medicament.Thus need supplementary villaumite when electrolysis nitrogen water outlet, after preferred addition, in electrolytic solution, the concentration of chlorion is 5 ~ 40g/L.Now lower simultaneously the avoiding of electrolysis energy consumption adds too much villaumite and increases cost.Preferred chlorine ion concentration is 20 ~ 30g/L.Now energy consumption reaches minimum.Villaumite can for conventional all kinds of villaumites, and preferably added villaumite is sodium-chlor or Repone K.The two does not introduce other impurity, and electrolysis effectiveness is more excellent.
In preferably treatment ammonia nitrogen waste water, ammonia nitrogen concentration is the waste water of 20 ~ 400mg/L, and now energy consumption is lower, and treatment effect is good.
Embodiment
In following examples and comparative example, raw materials used and equipment is commercially available.
In following examples and comparative example, electrolytic condition is: electrolyzer is commercially available, be made up of UPVC material, electrolyzer anodic-cathodic all with pure titanium for base material is made, power supply is ZB type direct supply, electrode bed course adopts PVDF material, electrode length 1110mm, electrode tube external diameter 250mm, polar plate spacing 3mm, current density 800A/m
2, electrolysis voltage 12V, electrolysis time is 60 minutes.
Embodiment 1:
Ammonia nitrogen waste water derives from tungsten smelting process, and wastewater flow is 1.0m
3/ h, ammonia nitrogen concentration is 400mg/L, and in waste water, chlorine ion concentration is 200mg/L.The shown technique that sees figures.1.and.2 processes waste water.
Ammonia nitrogen waste water enters pH regulator pond, regulates wastewater pH=8.0 with lime.With waste water pump, waste water is added to three grades of catalytic oxidation grooves, the stirring total reaction time controlling tertiary oxidation reactive tank controls to be 15 minutes.
Dissolve solid sodium chloride as electrolytic solution in dissolved salt groove, the solution obtained successively through strainer and brine tank, adds sodium chloride solution by volume pump by submersible pump in electrolyzer, keeps chlorine ion concentration in electrolyzer to be 10g/L.
W pressed by the water yield of denitrogenation water outlet and the flooding quantity of ammonia nitrogen waste water
c1× Q
e=(7.6 ~ 8.0) W
n× Q
icalculate, wherein W
c1=10g/L, W
n=400mg/L.Waste water after catalytic oxidation process, gained Q
e: Q
ithan being 0.32: 1.Be 0.68m with going out water pump by flow
3the water outlet of/h is directly discharged, residue 0.32m
3the denitrogenation water outlet of/h enters electrolyzer.Under the effect of electrolysis, the sodium chloride solution in electrolyzer is converted into catalytic oxidant, and adds in three grades of catalytic oxidation grooves by dosing pump, regulates dosing pump flow, keeps catalytic oxidation ORP=800mv, so circulates.
In continuous operational process, electrolysis energy consumption is 40kWh/kg (N), in electrolyzer, chlorine utilization ratio is 50%, water outlet ammonia nitrogen concentration is 7.0mg/L, water outlet does not detect nitrite, have no foul gas to produce, effluent quality reaches integrated wastewater discharge standard (GB8978-1996) requirement.
Embodiment 2
Ammonia nitrogen waste water derives from vanadium smelting process, and wastewater flow is 1.0m
3/ h, ammonia nitrogen concentration is 350mg/L, and in waste water, chlorine ion concentration is 12g/L, and the shown technique that sees figures.1.and.2 processes waste water.
Ammonia nitrogen waste water enters pH regulator pond, regulates wastewater pH=8.0 with lime.With waste water pump, waste water is added to three grades of catalytic oxidation grooves, the stirring total reaction time controlling tertiary oxidation reactive tank controls to be 15 minutes, catalytic oxidation ORP=850mv.
W pressed by the water yield of denitrogenation water outlet and the flooding quantity of ammonia nitrogen waste water
c1× Q
e=(7.6 ~ 8.0) W
n× Q
icalculate, wherein, W
c1=12g/L, W
n=350mg/L.Waste water after catalytic oxidation process, gained Q
e: Q
ithan being 0.23: 1.Be 0.77m with going out water pump by flow
3the water outlet of/h is directly discharged, residue 0.23m
3the denitrogenation water outlet of/h enters electrolyzer.
In operational process, electrolysis energy consumption is 40kWh/kg (N), in electrolyzer, chlorine utilization ratio is 45%, water outlet ammonia nitrogen concentration is 6.0mg/L, water outlet does not detect nitrite, have no foul gas to produce, effluent quality reaches integrated wastewater discharge standard (GB8978-1996) requirement.
Embodiment 3
Ammonia nitrogen waste water derives from tungsten smelting process, and wastewater flow is 1.0m
3/ hour, the ammonia nitrogen concentration of waste water is 400mg/L, refers again to technique shown in Fig. 1 and Fig. 2 and processes waste water.
Ammonia nitrogen waste water enters pH regulator pond, regulates wastewater pH=8.0 with lime.With waste water pump, waste water is added to three grades of catalytic oxidation grooves, the stirring total reaction time controlling tertiary oxidation reactive tank controls to be 15 minutes, ORP=600mv in catalytic oxidation.Add Repone K in denitrogenation water outlet after, chlorine ion concentration in electrolyzer is kept to be 20g/L.
W pressed by the water yield of denitrogenation water outlet and the flooding quantity of ammonia nitrogen waste water
c1× Q
e=(7.6 ~ 8.0) W
n× Q
icalculate, wherein, W
c1=20g/L, W
n=400mg/L.Waste water after catalytic oxidation process, gained Q
e: Q
ithan being 0.16: 1.Be 0.84m with going out water pump by flow
3the water outlet of/h is directly discharged, residue 0.16m
3the denitrogenation water outlet of/h enters electrolyzer.In operational process, electrolysis energy consumption is 40kWh/kg (N), in electrolyzer, chlorine utilization ratio is 50%, in the water body of discharging after treatment, ammonia nitrogen concentration is 7.0mg/L, water outlet does not detect nitrite, have no foul gas to produce, effluent quality reaches integrated wastewater discharge standard (GB8978-1996) requirement.
Embodiment 4
Be with the difference of embodiment 1: ORP=1000mv, pH value is 9, after adding sodium chloride solution during electrolysis, keeps chlorine ion concentration in electrolyzer to be 30g/L.
Embodiment 5
Be with the difference of embodiment 1: ORP=400mv, pH value is 7.
Comparative example 1
Be with the difference of embodiment 1, regulate wastewater pH=4.0 with lime.Then water outlet ammonia nitrogen concentration is 8.0mg/L, and in electrolytic process, foul smelling gas produces, and is NCl after testing
3.
Comparative example 2
Be with the difference of embodiment 1, catalytic oxidation ORP=200mv.Then water outlet ammonia nitrogen concentration is 30.0mg/L, higher than integrated wastewater discharge standard requirement.
Comparative example 3
Be with the difference of embodiment 1, in electrolyzer, chlorine ion concentration is 3g/L.Then water outlet ammonia nitrogen concentration is 10.0mg/L, and electrolysis energy consumption increases to 70kWh/kg (N).
Comparative example 4
Be with the difference of embodiment 1, the throughput ratio of the denitrogenation water outlet and ammonia nitrogen waste water that enter electrolyzer is 0.1: 1.Then water outlet ammonia nitrogen concentration is 8.0mg/L, but in electrolyzer, chlorine utilization ratio is reduced to 25%, and electrolysis energy consumption increases to 48kWh/kg (N).
Comparative example 5
Ammonia nitrogen waste water derives from tungsten smelting process, and wastewater flow is 1.0m
3/ h, ammonia nitrogen concentration is 400mg/L, and in waste water, chlorine ion concentration is 200mg/L.
Ammonia nitrogen waste water enters pH regulator pond, regulates wastewater pH=8.0 with lime, with waste water pump, waste water is all directly added to electrolyzer.Solid sodium chloride dissolved in dissolved salt groove, the solution obtained successively through strainer and brine tank, adds sodium chloride solution by volume pump by submersible pump in electrolyzer, keeps chlorine ion concentration in electrolyzer to be 10g/L.Under the acting in conjunction of electrolysis and catalytic oxidant, by the ammonia nitrogen removal in waste water.
In continuous operational process, electrolysis energy consumption is 46kWh/kg (N), and in electrolyzer, chlorine utilization ratio is only 15%, and water outlet ammonia nitrogen concentration is 6.5mg/L, and it is 2mg/L that water outlet detects nitrite concentration, causes secondary pollution to water outlet.
Contrasted from above embodiment 1 ~ 5 and comparative example 1 ~ 5, adopt catalytic oxidation process ammonia nitrogen waste water of the present invention, effectively can avoid the generation of nitrite or nitrogen trichloride, avoid the secondary pollution to environment, water outlet stably reaching standard is discharged.Simultaneously by denitrogenation water part is back to electrolyzer, can effectively improve villaumite utilization ratio, reduce electrolysis energy consumption.
From comparative example 1, if catalyzed oxidation pH is not controlled, in scope provided by the invention, cannot NCl be avoided
3the generation of foul gas.
From comparative example 2, if do not control in scope provided by the invention by catalyzed oxidation ORP, cannot ensure that water outlet ammonia nitrogen concentration is lower than 10mg/L.
From comparative example 3, if do not control in scope provided by the invention by the chlorine ion concentration in electrolyzer, the increase of electrolysis energy consumption will be caused.
From comparative example 4, if denitrogenation water outlet enters the throughput ratio of electrolyzer and ammonia nitrogen waste water lower than scope provided by the invention, villaumite utilization ratio will be caused to decline, electrolysis energy consumption increases.
From comparative example 5, if ammonia nitrogen waste water is all added electrolyzer, directly carry out electrolysis and catalytic oxidation, then cannot avoid the generation of nitrite, in electrolyzer, villaumite utilization ratio is lower.
Contrasted from above embodiment 1 ~ 5 and comparative example 1 ~ 5, adopt catalytic oxidation process ammonia nitrogen waste water of the present invention, effectively can avoid the generation of nitrite or nitrogen trichloride, avoid the secondary pollution to environment, water outlet stably reaching standard is discharged.Simultaneously by by denitrogenation effluent recycling to electrolyzer, can effectively improve villaumite utilization ratio, reduce electrolysis energy consumption.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. an ammonia nitrogen waste water treatment by catalytic oxidation, is characterized in that, comprises the following steps:
Catalyzed oxidation: add catalytic oxidant in described ammonia nitrogen waste water, carries out catalytic oxidation under pH value 5 ~ 10 condition, obtains water outlet and denitrogenation water outlet;
Electrolysis: carry out electrolysis after described denitrogenation water outlet supplements villaumite, obtain described catalytic oxidant, described catalytic oxidant passes back in described catalytic oxidation stage, uses as catalytic oxidant;
W pressed by the water yield of wherein said denitrogenation water outlet and the flooding quantity of described ammonia nitrogen waste water
c1× Q
e=(7.6 ~ 8.0) W
n× Q
icalculate, wherein Q
efor the flow of described denitrogenation water outlet, Q
ifor the flow of described ammonia nitrogen waste water, W
c1for the mass concentration of the chlorine of electrolytic solution in described electrolysis step, W
nfor the mass concentration of ammonia nitrogen in described ammonia nitrogen waste water.
2. method according to claim 1, is characterized in that, the pH value in described catalytic oxidation treatment step is 7 ~ 9.
3. method according to claim 1, is characterized in that, in described catalytic oxidation process, redox potential is 400 ~ 1000mV.
4. method according to claim 3, is characterized in that, the redox potential in described catalytic oxidation treatment step is 600 ~ 800mV.
5. the method according to any one of Claims 1 to 4, is characterized in that, during described electrolysis, the chlorine ion concentration of electrolytic solution is 5 ~ 40g/L; Preferred described villaumite is sodium-chlor or Repone K.
6. method according to claim 5, is characterized in that, during described electrolysis, the chlorine ion concentration of electrolytic solution is 20 ~ 30g/L.
7. method according to claim 5, is characterized in that, the reference electrode measuring described redox potential is Hg and HgCl
2.
8. method according to claim 5, is characterized in that, in described ammonia nitrogen waste water, ammonia nitrogen concentration is 20 ~ 400mg/L.
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| CN105130070A (en) * | 2015-09-05 | 2015-12-09 | 浙江大学 | Device and method for removing ammonia nitrogen in output water of seawater denitrification reactor |
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