CN110498537A - A kind of technique that the phosphorus fluorine sewage containing ammonia nitrogen efficiently removes ammonia nitrogen - Google Patents
A kind of technique that the phosphorus fluorine sewage containing ammonia nitrogen efficiently removes ammonia nitrogen Download PDFInfo
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- CN110498537A CN110498537A CN201910829648.2A CN201910829648A CN110498537A CN 110498537 A CN110498537 A CN 110498537A CN 201910829648 A CN201910829648 A CN 201910829648A CN 110498537 A CN110498537 A CN 110498537A
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5254—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using magnesium compounds and phosphoric acid for removing ammonia
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
-
- 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
-
- 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
- C02F2001/007—Processes including a sedimentation step
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
Abstract
The invention discloses a kind of, and the phosphorus fluorine sewage containing ammonia nitrogen efficiently removes the technique of ammonia nitrogen, which can combine with the technique of conventional lime cream dephosphorization fluorine, not only removal ammonia nitrogen in sewage efficiently, inexpensive, while can also remove phosphorus fluorine in water removal.This method is optimized and innovates on the basis of the traditional chemical precipitation method, when within raw water ammonia-nitrogen content 350ppm, ammonia nitrogen removal frank has reached 97% or more, water outlet ammonia nitrogen can control within 10ppm, fully meet " Phosphate Fertilizer Industry pollution discharge standard " (GB15580-2011) related request, and processing cost can control within 2 yuan/ton, be far below conventional method.P in the slag that new process generates2O5Content is higher, recyclable to use as compound fertilizer.The present invention uses second level ammonia nitrogen removal method, has the characteristics that small investment, operating cost are low, easy to operate, stable, is generally applicable to the processing of the phosphorous ammonia nitrogen waste water of phosphate fertilizer industry.
Description
Technical field
The present invention relates to phosphate fertilizer, are specifically related to the processing technique of phosphor fluorine containing ammonia-nitrogen sewage.
Background technique
Since phosphate fertilizer industry relates generally to phosphorus ammonium, anhydrous hydrogen fluoride product so that in phosphate fertilizer industry phosphorus fluorine waste water containing compared with
The ammonia nitrogen of high concentration, by taking Wengfu chemical company as an example, ammonia-nitrogen content reaches 350ppm or so, periphery phosphorus fluorine in acid phosphorus fluorine sewage
There is the higher phenomenon of ammonia-nitrogen content in waste water in industry.
The method of ammonia nitrogen has blow-off method, membrane separation process, break point chlorination method, ion-exchange in removal phosphate waste at present
And chemical precipitation method.
Blow-off method is that solution ph is adjusted to alkalinity, is taken free ammonia out of from waste water by carrier gas, which, which exists, blows
The shortcomings that Tuo Taneiyi fouling, ammonia nitrogen removal efficiency are lower, and there are secondary pollutions, currently, the technique is mostly pretreating process.
Membrane separation process is to be separated using the selectivity of film to solution ammonia nitrogen, technique there is the easy fouling blockage of film, again
The raw feature that backwash is frequent, processing cost is high, thus the technique compared be suitable for through pretreatment or low concentration ammonia nitrogen waste water at
Reason.
Break point chlorination method is that chlorine reacts the harmless nitrogen of generation, N with ammonia except the mechanism of ammonia nitrogen2Loss enters atmosphere and reaches de-
Out in waste water ammonia nitrogen purpose, break point chlorination method is suitable for the≤ammonia nitrogen in waste water concentration of 40ppm, and there is processing costs for the technique
It is high and have the shortcomings that secondary pollution of chlorine residue.
Ion-exchange is the method for utilizing ammonia nitrogen in the material removal waste water for having very strong selection suction-operated to ammonium ion,
When handling high-concentration ammonia nitrogenous wastewater, have the shortcomings that regeneration is frequent, complicated for operation, is usually used in administering controlling for Low Concentration Ammonia Containing Wastewater
Reason.
Chemical precipitation method is by making the NH in waste water to containing magnesium compound and phosphate is added in ammonia nitrogen waste water4 +With Mg2 +、PO4 3-Reaction generates magnesium ammonium phosphate sediment in aqueous solution, to achieve the purpose that remove ammonia nitrogen.Existing literature is shown, to be made
Ammonia nitrogen removal rate highest need to keep proportion n (NH4 +): n(Mg2+): n (PO4 3+)=1:1.4:1, when initial concentration is 200ppm,
Aqueous concentration is 18~30ppm, and removal rate is 88% or so, can not disposably remove in place ammonia nitrogen, depth ammonia nitrogen need to be taken to go
Except technique could will be within ammonia nitrogen removal to discharge standard in water.Existing literature is all made of primary first-order equation removal ammonia nitrogen technique, makes
It obtains except discharge standard is not achieved in ammonia nitrogen effect, limits the extensive use of the technique.
Summary of the invention
It is high the technical problem to be solved by the present invention is to provide a kind of phosphorus fluorine sewage containing ammonia nitrogen in view of the drawbacks of the prior art
The technique that effect removes ammonia nitrogen.
Realize technological means of the invention:
Dephosphorization fluorine ammonia nitrogen in waste water new process of the present invention, comprising the following steps:
(1) it is 6~7 by sour water pH Con trolling index with milk of lime, technical grade oxidation is added in the clear liquid after settlement treatment
Magnesium, additional amount are 3 times or more of ammonia nitrogen concentration in water, and phosphorus content need to control the 2 times or more in ammonia nitrogen concentration in water；
(2) at 1.5~2 hours, pH was controlled 8~9, if reaction slurry pH is low the slurry reaction time control after magnesia is added
In 8, lime slurry is suitably filled into slurry, its pH is made to reach requirement, and temperature is room temperature.
(3) the slurry reaction slurry of magnesia is added after settlement treatment, a small amount of milk of lime is added into clear liquid, by solution
9~10, the reaction time is 20 minutes or more for pH control, and slurry carries out supernatant processing, and clear liquid enters lower one of dephosphorization program.
(4) clear liquid after third step reaction supernatant enters the milk of lime neutralization reaction in dephosphorization stage, and pH is controlled 11.5
More than, the reaction time is 20 minutes or more.
In above-mentioned steps: the medicament configuration method: MgO is technical grade, and using aqueous solution addition manner, concentration is not
By；Milk of lime setup time is more than 30 minutes, and concentration is 10~15%.
In above-mentioned steps (2): the slurry reaction time after magnesia is added controlled at 1.5~2 hours.
Wherein: step (2), (3) are the ammonia nitrogen removal stage of reaction, and the slag of generation is mainly magnesium phosphate and entrainment portions phosphoric acid
Ammonium magnesium, phosphorus pentoxide content is higher in slag, reaches 27% or more, this part slag can reuse do fertilizer or additive for compound fertilizer into
Row recycling.
For the present invention compared with current chemical precipitation method process description, it is n that the present invention, which has redefined first step proportion,
(NH4 +): n(Mg2+): n (PO4 3+The ammonia nitrogen method for pretreating of)=1:3.6:2, and increased second step milk of lime newly and removed ammonia nitrogen technique,
Two steps, which combine, removes ammonia nitrogen, so that raw water ammonia-nitrogen content is discharged ammonia-nitrogen content≤10ppm, completely not higher than in the case of 350ppm
Meet current " Phosphate Fertilizer Industry pollution discharge standard " (GB15580-2011) related request, and processing cost can control
Within 2 yuan/ton.
The present invention has innovated chemical precipitation to be had low cost, efficiently removes the advantages of ammonia nitrogen except ammonia nitrogen technique, while can and be passed
System dephosphorization fluorine technique combines, and has and is widely popularized value.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
In figure: 1-pH regulating tank；2- primary sedimentation tank；3- ammonia nitrogen pretreatment tank；4- preliminary sedimentation tank；5- NH_3-N treating slot；6- sedimentation
Slot；7- dephosphorization reactive tank；8- dephosphorization subsider.
Specific embodiment
Example 1
Phosphorous ammonia nitrogen waste water 800ml is measured in 1000mlA beaker, sampling analysis [NH3-N]348ppm、pH3.5、[P5+]
1100ppm、[F-] 298ppm, pre-configured milk of lime is added into beaker, pH is adjusted to 6.8 under agitation, instead
After answering 30 minutes, into beaker plus a small amount of PAM liquid (1 ‰) is added, to slurry supernatant 10 minutes.
Take supernatant liquid into 1000mlB beaker, volume about 720ml takes clear liquid to analyze [NH3-N]320ppm、pH6.5、
[P5+]720ppm、[F-]20ppm.Weigh technical grade MgO(MgO >=85%) 0.9 gram, after adding 5.0 grams of water to be adjusted into solution state
It pours into B beaker reaction slurry, is reacted 1.5 hours under stirring state.
After 1.5 hours, reaction slurry pH value rises to 8.6, into beaker plus a small amount of PAM liquid (1 ‰) is added, to slurry supernatant
After ten minutes, clear liquid is moved in 1000mlC beaker, clear liquid is taken to analyze [NH3- N] 18ppm, a small amount of lime is added to C beaker
PH value is promoted to 9.4 under agitation by lotion, is controlled the reaction time 30 minutes.
After 30 minutes, into beaker plus a small amount of PAM liquid (1 ‰) of addition after ten minutes to slurry supernatant moves to clear liquid
In 1000mlD beaker, clear liquid is taken to analyze [NH3- N] 5.6ppm, a small amount of lime slurry is added to D beaker, under agitation will
PH value is promoted to 11.7, controls the reaction time 30 minutes.
After 30 minutes, into beaker plus a small amount of PAM liquid (1 ‰) is added, after ten minutes to slurry supernatant, analyzes in clear liquid
[NH3-N] 5.2ppm、[P5+]0.3ppm、[F-]3ppm。
Example 2
Phosphorous ammonia nitrogen waste water 800ml is measured in 1000mlA beaker, sampling analysis [NH3-N]316ppm、pH3.1、[P5+]
1260ppm、[F-] 314ppm, pre-configured milk of lime is added into beaker, pH is adjusted to 6.2 under agitation, instead
After answering 30 minutes, into beaker plus a small amount of PAM liquid (1 ‰) is added, allows slurry supernatant 10 minutes.
Take supernatant liquid into 1000mlB beaker, volume about 740ml takes clear liquid to analyze [NH3-N]289ppm、pH6.4、
[P5+]670ppm、[F-]32ppm.Weigh technical grade MgO(MgO >=85%) 0.9 gram, after adding 5.0 grams of water to be adjusted into solution state
It pours into B beaker reaction slurry, reacts 1.5 hours under agitation.
After 1.5 hours, reaction slurry pH value rises to 8.2, into beaker plus a small amount of PAM liquid (1 ‰) is added, to slurry supernatant
After ten minutes, clear liquid is moved in 1000mlC beaker, clear liquid is taken to analyze [NH3- N] 24ppm, a small amount of milk of lime is added to C beaker
PH value is promoted to 9.2 under agitation by liquid, is controlled the reaction time 30 minutes.
After 30 minutes, into beaker plus a small amount of PAM liquid (1 ‰) of addition after ten minutes to slurry supernatant moves to clear liquid
In 1000mlD beaker, clear liquid is taken to analyze [NH3- N] 7.2ppm, a small amount of lime slurry is added to D beaker, under agitation will
PH value is promoted to 11.6, controls the reaction time 30 minutes.
After 30 minutes, into beaker plus a small amount of PAM liquid (1 ‰) is added, after ten minutes to slurry supernatant, analyzes in clear liquid
[NH3-N] 6.7ppm、[P5+]0.4ppm、[F-]5ppm。
Example 3
Phosphorous ammonia nitrogen waste water 800ml is measured in 1000mlA beaker, sampling analysis [NH3-N]350ppm、pH2.8、[P5+]
1354ppm、[F-] 426ppm, pre-configured milk of lime is added into beaker, pH is adjusted to 6.1 under agitation, instead
After answering 30 minutes, into beaker plus a small amount of PAM liquid (1 ‰) is added, allows slurry supernatant 10 minutes.
Take supernatant liquid into 1000mlB beaker, volume about 690ml takes clear liquid to analyze [NH3-N]326ppm、pH6.1、
[P5+]683ppm、[F-]29ppm.Weigh technical grade MgO(MgO >=85%) 0.9 gram, after adding 5.0 grams of water to be adjusted into solution state
It pours into B beaker reaction slurry, reacts 1.5 hours under agitation.
After 1.5 hours, reaction slurry pH value rises to 7.9, adds a small amount of milk of lime of addition will into beaker under agitation
PH is promoted to 8.6, reacts 30 minutes, a small amount of PAM liquid (1 ‰) is added and after ten minutes to slurry supernatant moves to clear liquid
In 1000mlC beaker, clear liquid is taken to analyze [NH3- N] 26ppm, a small amount of lime slurry is added to C beaker, under agitation by pH
Value is promoted to 9.6, controls the reaction time 30 minutes.
After 30 minutes, into beaker plus a small amount of PAM liquid (1 ‰) of addition after ten minutes to slurry supernatant moves to clear liquid
In 1000mlD beaker, clear liquid is taken to analyze [NH3- N] 8.6ppm, a small amount of lime slurry is added to D beaker, under agitation will
PH value is promoted to 11.8, controls the reaction time 30 minutes.
After 30 minutes, into beaker plus a small amount of PAM liquid (1 ‰) is added, after ten minutes to slurry supernatant, analyzes in clear liquid
[NH3-N] 7.8ppm、[P5+]0.3ppm、[F-]4ppm。
The phosphorous ammonia nitrogen waste water of table 1 removes ammonia nitrogen experimental conditions table (concentration is in terms of ppm)
Claims (4)
1. a kind of phosphorus fluorine sewage containing ammonia nitrogen efficiently removes the technique of ammonia nitrogen, it is characterized in that the following steps are included:
(1) it is 6~7 by sour water pH Con trolling index with milk of lime, technical grade oxidation is added in the clear liquid after settlement treatment
Magnesium, additional amount are 3 times or more of ammonia nitrogen concentration in water, and phosphorus content need to control the 2 times or more in ammonia nitrogen concentration in water；
(2) at 1.5~2 hours, pH was controlled 8~9, if reaction slurry pH is low the slurry reaction time control after magnesia is added
In 8, lime slurry is suitably filled into slurry, its pH is made to reach requirement, and temperature is room temperature；
(3) the slurry reaction slurry of magnesia is added after settlement treatment, a small amount of milk of lime is added into clear liquid, by pH value of solution control
For system 9~10, the reaction time is 20 minutes or more, and slurry carries out supernatant processing, and clear liquid enters lower one of dephosphorization program；
(4) clear liquid after third step reaction supernatant enters the milk of lime neutralization reaction in dephosphorization stage, by pH control 11.5 or more,
Reaction time is 20 minutes or more.
2. the phosphorus fluorine sewage containing ammonia nitrogen efficiently removes the technique of ammonia nitrogen as described in claim 1, it is characterized in that: MgO is technical grade,
Using aqueous solution addition manner, no matter concentration；Milk of lime setup time is more than 30 minutes, and concentration is 10~15%.
3. the phosphorus fluorine sewage containing ammonia nitrogen efficiently removes the technique of ammonia nitrogen as described in claim 1, it is characterized in that: after magnesia is added
The slurry reaction time control at 1.5~2 hours.
4. the phosphorus fluorine sewage containing ammonia nitrogen efficiently removes the technique of ammonia nitrogen as described in claim 1, it is characterized in that:
Step (2), (3) are the ammonia nitrogen removal stage of reaction, and the slag of generation is mainly magnesium phosphate and entrainment portions ammonium magnesium phosphate, in slag
Phosphorus pentoxide content is higher, reaches 27% or more, this part slag can reuse make fertilizer or additive for compound fertilizer is recycled.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111115912A (en) * | 2020-03-02 | 2020-05-08 | 瓮福（集团）有限责任公司 | Process for removing ammonia nitrogen from phosphorus-fluorine sewage containing ammonia nitrogen by one-step method |
| CN111233194A (en) * | 2020-01-15 | 2020-06-05 | 东江环保股份有限公司 | Method for treating waste liquid |
| CN112062343A (en) * | 2020-09-08 | 2020-12-11 | 湖北美辰环保股份有限公司 | MAP method-based harmless recycling treatment method for phosphogypsum yard leachate |
| CN115073242A (en) * | 2022-07-22 | 2022-09-20 | 中南民族大学 | Composite soil conditioner based on phosphorus chemical alkaline residue and preparation method and application thereof |
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| CN112062343A (en) * | 2020-09-08 | 2020-12-11 | 湖北美辰环保股份有限公司 | MAP method-based harmless recycling treatment method for phosphogypsum yard leachate |
| CN115073242A (en) * | 2022-07-22 | 2022-09-20 | 中南民族大学 | Composite soil conditioner based on phosphorus chemical alkaline residue and preparation method and application thereof |
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Application publication date: 20191126 |