CN105174241A - Method for recovering high-purity magnesium ammonium phosphate from swine wastewater - Google Patents
Method for recovering high-purity magnesium ammonium phosphate from swine wastewater Download PDFInfo
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- CN105174241A CN105174241A CN201510577385.2A CN201510577385A CN105174241A CN 105174241 A CN105174241 A CN 105174241A CN 201510577385 A CN201510577385 A CN 201510577385A CN 105174241 A CN105174241 A CN 105174241A
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- magnesium
- ammonium phosphate
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Abstract
The invention relates to a method for recovering high-purity magnesium ammonium phosphate from swine wastewater. The method mainly comprises the following steps of a, adding the swine wastewater into a magnesium ammonium phosphate continuous flow reaction tank, building an aeration column filling with magnesium metal balls and graphite particles in the reaction tank, after the wastewater is entered, starting an aeration pump to aerate an air diffuser on the lower end of the aeration column, meanwhile, starting a stirrer in the reaction tank, and controlling the water power of the reaction tank to stay for 10 to 20min; b, continuously and automatically flowing the wastewater processed by the reaction tank to a settling basin for chemicals, standing for 60 to 80min, automatically flowing supernate into other follow-up processing steps, continuously discharging generated magnesium ammonium phosphate sediments from the bottom part of the settling basin for chemicals through static pressure, then dehydrating through a centrifugal machine, and naturally drying to obtain the high-purity magnesium ammonium phosphate. The method is simple to operate, and has no need to add magnesium salt and sodium hydroxide tediously, and the phosphorus recovery efficiency can achieve more than 97 percent; the purity of the recovered magnesium ammonium phosphate can achieve more than 95 percent, so that the recovered magnesium ammonium phosphate can be used as agricultural fertilizers.
Description
Technical field
The invention belongs to technical field of resource recovery, particularly a kind of method reclaiming magnesium ammonium phosphate from waste water.
Background technology
Total institute is known, and phosphorus is the necessary element of various biology, is also one of key pollutants causing body eutrophication simultaneously.In recent years, along with China's economy and population increase fast, water environmental problems is just becoming and is becoming increasingly conspicuous, especially body eutrophication problem, now serious threat to the productive life of the mankind and the eubiosis.Phosphoric in water body mainly comes from the discharge of production and sanitary sewage, and receiving water body phosphorus content is exceeded standard, and causes various algae and microbiological anomaly in water body to increase, makes the smelly and various fish kills of water body blackout.Phosphorus in sewage directly discharges without strict process, not only makes receiving water body face severe contamination and threatens, this valuable resource of phosphorus also can be caused to waste greatly simultaneously.According to the literature, phosphorus is that modern production is lived necessary element, the exploitation of Rock Phosphate (72Min BPL) and refinement are that the current mankind obtain phosphoric main path, if but according to the spending rate of the existing Rock Phosphate (72Min BPL) of the mankind, when not taking any sustainable use measure, existing explored Rock Phosphate (72Min BPL) reserves will at 100 years internal consumptions totally in the world.Therefore, from waste water, reclaim phosphorus will become extremely meaningful for the prevention of water pollution and the Sustainable development of phosphate rock resource.
China is that pork consumes big country, and live pig breeding stock is large, and this just makes China's Pig raising wastewater quantity discharged very big.Pig raising wastewater is a kind of waste water containing ammonia nitrogen in high density and phosphorus, and phosphorus concentration is raised to hundreds of milligrams per liter scope at tens of micrograms usually, and ammonia nitrogen then reaches hundreds of to thousands of milligrams per liter.Therefore, the impact of this kind of wastewater in waters eutrophication is very big, and from this kind of waste water, reclaim the valuable resource such as nitrogen, phosphorus, not only can solve the problem of contaminated wastewater, also can obtain certain economic benefit simultaneously.Reclaiming phosphorus and ammonia nitrogen with the form of magnesium ammonium phosphate sediment is a kind of resource reclaim technology being subject to extensive concern in recent years.Magnesium ammonium phosphate is commonly called as struvite (MagnesiumAmmoniumPhosphate, MAP), and it is found by Rawn early than nineteen thirty-nine in the research process utilizing digested sludge process waste water, and its molecular formula is MgNH
4pO
46H
2o is a kind of white crystalline material of indissoluble.As Mg in solution
2+, NH
4 +and PO
4 3 –ionic concn reaches a threshold value, and when being within the scope of optimum pH, MAP by following reaction formula generation spontaneous nucleation, thus can reach the object reclaiming ammonia nitrogen and phosphorus in waste water.
Mg
2++NH
4 ++HPO
4 3–+6H
2O→MgNH
4PO
4·6H
2O↓+H
+(1)
It is high that this technology has nitrogen phosphorous recovery, is swift in response, the advantage that precipitate and separate is effective.But, owing to lacking magnesium ion in Pig raising wastewater, a certain amount of magnesium ion must be supplemented from the external world and just can make ammonia nitrogen and the reaction of phosphorus generation ammoniomagnesium phosphate crystal waste water.In addition, can find from reaction formula (1), this reaction be made to carry out also must adding alkali to regulate pH to optimum range.At present, utilize magnesium ammonium phosphate sediment technology from Pig raising wastewater, reclaim nitrogen phosphorus mainly real by adding magnesium chloride and magnesium sulfate in waste water, during reaction also needing to add sodium hydroxide carrys out regulator solution pH simultaneously.Although the method can obtain the magnesium ammonium phosphate crystal of higher degree, but in practice process, there is many problems: 1) reagent adition process is difficult to realize automated operation, 2) in reaction process, the content strictly determining Phosphorus From Wastewater is needed, to guarantee the dosage of magnesium, 3) in reaction process, the adjustment of pH is very loaded down with trivial details, 4) magnesium salts and sodium hydroxide reagent consumption greatly, increase manual operation cost.In addition, for reducing the cost reclaiming magnesium ammonium phosphate, also have use magnesium oxide, produce in calcined magnesite process containing magnesium by product (main component is MgO), magnisite thing, seawater nanofiltration concentrated solution, report as the technology in magnesium source containing magnesium waste water etc.Although use this kind of magnesium medicament that contains can effectively reduce magnesium ammonium phosphate cost recovery, the magnesium ammonium phosphate quality reclaimed is extremely low, is substantially difficult to as product application to other approach.
, mainly there is following problem for the technology of nitrogen phosphorus in magnesium ammonium phosphate sediment recovery Pig raising wastewater at present in comprehensive above-mentioned discussion:
1. use the magnesium salts such as magnesium chloride and magnesium sulfate to reclaim nitrogen phosphorus in Pig raising wastewater as precipitation agent, there is complicated operation, be difficult to realize automatic business processing, and processing cost is higher.
2. adopt magnesium oxide or other containing magnesium by product as magnesium source, not only there is complicated operation equally and be difficult to the problem of automatic business processing, also there is the problem that the magnesium ammonium phosphate quality of recovery is low simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of simple to operate, with low cost, method reclaiming high-purity phosphoric acid ammonium magnesium from Pig raising wastewater that phosphorous recovery is high.
Method of the present invention is as follows:
A, first wastewater streams of raising pigs enters magnesium ammonium phosphate Continuous Flow reaction tank, the built-in self-control air aeration post of this reaction tank, the plastic wire that this aeration post is 0.5mm by screen distance is made, interior filling magnesium prill and graphite granule, aeration column bottom is an air diffuser, this air diffuser is connected with an outside aeration pump, after Pig raising wastewater enters this reaction tank, start aeration pump and carry out aeration, start the agitator be built in this reaction tank simultaneously, keep the water flow identical with flooding velocity, controlling this reaction tank hydraulic detention time is 10 ~ 20min, ensure that wastewater pH is 8.5 ~ 9.
Described magnesium prill is the metal simple-substance bead of purity more than 95%, and described graphite granule is common graphite bead, and without concrete purity requirement, the particle diameter of magnesium Metal Ball and graphite granule must be greater than aeration post mesh aperture more than 2 times.
The magnesium prill quality of described aeration column packed determines according to the volume of waste water in Continuous Flow reaction tank, magnesium metal quality controls at 4 ~ 6g/L with wastewater volume ratio, graphite granule adds by with magnesium Metal Ball mass ratio, and graphite and magnesium mass ratio are 0 ~ 1:1.
Aeration rate in described aeration post is determined according to Metal Ball quality, and in reaction process, aeration control is at 0.2 ~ 0.3L/gmin.
B, waste water after step a process, from reaction tank continuous self-flowing to chemical precipitation pond, then leave standstill 60 ~ 80min, and supernatant liquor gravity flow enters other processing links follow-up, and the magnesium ammonium phosphate white precipitate of generation is discharged by static pressure continuously by bottom chemical precipitation pond.
The magnesium ammonium phosphate sediment that c, chemically settling tank discharge, after centrifuge dewatering, naturally dries and can obtain highly purified magnesium ammonium phosphate product.
Know-why of the present invention:
Very easily there is following galvanic corrosion in magnesium metal, add graphite granule and then can accelerate this galvanic corrosion effect in waste water.
Mg→Mg
2++2e
–(1)
H
2O+2e
–→H
2+2OH
–(2)
Air aeration then can accelerate magnesium Metal Ball surface produce magnesium ion and hydroxide ion enter in the middle of waste water system.Can find out that waste water, pH value of solution and magnesium ion concentration have closely related from above-mentioned reaction formula, test-results shows, according to aforesaid operations method and step, control waste water hydraulic detention time 10 ~ 20min, then can ensure that wastewater pH is in 8.5 ~ 9 scopes, and this pH scope is just in time the optimum PH range of ammoniomagnesium phosphate crystal, magnesium ion residual concentration is minimum in solution under this condition in addition, this greatly reduces the consumption of magnesium metal, decreases phosphorus cost recovery.
The present invention compared with prior art tool has the following advantages:
1, simple to operate, do not need loaded down with trivial details to add magnesium salts and sodium hydroxide, after once adding enough magnesium Metal Ball, automatization can be realized and reclaim magnesium ammonium phosphate, greatly reduce human users's cost.
2, phosphorus organic efficiency is high, can reach more than 97% to the phosphorous recovery in Pig raising wastewater.
3, the magnesium ammonium phosphate purity reclaimed is high, and the magnesium ammonium phosphate purity of recovery can reach more than 95%, can be used as agrochemical completely and uses.
Accompanying drawing explanation
Fig. 1 is general flow chart of the present invention.
Embodiment
Embodiment 1:
The method flow diagram reclaiming high-purity phosphoric acid ammonium magnesium from Pig raising wastewater according to Fig. 1, first ammonia nitrogen and phosphorus concentration are respectively the Pig raising wastewater of 908mg/L and 125mg/L, first magnesium ammonium phosphate Continuous Flow reaction tank 2 (reactor reaction zone volume is for 17L) is entered with the flooding velocity of 102L/h, the built-in self-control air aeration post 3 of this reaction tank, the plastic wire that this aeration post is 0.5mm by screen distance is made, in aeration post, add 68g purity is respectively 96%, the common graphite bead of particle diameter to be the magnesium Metal Ball (i.e. 4g/L) of 2 ~ 3mm and 68g particle diameter be 1.5 ~ 2mm, aeration column bottom is an air diffuser, this air diffuser is connected with an outside aeration pump 1 (Japanese SECOH aeration pump TK0200), after Pig raising wastewater enters this reaction tank, start aeration pump and carry out aeration, control aeration rate at 13.6L/min (i.e. 0.2L/gmin), start the agitator 4 be built in this reaction tank simultaneously, control agitator stirring velocity at 200rpm, adjusting water outlet speed equals water intake velocity, controlling reaction tank hydraulic detention time is 10min, wastewater pH is 8.5.Waste water after the process of magnesium ammonium phosphate successive reaction pond flow to chemical precipitation pond 5 certainly from reaction tank, then 60min is left standstill, supernatant liquor gravity flow enters other processing links follow-up, the magnesium ammonium phosphate white precipitate generated is discharged by static pressure by bottom chemical precipitation pond, chemically the magnesium ammonium phosphate sediment of settling tank discharge is after whizzer 6 dewaters, and naturally dries and can obtain highly purified magnesium ammonium phosphate product.Result shows, after the method process, in Pig raising wastewater, phosphorous recovery is 97.7%, and the magnesium ammonium phosphate purity of recovery is 96.8%.
Embodiment 2:
Ammonia nitrogen and phosphorus concentration are respectively the Pig raising wastewater of 1215mg/L and 213mg/L, first magnesium ammonium phosphate Continuous Flow reaction tank (reactor reaction zone volume is for 17L) is entered with the flooding velocity of 68L/h, the built-in self-control air aeration post of this reaction tank, the plastic wire that this aeration post is 0.5mm by screen distance is made, in aeration post, add 68g purity is respectively 97%, the common graphite bead of particle diameter to be the magnesium Metal Ball (i.e. 4g/L) of 3 ~ 4mm and 34g particle diameter be 2 ~ 3mm, aeration column bottom is an air diffuser, this air diffuser is connected with an outside aeration pump 1 (Japanese SECOH aeration pump TK0200), after Pig raising wastewater enters this reaction tank, start aeration pump, control aeration rate at 20.4L/min (i.e. 0.3L/gmin), start the agitator be built in this reaction tank simultaneously, control agitator stirring velocity at 200rpm, adjusting water outlet speed equals water intake velocity, controlling reaction tank hydraulic detention time is 15min, wastewater pH is 9.Waste water after the process of magnesium ammonium phosphate successive reaction pond flow to chemical precipitation pond certainly from reaction tank, then 80min is left standstill, supernatant liquor gravity flow enters other processing links follow-up, the magnesium ammonium phosphate white precipitate generated is discharged by static pressure by bottom chemical precipitation pond, chemically the magnesium ammonium phosphate sediment of settling tank discharge is after centrifuge dewatering, naturally dries and can obtain highly purified magnesium ammonium phosphate product.Result shows, after the method process, in Pig raising wastewater, phosphorous recovery is 98.8%, and the magnesium ammonium phosphate purity of recovery is 96.1%.
Embodiment 3:
Ammonia nitrogen and phosphorus concentration are respectively the Pig raising wastewater of 1037mg/L and 113mg/L, first magnesium ammonium phosphate Continuous Flow reaction tank (reactor reaction zone volume is for 17L) is entered with the flooding velocity of 102L/h, the built-in self-control air aeration post of this reaction tank, the plastic wire that this aeration post is 0.5mm by screen distance is made, in aeration post, add 102g purity is 96%, particle diameter is the magnesium Metal Ball (i.e. 6g/L) of 2 ~ 3mm, aeration column bottom is an air diffuser, this air diffuser is connected with an outside aeration pump 1 (Japanese SECOH aeration pump TK0200), after Pig raising wastewater enters this reaction tank, start aeration pump, control aeration rate at 20.4L/min (i.e. 0.2L/gmin), start the agitator be built in this reaction tank simultaneously, control agitator stirring velocity at 200rpm, adjusting water outlet speed equals water intake velocity, controlling reaction tank hydraulic detention time is 10min, wastewater pH is 8.5.Waste water after the process of magnesium ammonium phosphate successive reaction pond flow to chemical precipitation pond certainly from reaction tank, then 70min is left standstill, supernatant liquor gravity flow enters other processing links follow-up, the magnesium ammonium phosphate white precipitate generated is discharged by static pressure by bottom chemical precipitation pond, chemically the magnesium ammonium phosphate sediment of settling tank discharge is after centrifuge dewatering, naturally dries and can obtain highly purified magnesium ammonium phosphate product.Result shows, after the method process, in Pig raising wastewater, phosphorous recovery is 98.3%, and the magnesium ammonium phosphate purity of recovery is 96.6%.
Embodiment 4:
Ammonia nitrogen and phosphorus concentration are respectively the Pig raising wastewater of 1537mg/L and 156mg/L, first magnesium ammonium phosphate Continuous Flow reaction tank (reactor reaction zone volume is for 17L) is entered with the flooding velocity of 51L/h, the built-in self-control air aeration post of this reaction tank, the plastic wire that this aeration post is 0.5mm by screen distance is made, in aeration post, add 85g purity is respectively 95%, the common graphite bead of particle diameter to be the magnesium Metal Ball (i.e. 5g/L) of 3 ~ 5mm and 85g particle diameter be 2 ~ 3mm, aeration column bottom is an air diffuser, this air diffuser is connected with an outside aeration pump 1 (Japanese SECOH aeration pump TK0200), after Pig raising wastewater enters this reaction tank, start aeration pump, control aeration rate at 17L/min (i.e. 0.2L/gmin), start the agitator be built in this reaction tank simultaneously, control agitator stirring velocity at 200rpm, adjusting water outlet speed equals water intake velocity, controlling reaction tank hydraulic detention time is 20min, wastewater pH is 9.Waste water after the process of magnesium ammonium phosphate successive reaction pond flow to chemical precipitation pond certainly from reaction tank, then 80min is left standstill, supernatant liquor gravity flow enters other processing links follow-up, the magnesium ammonium phosphate white precipitate generated is discharged by static pressure by bottom chemical precipitation pond, chemically the magnesium ammonium phosphate sediment of settling tank discharge is after centrifuge dewatering, naturally dries and can obtain highly purified magnesium ammonium phosphate product.Result shows, after the method process, in Pig raising wastewater, phosphorous recovery is 98.9%, and the magnesium ammonium phosphate purity of recovery is 96.9%.
Claims (5)
1. from Pig raising wastewater, reclaim a method for high-purity phosphoric acid ammonium magnesium, it is characterized in that: it comprises following treatment process and step:
A, first wastewater streams of raising pigs enters magnesium ammonium phosphate Continuous Flow reaction tank, the built-in self-control air aeration post of this reaction tank, this aeration post is made by plastic wire, interior filling magnesium prill and graphite granule, aeration column bottom is an air diffuser, this air diffuser is connected with an outside aeration pump, after Pig raising wastewater enters this reaction tank, start aeration pump and carry out aeration, start the agitator be built in this reaction tank simultaneously, keep the water flow identical with flooding velocity, controlling this reaction tank hydraulic detention time is 10 ~ 20min, ensure that wastewater pH is 8.5 ~ 9,
B, waste water after step a process, from reaction tank continuous self-flowing to chemical precipitation pond, then leave standstill 60 ~ 80min, and supernatant liquor gravity flow enters other processing links follow-up, and the magnesium ammonium phosphate white precipitate of generation is discharged by static pressure continuously by bottom chemical precipitation pond;
The magnesium ammonium phosphate sediment that c, chemically settling tank discharge, after centrifuge dewatering, naturally dries and can obtain highly purified magnesium ammonium phosphate product.
2. a kind of method reclaiming high-purity phosphoric acid ammonium magnesium from Pig raising wastewater according to claim 1, is characterized in that: the screen distance of described aeration post plastic wire is 0.5mm.
3. a kind of method reclaiming high-purity phosphoric acid ammonium magnesium from Pig raising wastewater according to claim 1, it is characterized in that: described magnesium prill is the metal simple-substance bead of purity more than 95%, described graphite granule is common graphite bead, without concrete purity requirement, the particle diameter of magnesium Metal Ball and graphite granule must be greater than aeration post mesh aperture more than 2 times.
4. a kind of method reclaiming high-purity phosphoric acid ammonium magnesium from Pig raising wastewater according to claim 1, it is characterized in that: the magnesium prill quality of described aeration column packed determines according to the volume of waste water in Continuous Flow reaction tank, magnesium metal quality controls at 4 ~ 6g/L with wastewater volume ratio, graphite granule adds by with magnesium Metal Ball mass ratio, and graphite and magnesium mass ratio are 0 ~ 1:1.
5. a kind of method reclaiming high-purity phosphoric acid ammonium magnesium from Pig raising wastewater according to claim 1, is characterized in that: the aeration rate in described aeration post is determined according to Metal Ball quality, and in reaction process, aeration control is at 0.2 ~ 0.3L/gmin.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012011375A (en) * | 2010-06-04 | 2012-01-19 | Blue Aqua Industry Kk | Method and apparatus for treating wastewater |
| US20140076804A1 (en) * | 2012-09-19 | 2014-03-20 | Damian J. Kruk | Struvite Precipitation Using Magnesium Sacrificial Anode |
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2015
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012011375A (en) * | 2010-06-04 | 2012-01-19 | Blue Aqua Industry Kk | Method and apparatus for treating wastewater |
| US20140076804A1 (en) * | 2012-09-19 | 2014-03-20 | Damian J. Kruk | Struvite Precipitation Using Magnesium Sacrificial Anode |
Non-Patent Citations (3)
| Title |
|---|
| ALEXANDRA HUG ET AL.: "Struvite precipitation from urine with electrochemical magnesium dosage", 《WATER RESEARCH》 * |
| DAMIAN J.KRUK ET AL.: "Struvite precipitation and phosphorus removal using magnesium sacrificial anode", 《CHEMOSPHERE》 * |
| HUAN ZHAO ET AL.: "A simple method for the preparation of magnesium phosphate conversion coatings on a AZ31 magnesium alloy with improved corrosion resistance", 《RSC ADVANCES》 * |
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Effective date of registration: 20210429 Address after: 066100 Room 101, 72 Lianfeng Road, Beidaihe District, Qinhuangdao City, Hebei Province Patentee after: Qinhuangdao Mingchao Environmental Technology Co.,Ltd. Address before: Hebei Street West Harbor area, 066004 Hebei city of Qinhuangdao province No. 438 Patentee before: Yanshan University |