CN107473444A - A kind of pig farm tail water nitrogen and phosphorus element recovery method - Google Patents
A kind of pig farm tail water nitrogen and phosphorus element recovery method Download PDFInfo
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- CN107473444A CN107473444A CN201710796657.7A CN201710796657A CN107473444A CN 107473444 A CN107473444 A CN 107473444A CN 201710796657 A CN201710796657 A CN 201710796657A CN 107473444 A CN107473444 A CN 107473444A
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/165—Natural alumino-silicates, e.g. zeolites
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
-
- 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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/20—Nature of the water, waste water, sewage or sludge to be treated from animal husbandry
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/20—Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Fertilizers (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention belongs to tail water application technology as the second resource field, discloses a kind of recovery of pig farm tail water nitrogen and phosphorus element.Recovery method of the present invention specifically includes following steps:(1) modified zeolite is added in tail water I, stirring, adds coagulant solution, be well mixed, obtain tail water II;(2) pH to 7~8 of tail water II is adjusted, is stirred, is stood, separation of solid and liquid, tail water and coagulation sludge after being handled.Recovery method of the present invention deepens high treating effect to livestock and poultry cultivation tail water particularly pig farm tail water, can high-efficient denitrification and dephosphorization and remove COD, nitrogen phosphorus organic composite fertilizer can be used as by reclaiming obtained coagulation sludge simultaneously, realize recycling, and technique simple and stable, production cost is low, easily realizes large-scale application.The present invention also provides the coagulation sludge that above-mentioned recovery method is prepared, and is obtained by being dehydrated the obtained coagulation sludge, draining processing.The obtained coagulation sludge can be applied to prepare in fertilizer.
Description
Technical field
The invention belongs to tail water application technology as the second resource field, more particularly to a kind of pig farm tail water nitrogen and phosphorus element returns
Receive.
Background technology
The element such as rich Nitrogen-and Phosphorus-containing is cause lake eutrophication and blue-green alga bloom large-scale outbreak important in the tail water of pig farm
Reason.Wherein tail water constituent in pig farm is complicated, COD, TP, NH4 +- N concentration is high, and intractability is big, cost is high, incompletely processed
A series of serious water environmental problems can be caused.State Ministry of Environmental Protection has been carried out secondary soliciting meaning to livestock breeding wastewater discharge standard
(ring does letter [2014] 335) is seen, wherein to TP, COD and NH4 +- N discharge standard is from original (GB 18596-2001)
8.0mg/L, 400mg/L, 80mg/L carry mark and arrive 5.0mg/L, 150mg/L, 40mg/L respectively, and conventional pig farm processing, which is difficult to reach, to be carried
Discharge standard after mark.Meanwhile conventional pig farm tail water processing can produce a large amount of sludge, the follow-up disposal of sludge also turns into a difficulty
Topic.But the phosphorous nitrogen substance contained in tail water is nutrient necessary to plant growth, by containing in the tail water of pig farm
Phosphorus nitrogen substance effectively solidifies, and prior art is mainly MAP guanite techniques, but MAP guanite techniques have more strict fit
With condition, such as certain N/P ratio, narrower pH scopes, operationally there is certain difficulty.Therefore, it is necessary to develop more
The technical method of effective and easily operated management.
Prior art, which also has, is modified research to zeolite, and the removal effect of existing zeolite and artificial zeolite to ammonia nitrogen
Fruit is preferable, but the removal to water quality index such as total phosphorus and COD is then unsatisfactory.In the prior art also not by cellulose grafting
Onto artificial zeolite, in being handled applied to pig farm tail water in-depth.
The content of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, primary and foremost purpose of the invention is to provide a kind of pig farm tail water
Nitrogen and phosphorus element recovery method.Pig farm tail water after the inventive method is handled, can reach State Ministry of Environmental Protection to livestock and poultry cultivation
Tail water reuse standard has been carried out secondary COD, NH consulted on4 +The water quality index standard such as-N, TP.And after the inventive method processing
Obtained coagulation sludge can realize recycling, and the nutriment in tail water is solidified, and realize Tailwater Depth processing
Meanwhile realize that nutriment recycles, compensate cost of water treatment.
Still a further object of the present invention is to provide the coagulation sludge that a kind of above-mentioned recovery method obtains.
The purpose of the present invention is realized by following proposal:
A kind of pig farm tail water nitrogen and phosphorus element recovery method, specifically includes following steps:
(1) modified zeolite is added in tail water I, stirring, adds coagulant solution, be well mixed, obtain tail water II;
(2) pH to 7~8 of tail water II is adjusted, is stirred, is stood, separation of solid and liquid, tail water and coagulation sludge after being handled.
The dosage of modified zeolite described in step (1) is 5~10g/L tail water I.
Stirring described in step (1) is preferably 30~60min of stirring under 200~250r/min.
Coagulant solution described in step (1) is the mixed solution containing magnesium ion and iron ion.
The mol ratio of magnesium ion and iron ion is preferably 2 in described coagulant solution:1~4:1.
Described coagulant solution can be obtained by the way that at least one of molysite and magnesium salts are added to the water into dissolving;Preferably
At least one of soluble ferric iron salt and soluble magnesium salt;More preferably FeCl3And MgCl2At least one of.
The dosage of coagulant solution metal ion final concentration in tail water II is defined, preferably 50~100mg/L.I.e.
[Mg2+]+[Fe3+]=50~100mg/L.
PH is adjusted described in step (2) to be preferably adjusted by adding sodium carbonate.
Stirring described in step (2) is first quick stirring, then mix slowly;Preferably first in 150~200r/min conditions
2~5min of lower stirring, 20~30min is then stirred under the conditions of 50~100r/min.
The time stood described in step (2) is preferably 30min or more, more preferably 30~60min.
The modified zeolite is prepared by comprising the following steps method:
A. artificial zeolite is immersed in NaCl solution, heats, obtain artificial zeolite A;
B. artificial zeolite A is immersed in the acetone soln of cellulose acetate, ultrasound, stirring reaction, obtains modified zeolite.
It is preferably that 1~5h is reacted at 80~120 DEG C to heat described in step a, is more preferably reacted at 100 DEG C
3h.The heating is preferably heating water bath.
The NaCl for removing residual is preferably washed with water in zeolite after the heating, is used further to react in next step after drying.
The concentration of NaCl solution used is 0.1~0.3mol/L, more preferably 0.3mol/L in step a.
Artificial zeolite used is commercially available artificial zeolite in step a, and 200 mesh sieve are crossed before preferably using.
The concentration of cellulose acetate is preferably 1~2g/L in the acetone soln of cellulose acetate described in step b, more preferably
For 2g/L.The solution can be by the way that cellulose acetate be dissolved in acetone, and ultrasound is to being completely dissolved to obtain.
The ultrasonic time is preferably 0.5~1h described in step b, more preferably 1h.The ultrasonic power is preferably 10
~30w, more preferably 20w.
The time of stirring reaction is preferably 1~2h described in step b, more preferably 1.5h.
Modified zeolite is obtained described in step b can remove acetone soln, the drying of residual by washing with water.More preferably 60
It is dried in DEG C baking oven.
The present invention also provides the coagulation sludge that above-mentioned recovery method is prepared, by the way that the obtained coagulation sludge is entered
Row dehydration, drain processing and obtain.
The obtained coagulation sludge can be applied to prepare in fertilizer.
Described fertilizer is phosphate fertilizer or potassium phosphorus organic composite fertilizer.
Recovery method of the present invention to livestock and poultry cultivation tail water particularly pig farm tail water deepen high treating effect, can efficient denitrification remove
Phosphorus and removal COD, while the coagulation sludge that recovery obtains can be used as nitrogen phosphorus organic composite fertilizer, realize recycling, and
And technique simple and stable, production cost is low, easily realizes large-scale application.
Recovery method of the present invention is uniformly distributed modified artificial by the way that hybrid metal solution to be added to contain with certain basicity
In the pig farm tail water of zeolite, coagulation can occur under the conditions of slow stir is stirred soon, a large amount of precipitation flcos are generated, by electrically neutralizing, sinking
Shallow lake net is caught to be acted on adsorption bridging, a large amount of pollutants can be reached into efficient removal by modes such as intermolecular force, chemical combination keys
The purpose of pollutant.The modified zeolite of the present invention has many microcellular structures, can largely adsorb the ammonia nitrogen in tail water.Coagulation process
In, the nutrient such as C, N, P in tail water is absorbed in coagulation sludge, coagulation sludge is had good fertility deterioration.
The present invention is had the following advantages and beneficial effect relative to prior art:
1st, recovery method of the present invention can realize the high-efficient denitrification and dephosphorization of pig farm tail water, while efficiently remove COD, make livestock and poultry
Breeding wastewater is to TP, COD and NH4 +- N discharge, which reaches, has been carried out the secondary standard for consulting on (ring does letter [2014] 335).
2nd, N, P nutrient in the recyclable pig farm tail water of the present invention, and be fixed in coagulation sludge, by reclaiming coagulation
Sludge can realize the recycling of sludge, as azophoska, compensate cost of water treatment.
3rd, for the present invention to pig farm tail water high treating effect, effect is effectively stable, and method is simple and easy, is easy to extensive
Popularization and application, processing cost is cheap, and recyclable coagulation sludge realizes recycling, realizes fixation and the release profit of nitrogen P elements
With.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of modified zeolite of the present invention, wherein, (a) unmodified artificial zeolite;(b) present invention is modified
Zeolite.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
The material being related in the following example can obtain from commercial channel.
Embodiment 1:
Artificial zeolite (being purchased from Chemical Reagent Co., Ltd., Sinopharm Group) is ground, crosses 200 mesh sieve.Take the artificial boilings of 20g
Stone is added in the NaCl solution that 2L concentration is 0.3mol/L, 100 DEG C of heating water bath 3h, centrifugation, is washed with deionized 3 times,
Dried at 60 DEG C.15g is taken to be added in the acetone soln that 1.5L has dissolved 3g cellulose acetates the artificial zeolite of processing, first
Ultrasonic 1h, 1.5h is stirred afterwards, centrifuge, be washed with deionized 3 times, dried at 60 DEG C, produce modified zeolite of the present invention.
The X-ray diffractogram of gained modified zeolite and unmodified artificial zeolite is as shown in figure 1, X-ray diffraction observable ore deposit
The crystal structure characteristic of thing material.As shown in figure 1, the X-ray diffractogram of modified zeolite and unmodified artificial zeolite is without obvious
Difference, show to utilize cellulose acetate modified artificial zeolite, do not change the crystal structure of artificial zeolite, cellulose acetate is in itself
X-ray diffraction signal is weaker, does not show the characteristic peak of correlation.X-ray diffraction understand, cellulose acetate be graft in it is artificial
The surface of zeolite, do not change the crystal structure of artificial zeolite, it is modified, it can effectively retain absorption effect of the artificial zeolite to ammonia nitrogen
Fruit.
Embodiment 2:
A kind of pig farm Tailwater Depth processing and resource recycling method, comprise the following steps:
(1) 12.10g FeCl accurately are weighed3·6H2O (0.045mol Fe) and 36.40g MgCl2·6H2O
(0.179mol Mg), while be dissolved in 1L distilled water, mixed salt solution is obtained after stirring and dissolving, and (now gained mixes
Salting liquid metal cation molar concentration Mg:Fe=4:1);
(2) modified zeolite that 2.00g embodiments 1 are prepared is weighed into 250mL pig farms tail water, is stirred under 225r/min
Mix 45min;
(3) obtained mixed salt solution is added in 7mL steps (1) into step (2) system, makes Mg, Fe mass dense
Spend [Mg2+]+[Fe3+]=70mg/L;
(4) Na is used2CO3The pH of pig farm tail water obtained by step (3) is adjusted to 7 by solution, turns 5min under the conditions of 150r/min,
Turn 30min under the conditions of 50r/min again, stand 30min, supernatant is drained, remaining coagulation sludge dewatering, drained.
Determine TN (total nitrogen), NO respectively to tail water before and after the processing3- N (nitrate nitrogen), NH4 +- N (ammonium nitrogen), TP are (total
Phosphorus), COD (chemical oxygen demand), turbidity, calculate clearance, the results are shown in Table 1.
The pig farm tail water of table 1 water quality index before and after the processing
Embodiment 3:
(1) 12.10g FeCl accurately are weighed3·6H2O (0.045mol Fe) and 27.30g MgCl2·6H2O
(0.134mol Mg), while be dissolved in 1L distilled water, mixed salt solution is obtained after stirring and dissolving, and (now gained mixes
Salting liquid metal cation molar concentration Mg:Fe=3:1);
(2) modified zeolite that 1.25g embodiments 1 are prepared is weighed into 250mL pig farms tail water, is stirred under 250r/min
Mix 30min;
(3) obtained mixed salt solution is added in 10mL steps (1) into step (2) system, makes Mg, Fe mass dense
Spend [Mg2+]+[Fe3+]=100mg/L;
(4) Na is used2CO3The pH of pig farm tail water obtained by step (3) is adjusted to 7 by solution, turns 2min under the conditions of 200r/min,
Turn 20min under the conditions of 100r/min again, stand 60min, supernatant is drained, remaining coagulation sludge dewatering, drained.
Element in tail water, the results are shown in Table 2 after detection process.
Water quality index after the pig farm tail water processing of table 2
Element | Carbon | Oxygen | Nitrogen | Phosphorus | Magnesium | Potassium | Iron | Silicon |
Wt% | 12.23 | 21.93 | 3.12 | 5.29 | 4.38 | 2.37 | 12.42 | 23.03 |
Understanding above, recovery method of the present invention can realize the high-efficient denitrification and dephosphorization of pig farm tail water particularly pig farm tail water,
COD is efficiently removed simultaneously, makes livestock breeding wastewater to TP, COD and NH4 +- N discharge, which reaches, to be had been carried out secondary consulting on (ring
Do letter [2014] 335) standard.And N, P nutrient in recovery pig farm tail water are fixed in coagulation sludge, pass through recovery
Coagulation sludge can realize the recycling of sludge, as azophoska, compensate cost of water treatment.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of pig farm tail water nitrogen and phosphorus element recovery method, it is characterised in that specifically include following steps:
(1) modified zeolite is added in tail water I, stirring, adds coagulant solution, be well mixed, obtain tail water II;
(2) pH to 7~8 of tail water II is adjusted, is stirred, is stood, separation of solid and liquid, tail water and coagulation sludge after being handled.
2. pig farm tail water nitrogen and phosphorus element recovery method according to claim 1, it is characterised in that:The modified zeolite
It is prepared by comprising the following steps method:
A. artificial zeolite is immersed in NaCl solution, heats, obtain artificial zeolite A;
B. artificial zeolite A is immersed in the acetone soln of cellulose acetate, ultrasound, stirring reaction, obtains modified zeolite.
3. pig farm tail water nitrogen and phosphorus element recovery method according to claim 2, it is characterised in that:Described in step a
Heat to react 1~5h at 80~120 DEG C;The concentration of NaCl solution used is 0.1~0.3mol/L in step a;Step
The concentration of cellulose acetate is 1~2g/L in the acetone soln of cellulose acetate described in rapid b;When ultrasonic described in step b
Between be 0.5~1h;The time of stirring reaction described in step b is 1~2h.
4. pig farm tail water nitrogen and phosphorus element recovery method according to claim 2, it is characterised in that:Described in step a
Heat to react 3h at 100 DEG C;The concentration of NaCl solution used is 0.3mol/L in step a;Acetic acid described in step b
The concentration of cellulose acetate is 2g/L in the acetone soln of cellulose;The ultrasonic time described in step b is 1h;Institute in step b
The time for stating stirring reaction is 1.5h.
5. pig farm tail water nitrogen and phosphorus element recovery method according to claim 1, it is characterised in that:Institute in step (1)
The dosage for stating modified zeolite is 5~10g/L tail water I;Stirring described in step (1) be stirring 30 under 200~250r/min~
60min;Coagulant solution described in step (1) is the mixed solution containing magnesium ion and iron ion.
6. pig farm tail water nitrogen and phosphorus element recovery method according to claim 1, it is characterised in that:Institute in step (1)
The mol ratio of magnesium ion and iron ion is 2 in the coagulant solution stated:1~4:1;Described coagulant solution by by molysite and
At least one of magnesium salts is added to the water dissolving and obtained;The dosage of the coagulant solution is with metal ion final concentration in tail water II
It is defined, is 50~100mg/L.
7. pig farm tail water nitrogen and phosphorus element recovery method according to claim 1, it is characterised in that:Institute in step (1)
The coagulant solution stated is by by FeCl3And MgCl2At least one of be added to the water dissolving and obtain.
8. pig farm tail water nitrogen and phosphorus element recovery method according to claim 1, it is characterised in that:Institute in step (2)
Stirring is stated as first quick stirring, then mix slowly;2~5min is first stirred under the conditions of 150~200r/min, then 50~
20~30min is stirred under the conditions of 100r/min;The time stood described in step (2) is 30min or more.
9. a kind of coagulation sludge, it is characterised in that the recovery method according to any one of claim 1~8 obtains.
10. application of the coagulation sludge in fertilizer is prepared described in claim 9.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110104828A (en) * | 2019-05-07 | 2019-08-09 | 沭阳利民畜禽无害化处理有限公司 | A kind of dead livestock and poultry harmless treatment waste water treatment process |
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US20090069181A1 (en) * | 2006-05-30 | 2009-03-12 | Solvay Sa | Product and Process for Treating Water Bodies, Sediments and Soils |
CN106995223A (en) * | 2017-04-07 | 2017-08-01 | 华南农业大学 | A kind of piggery wastewater advanced treating and resource recycling method |
CN107129000A (en) * | 2017-07-03 | 2017-09-05 | 吉林大学 | A kind of method that utilization artificial zeolite cellulose acetate composite removes ammonia nitrogen in super low concentration ammonia nitrogen waste water |
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2017
- 2017-09-06 CN CN201710796657.7A patent/CN107473444B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US20090069181A1 (en) * | 2006-05-30 | 2009-03-12 | Solvay Sa | Product and Process for Treating Water Bodies, Sediments and Soils |
CN106995223A (en) * | 2017-04-07 | 2017-08-01 | 华南农业大学 | A kind of piggery wastewater advanced treating and resource recycling method |
CN107129000A (en) * | 2017-07-03 | 2017-09-05 | 吉林大学 | A kind of method that utilization artificial zeolite cellulose acetate composite removes ammonia nitrogen in super low concentration ammonia nitrogen waste water |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110104828A (en) * | 2019-05-07 | 2019-08-09 | 沭阳利民畜禽无害化处理有限公司 | A kind of dead livestock and poultry harmless treatment waste water treatment process |
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