CN107473444B - Method for recovering nitrogen and phosphorus nutrient elements from pig farm tail water - Google Patents

Method for recovering nitrogen and phosphorus nutrient elements from pig farm tail water Download PDF

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CN107473444B
CN107473444B CN201710796657.7A CN201710796657A CN107473444B CN 107473444 B CN107473444 B CN 107473444B CN 201710796657 A CN201710796657 A CN 201710796657A CN 107473444 B CN107473444 B CN 107473444B
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tail water
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coagulated sludge
zeolite
water
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CN107473444A (en
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黄柱坚
黄芷嫣
崔理华
蔡丽苗
毛小云
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South China Agricultural University
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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 the technical field of tail water resource utilization, and discloses a method for recovering nitrogen and phosphorus nutrient elements from a pig farm tail water. The recovery method specifically comprises the following steps: (1) adding the modified zeolite into the tail water I, stirring, adding a coagulant solution, and uniformly mixing to obtain tail water II; (2) and adjusting the pH value of the tail water II to 7-8, stirring, standing, and carrying out solid-liquid separation to obtain the treated tail water and the coagulated sludge. The recycling method has good effect of deeply treating the livestock and poultry breeding tail water, particularly the pig farm tail water, can efficiently remove nitrogen and phosphorus and COD, simultaneously can recycle the obtained coagulated sludge as a nitrogen-phosphorus organic compound fertilizer to realize resource utilization, has simple and stable process and low production cost, and is easy to realize large-scale application. The invention also provides the coagulated sludge prepared by the recovery method, which is obtained by dewatering and draining the obtained coagulated sludge. The obtained coagulated sludge can be applied to the preparation of fertilizer.

Description

Method for recovering nitrogen and phosphorus nutrient elements from pig farm tail water
Technical Field
The invention belongs to the technical field of tail water resource utilization, and particularly relates to recovery of nitrogen and phosphorus nutrient elements in tail water of a pig farm.
Background
The pig farm tail water is rich in nitrogen, phosphorus and other elements which cause the lake to be rich in nutritionThe important reasons for the large-scale outbreak of cyanobacterial bloom. Wherein the composition of the pig farm tail water is complex, COD, TP and NH4 +high-N concentration, high treatment difficulty and high cost, and can cause a series of serious water environment problems due to incomplete treatment. The national ministry of environmental protection has implemented secondary solicitation opinions on livestock and poultry breeding wastewater discharge standards (environmental letter [ 2014)]335) in which TP, COD and NH are added4 +The emission standards of-N are respectively upgraded from 8.0mg/L, 400mg/L and 80mg/L of the original (GB 18596-2001) to 5.0mg/L, 150mg/L and 40mg/L, and the emission standards after upgrading are difficult to reach in the conventional pig farm treatment. Meanwhile, a large amount of sludge is generated in the conventional pig farm tail water treatment, and the subsequent treatment of the sludge also becomes a difficult problem. However, the phosphorus and nitrogen containing substances contained in the tail water are essential nutrient elements for the growth of crops, the phosphorus and nitrogen containing substances in the pig farm tail water are effectively solidified, the prior art is mainly a MAP struvite process, however, the MAP struvite process has strict application conditions, such as a certain nitrogen-phosphorus ratio, a narrow pH range and the like, and has certain difficulty in operation. Therefore, there is a need to develop a more efficient and easy to manage technical method.
In the prior art, modification research is carried out on zeolite, but the prior zeolite and artificial zeolite have good ammonia nitrogen removal effect, but the removal of water quality indexes such as total phosphorus, COD (chemical oxygen demand) and the like is not satisfactory. In the prior art, cellulose is not grafted on artificial zeolite and is applied to the deepening treatment of the tail water of a pig farm.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a method for recovering nitrogen and phosphorus nutrient elements from the tail water of a pig farm. The piggery tail water treated by the method can reach COD and NH which are subjected to secondary solicitation on the discharge standard of the livestock and poultry breeding tail water by the national ministry of environmental protection4 +-N, TP and other water quality index standards. The coagulated sludge obtained after the treatment by the method can realize resource utilization, and the nutrient substances in the tail water are solidified, so that the tail water is deeply treated, the nutrient substances are recycled, and the water treatment cost is compensated.
The invention further aims to provide the coagulated sludge obtained by the recovery method.
The purpose of the invention is realized by the following scheme:
a method for recovering nitrogen and phosphorus nutrient elements from pig farm tail water specifically comprises the following steps:
(1) adding the modified zeolite into the tail water I, stirring, adding a coagulant solution, and uniformly mixing to obtain tail water II;
(2) and adjusting the pH value of the tail water II to 7-8, stirring, standing, and carrying out solid-liquid separation to obtain the treated tail water and the coagulated sludge.
The amount of the modified zeolite used in the step (1) is 5-10 g/L of tail water I.
The stirring in the step (1) is preferably performed for 30-60 min at 200-250 r/min.
The coagulant solution in the step (1) is a mixed solution containing magnesium ions and iron ions.
The molar ratio of magnesium ions to iron ions in the coagulant solution is preferably 2: 1-4: 1.
The coagulant solution can be obtained by adding at least one of ferric salt and magnesium salt into water for dissolving; preferably at least one of a soluble iron salt and a soluble magnesium salt; more preferably FeCl3And MgCl2At least one of (1).
The dosage of the coagulant solution is based on the final concentration of metal ions in the tail water II, and preferably is 50-100 mg/L. I.e. [ Mg ]2+]+[Fe3+]＝50～100mg/L。
The adjustment of the pH in step (2) is preferably carried out by adding sodium carbonate.
In the step (2), the stirring is firstly carried out at a high speed, and then is carried out at a low speed; preferably, the mixture is stirred for 2-5 min under the condition of 150-200 r/min and then stirred for 20-30 min under the condition of 50-100 r/min.
The standing time in the step (2) is preferably 30min or more, and more preferably 30-60 min.
The modified zeolite is prepared by the method comprising the following steps:
a. immersing artificial zeolite into a NaCl solution, and heating to obtain artificial zeolite A;
b. and (3) immersing the artificial zeolite A into an acetone solution of cellulose acetate, and performing ultrasonic and stirring reaction to obtain the modified zeolite.
The heating treatment in the step a is preferably carried out for 1-5 h at 80-120 ℃, and more preferably for 3h at 100 ℃. The heating is preferably water bath heating.
The heat-treated zeolite is preferably washed with water to remove residual NaCl, dried and used in the next reaction.
The concentration of the NaCl solution used in the step a is 0.1-0.3 mol/L, and more preferably 0.3 mol/L.
The artificial zeolite used in step a may be a commercially available artificial zeolite, and is preferably sieved with a 200-mesh sieve before use.
The concentration of the cellulose acetate in the acetone solution of the cellulose acetate in the step b is preferably 1-2 g/L, and more preferably 2 g/L. The solution can be obtained by dissolving cellulose acetate in acetone and sonicating until completely dissolved.
The time of the ultrasonic treatment in the step b is preferably 0.5-1 h, and more preferably 1 h. The power of the ultrasonic wave is preferably 10-30 w, and more preferably 20 w.
The stirring reaction time in the step b is preferably 1-2 h, and more preferably 1.5 h.
The modified zeolite obtained in step b can be washed with water to remove residual acetone solution and dried. More preferably in an oven at 60 ℃.
The invention also provides the coagulated sludge prepared by the recovery method, which is obtained by dewatering and draining the obtained coagulated sludge.
The obtained coagulated sludge can be applied to the preparation of fertilizer.
The fertilizer is phosphate fertilizer or potassium-phosphorus organic compound fertilizer.
The recycling method has good effect of deeply treating the livestock and poultry breeding tail water, particularly the pig farm tail water, can efficiently remove nitrogen and phosphorus and COD, simultaneously can recycle the obtained coagulated sludge as a nitrogen-phosphorus organic compound fertilizer to realize resource utilization, has simple and stable process and low production cost, and is easy to realize large-scale application.
The recovery method of the invention adds the mixed metal solution into the pig farm tail water with certain alkalinity and evenly distributed modified artificial zeolite, coagulation can occur under the condition of fast stirring and slow stirring to generate a large amount of precipitation flocs, and the purpose of efficiently removing pollutants can be achieved by the modes of intermolecular force, chemical bonding and the like through the actions of electrical neutralization, precipitation net capturing and adsorption bridging. The modified zeolite has a plurality of microporous structures and can adsorb a large amount of ammonia nitrogen in the tail water. In the coagulation process, C, N, P and other nutrient elements in the tail water are absorbed into the coagulated sludge, so that the coagulated sludge has a good fertility effect.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the recovery method can realize the high-efficiency nitrogen and phosphorus removal of the pig farm tail water and the high-efficiency removal of COD at the same time, so that the livestock and poultry breeding wastewater can carry out TP, COD and NH treatment on the wastewater4 +Emission of-N reaches implemented Secondary solicitation (Do letter [ 2014)]335) of the same standard.
2. The invention can recover N, P nutrient elements in the pig farm tail water and fix the nutrient elements in the coagulated sludge, can realize resource utilization of the sludge by recovering the coagulated sludge, and can be used as nitrogen, phosphorus and potassium fertilizers to compensate the water treatment cost.
3. The method has the advantages of good treatment effect on the pig farm tail water, effective and stable effect, simplicity and feasibility, convenience for large-scale popularization and application, low treatment cost, capability of recycling coagulated sludge to realize resource utilization and fixation and release utilization of nitrogen and phosphorus elements.
Drawings
FIG. 1 is an X-ray diffraction pattern of a modified zeolite of this invention wherein (a) is an unmodified artificial zeolite; (b) the modified zeolite of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The materials referred to in the following examples are commercially available.
Example 1:
artificial zeolite (available from national pharmaceutical group chemical Co., Ltd.) was ground and sieved through a 200 mesh sieve. Adding 20g of artificial zeolite into 2L of NaCl solution with the concentration of 0.3mol/L, heating in a water bath at 100 ℃ for 3h, centrifuging, washing with deionized water for 3 times, and drying at 60 ℃. Adding 15g of the treated artificial zeolite into 1.5L of acetone solution in which 3g of cellulose acetate is dissolved, firstly carrying out ultrasonic treatment for 1h, then stirring for 1.5h, centrifuging, washing for 3 times by using deionized water, and drying at 60 ℃ to obtain the modified zeolite.
The resulting modified zeolite and unmodified artificial zeolite have X-ray diffraction patterns as shown in FIG. 1, and the crystal structure characteristics of the mineral material can be observed by X-ray diffraction. As shown in fig. 1, the X-ray diffraction patterns of the modified zeolite and the unmodified artificial zeolite are not significantly different, which indicates that the crystal structure of the artificial zeolite is not changed by using the cellulose acetate modified artificial zeolite, and the X-ray diffraction signal of the cellulose acetate is weaker and does not show related characteristic peaks. According to X-ray diffraction, the cellulose acetate is grafted on the surface of the artificial zeolite, the crystal structure of the artificial zeolite is not changed, and the adsorption effect of the artificial zeolite on ammonia nitrogen can be effectively reserved after modification.
Example 2:
a pig farm tail water deep treatment and resource recycling method comprises the following steps:
(1) accurately weighing 12.10g FeCl3·6H2O (0.045mol Fe) and 36.40g MgCl2·6H2Dissolving O (0.179mol Mg) in 1L of distilled water, and stirring to obtain a mixed metal salt solution (the molar concentration of metal cations Mg: Fe is 4:1 in the mixed salt solution);
(2) weighing 2.00g of the modified zeolite prepared in example 1 into 250mL of pig farm tailwater, and stirring for 45min at 225 r/min;
(3) adding 7mL of mixed metal salt solution obtained in the step (1) into the system in the step (2) to ensure that the mass concentration of Mg and Fe [ Mg2+]+[Fe3+]＝70mg/L；
(4) With Na2CO3Adjusting the pH value of the pig farm tail water obtained in the step (3) to 7 by using the solution at 150r/minRotating for 5min under the condition of 50r/min, rotating for 30min under the condition of 50r/min, standing for 30min, discharging supernatant, and dehydrating and draining the remaining coagulated sludge.
Separately measuring TN (total Nitrogen) and NO in the tail water before and after the treatment3N (nitrate nitrogen), NH4 +N (ammonium nitrogen), TP (total phosphorus), COD (chemical oxygen demand), turbidity, calculated removal rate, results are shown in Table 1.
TABLE 1 Water quality index before and after treatment of the pig farm tailwater
Figure BDA0001400511570000051
Example 3:
(1) accurately weighing 12.10g FeCl3·6H2O (0.045mol Fe) and 27.30g MgCl2·6H2Dissolving O (0.134mol of Mg) in 1L of distilled water, and stirring to obtain a mixed metal salt solution (the molar concentration of metal cations Mg: Fe is 3:1 in the mixed salt solution);
(2) weighing 1.25g of the modified zeolite prepared in example 1 into 250mL of pig farm tail water, and stirring for 30min at the speed of 250 r/min;
(3) adding 10mL of mixed metal salt solution obtained in the step (1) into the system in the step (2) to ensure that the mass concentration of Mg and Fe [ Mg2+]+[Fe3+]＝100mg/L；
(4) With Na2CO3And (3) adjusting the pH value of the pig farm tail water obtained in the step (3) to 7 by using the solution, rotating for 2min at 200r/min, rotating for 20min at 100r/min, standing for 60min, discharging supernatant, and dehydrating and draining the remaining coagulated sludge.
The elements in the treated tail water were detected, and the results are shown in Table 2.
TABLE 2 Water quality index after treatment of the pig farm tailwater
Element(s) Carbon (C) Oxygen gas Nitrogen is present in Phosphorus (P) Magnesium alloy Potassium salt Iron Silicon
wt％ 12.23 21.93 3.12 5.29 4.38 2.37 12.42 23.03
As can be seen from the above, the recovery method of the invention can realize the high-efficiency nitrogen and phosphorus removal of the pig farm tail water, particularly the pig farm tail water, and simultaneously remove COD efficiently, so that the livestock and poultry breeding wastewater can carry out TP, COD and NH treatment on the wastewater4 +Emission of-N reaches implemented Secondary solicitation (Do letter [ 2014)]335) of the same standard. And N, P nutrient elements in the recovered pig farm tail water are fixed in the coagulated sludge, and the sludge can be recycled by recovering the coagulated sludge and used as nitrogen, phosphorus and potassium fertilizers to compensate the water treatment cost.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (3)

1. A method for recovering nitrogen and phosphorus nutrient elements from pig farm tail water is characterized by comprising the following steps:
(1) adding the modified zeolite into the tail water I, stirring, adding a coagulant solution, and uniformly mixing to obtain tail water II;
(2) adjusting the pH value of the tail water II to 7-8, stirring, standing, and carrying out solid-liquid separation to obtain treated tail water and coagulated sludge;
the modified zeolite in the step (1) is used in an amount of 5-10 g/L of tail water I, stirred for 30-60 min at a speed of 200-250 r/min, the molar ratio of magnesium ions to iron ions in a coagulant solution is 2: 1-4: 1, and iron salt and magnesium salt are added into water to be dissolved to obtain the modified zeolite; the dosage of the coagulant solution is based on the final concentration of metal ions in tail water II and is [ Mg2+]+[Fe3+]=50～100mg/L；
In the step (2), the stirring is firstly carried out at a high speed, and then is carried out at a low speed; firstly stirring for 2-5 min under the condition of 150-200 r/min, then stirring for 20-30 min under the condition of 50-100 r/min, and standing for more than 30 min;
the modified zeolite is prepared by the following steps:
a. soaking the artificial zeolite into NaCl solution with the concentration of 0.3mol/L, and reacting for 3 hours at 100 ℃ to obtain artificial zeolite A;
b. immersing the artificial zeolite A into an acetone solution with the concentration of cellulose acetate of 2g/L, performing ultrasonic treatment for 1h, and stirring for reaction for 1.5h to obtain modified zeolite; and (c) washing the obtained modified zeolite in the step b with water to remove residual acetone solution, and drying, wherein the amount of the added zeolite is 10g per 1L of cellulose acetate acetone solution.
2. A coagulated sludge characterized by being obtained by the recovery method according to claim 1.
3. Use of the coagulated sludge of claim 2 in the preparation of a fertilizer.
CN201710796657.7A 2017-09-06 2017-09-06 Method for recovering nitrogen and phosphorus nutrient elements from pig farm tail water Active CN107473444B (en)

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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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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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