Nutrient extraction and recovery device for isolation and separation of target products from animal produced waste streams

Abstract

The present invention provides for nutrient extraction and recovery devices that use the Donnan Membrane Principle (DMP) to cause spontaneous separation of dissolved ions along electrochemical potential gradients, wherein anions and cations such as H.sub.2PO.sub.4.sup.−, HPO.sub.4.sup.2−, PO.sub.4.sup.3−, Mg.sup.2+, Ca.sup.2+, NH.sub.4.sup.+, and K.sup.+ are moved from manure containing waste streams through cation and anion exchange membranes into a recovery stream thereby precipitating target compounds including but not limited to struvite, potassium struvite and hydroxyapatite.

Claims

1. A system for processing a source of waste to produce at least one target product selected from the group consisting of struvite, potassium struvite, hydroxyapatite, and any combination thereof, the system comprising: a chamber-type device comprising at least one wall, a cation exchange membrane having a first side and a second side, and an anion exchange membrane having a first side and a second side, wherein the at least one wall, the first surface of the cation exchange membrane and the first surface of the anion exchange membrane define an interior of a recovery compartment for containing a recovery or draw solution, wherein the chamber-type device is communicatively connected to a gravimetric separator that permits collection of the at least one target product from the device, and recirculation of, the recovery or draw solution to the device, wherein, following insertion of the chamber-type device into the source of waste, the second surface of the cation exchange membrane and the second surface of the anion exchange membrane are in contact with the source of waste, wherein the recovery or draw solution comprises at least one cation and at least one anion, wherein the at least one cation is selected from the group consisting of Na.sup.+, K.sup.+, Mg.sup.2+, Ca.sup.2+, NH.sub.4.sup.+ and combinations thereof, and the at least one anion is selected from the group consisting of HPO.sub.4.sup.2−, PO.sub.4.sup.3−, Cl.sup.−, HO.sup.−, HCO.sub.3.sup.−, and HCOO.sup.− and combinations thereof, and wherein the at least one cation and at least one anion in the recovery or draw solution precipitate to form the at least one target product, and wherein the system does not require an electric current supply to produce the at least one target product.

2. The system of claim 1, wherein the system does not require a pressure gradient to produce the at least one target product.

3. The system of claim 1, wherein the waste source comprises at least one of manure, wastewater, waste activated sludge, and agricultural waste.

4. The system of claim 1, wherein the chamber-type device further comprises at least one outlet for accessing the compartment.

5. The system of claim 1, wherein the cation exchange membrane comprises a polymer containing anionic groups including sulfonic and/or carboxylic groups.

6. The system of claim 1, wherein the anion exchange membrane comprises a polymer containing quaternary or tertiary amine groups.

7. The system of claim 1, wherein the recovery or draw solution has a pH ranging from about 7 to 11.

8. The system of claim 1, wherein the chamber-type device is assembled into a manifold.

9. The system of claim 1, wherein the recovery or draw solution comprises sodium chloride.

10. A method of processing a source of waste to produce at least one target product selected from the group consisting of struvite, potassium struvite, hydroxyapatite, and any combination thereof, said method comprising introducing the system of claim 1 into a waste source, wherein the at least one cation and at least one anion in the recovery or draw solution precipitate to form the at least one target product, and collecting the at least one target product in the gravimetric separator.

11. The method of claim 10, wherein the waste source comprises at least one of manure, wastewater, waste activated sludge, and agricultural waste.

Description

BRIEF DESCRIPTION OF THE FIGURES

(1) FIG. 1 shows Simultaneous recovery of nutrient-rich solutions that can be used to precipitate struvite-based solids using a three-chamber design that incorporates both anion and cation exchange membranes. Note that the two waste chambers are one container, and the second compartment is essentially an insert containing an anion exchange membrane on one side, and a cation exchange membrane on the other. This setup ensures that changes to the chemistry of the first chamber are reflected in the third chamber. (a) initial conditions with waste compartments and a NaCl-based draw solution; (b) transport of anions and cations across the anion and cation exchange membranes, respectively; (c) equilibrium situation with selective recovery of PO.sub.4.sup.3− (as HPO.sub.4.sup.2− here), Mg.sup.2+, and NH.sub.4.sup.+, which precipitate to form struvite.

(2) FIG. 2 shows (a) phosphorus and (b) magnesium/ammonium recovery using the Donnan Membrane Principle with anion and cation exchange membranes. Note that solid particles and cations cannot cross the anion exchange membrane and anions cannot cross the cation exchange membrane and electroneutrality is maintained.

(3) FIG. 3 shows and illustration of the impact of the Donnan Membrane Principle for nutrient recovery.

(4) FIG. 4 shows a schematic representation of a chamber-type nutrient extraction and recovery device (NERD) wherein the recovery compartment is included in a waste compartment (not shown).

(5) FIG. 5 shows an alternative system for recovery of nutrients from waste material.

(6) FIG. 6 is a photograph of laboratory-scale DMP-based NERD reactor containing (left) poultry litter extract and (right) NaCl draw solution.

(7) FIG. 7 shows the recovery of >99% phosphorus from a synthetic wastewater using a NaCl draw solution.

(8) FIG. 8 shows the recovery of >99% phosphorus from synthetic wastewater using an NaOH-based draw solution.

(9) FIG. 9 shows data demonstrating the use of a regular precipitation scheme to maintain the electrochemical potential gradient for long-term phosphorus recovery.

(10) FIG. 10 shows SEM microphotographs of (a-b) struvite and (c-d) potassium struvite recovered from NERD reactors treating synthetic wastewater.

(11) FIG. 11 shows recovery of P(V) from a slurry containing 1 g/L of poultry litter using a draw solution of 10 g/L NaCl.

DETAILED DESCRIPTION OF THE INVENTION

(12) Nutrient extraction and recovery devices (NERDs) exploit the Donnan Membrane Principle (DMP) [1-4] to cause spontaneous separation of dissolved ions along electrochemical potential gradients. This innovative technology challenges conventional wisdom by taking a completely different approach to nutrient recovery. Given the high energy and chemical costs associated with traditional approaches, the present invention provides for a novel and effective extraction system.

(13) The invention takes advantage of the DMP for removal and recovery of P(V) (as HPO.sub.4.sup.2− here), Mg.sup.2+, Ca.sup.2+, NH.sub.4.sup.+, and K.sup.+ ions from waste sludge such as manure. The Donnan membrane principle is based on the Donnan co-ion exclusion phenomenon, according to which negatively charged cation exchange membranes will reject anions, while positively charged anion exchange membranes will reject cations. Unlike other membrane processes, the Donnan membrane principle does not require a pressure gradient or an electric current supply, and operates by virtue of the electrochemical potential difference between electrolytes on two sides of an ion exchange membrane.

(14) The term “manure” refers to any medium that includes animal waste and may also include but is not limited to water, feed, urine, fecal matter, straw, hay, bedding material, peat moss, and composts.

(15) The system and individual compartments may be fabricated from any material that does not interact with any ions in the waste or recovery streams, including but not limited to polymeric, metallic or ceramic material.

(16) In some embodiments, the cation exchange membranes, as disclosed herein, are conventional and are available from, for example, Asahi Kasei of Tokyo, Japan; or from Membranes International of Glen Rock, N.J., or DuPont, in the USA or SELEMION® by AGC Engineering Co., Ltd. Examples of cation exchange membranes include, but are not limited to, N2030WX (Dupont), F8020/F8080 (Flemion), FKE (Fuma Tech), CMI-7000 (Membranes International, Nafion 117 (Dupont) and F6801 (Aciplex). Cation exchange membranes that are desirable in the methods and systems of the invention have minimal resistance loss, greater than 90% selectivity, and high stability in concentrated caustic. Examples of cationic exchange membranes include, but not limited to, cationic membrane consisting of a polymer containing anionic groups, for example sulfonic and/or carboxylic groups. However, it may be appreciated that in some embodiments, depending on the need to restrict or allow migration of a specific cation or an anion species between the electrolytes, a cation exchange membrane that is more restrictive and thus allows migration of one species of cations while restricting the migration of another species of cations may be used.

(17) Anion exchange membranes allow passage of salt ion such as chloride ion to the waste stream. Preferably the anion exchange membrane is also substantially resistant to the organic compounds such that the anion exchange membranes does not interact with the organics. For example only, polymers containing fixed tertiary or quaternary ammonium groups may be used as anion exchange membranes. Similarly, depending on the need to restrict or allow migration of a specific anion species, an anion exchange membrane that is more restrictive and thus allows migration of one species of anions while restricting the migration of another species of anions may be used. Examples of anion exchange membranes include, but are not limited to, FAA-3 (Fuma Tech), AMI-7001 (Membranes International) and AMX (Astom).

(18) In some embodiments, the membranes used in the methods and systems provided herein are ion exchange membranes reinforced with a material for reinforcement and are of a certain thickness. For example, in some embodiments, the thickness of the membrane is between 20-130 um; or between 20-110 um; or between 20-110 um; or between 20-80 um; or between 20-75 um; or between 20-60 um; or between 20-50 um; or between 20-40 um; or between 20-35 um. In some embodiments, the membrane may be reinforced with materials such as, but not limited to, polymers, such as, polyethylene (PET), polypropylene (PP), and polyether ether ketone (PK), and glass fiber (GF).

(19) The present invention works by exploiting DMP, which drives electrochemical potential equilibrium between two solutions separated by an ion exchange membrane, to recover nutrients. In particular, a recovery or draw solution containing less preferred species (e.g., Cl.sup.−) facilitates exponential recovery of more preferred species, such as PO.sub.4.sup.3− and valuable cationic species (e.g., NH.sub.4.sup.+, Mg.sup.2+, Ca.sup.2+) can also be recovered. In tandem, the selectively separated nutrients facilitate recovery of value-added products, such as struvite, potassium struvite and hydroxyapatite.

(20) Phosphorus and other nutrients can be selectively extracted from animal manure and concentrated in high-purity solutions. The chemical conditions in the recovery solution cause precipitation of valuable fertilizers. The present system does not require chemical addition or electricity; furthermore, this technology can be directly incorporated into manure pits and lagoons.

(21) Current technologies rely on effective separation of nutrients before a forced chemical precipitation. For instance, previous researchers have used hybrid ion exchange resins and modified clay sorbents to effectively isolate phosphate (PO.sub.4.sup.3−) and/or ammonium (NH.sub.4.sup.+); following separation, nutrients are eluted from the sorbent media, mixed with MgCl.sub.2, and recovered as struvite [5-8]. The present invention does not require energy intensive processes or external chemical addition.

(22) The process works by exploiting electrochemical potential equilibrium between two solutions separated by an ion exchange membrane. For simplicity, the two chambers will be labeled as waste (that containing manure from animal, such as poultry) and recovery (the draw solution) as shown in FIG. 1. To highlight the fundamentals of the proposed process, consider FIG. 2a, which illustrates P(V) recovery. The waste chamber contains wastewater, waste activated sludge, or agricultural waste and the recovery chamber contains a draw solution composed of high-strength sodium chloride. While the process looks similar to an electrodialysis cell, no electricity is used here. Instead, the differences in electrochemical potential between the waste and draw solutions drives the system to thermodynamic equilibrium by exchanging ions.

(23) At equilibrium,
μ.sub.F(V).sup.waste=μ.sub.F(V).sup.recovery  (Eq. 1)
where, μ is the electrochemical potential, waste designates the chamber containing a poultry litter slurry, and recovery designates the chamber in which P(V) (i.e., the H.sub.3PO.sub.4, H.sub.2PO.sub.4.sup.−, HPO.sub.4.sup.2−, and PO.sub.4.sup.3− system) is recovered. Eq. 1 can be expanded to Eq. 2.
μ.sub.F(V).sup.o+RT ln a.sub.F.sup.waste+zFϕ.sup.waste=μ.sub.F(V).sup.o+RT ln a.sub.F(V).sup.recovery+zFϕ.sup.recovery  (Eq. 2)
In Eq. 2, μ.sup.o is the electrochemical potential at standard conditions, R is the gas constant, T is temperature, a is activity, z is the charge of the diffusing ion, F is the Faraday constant, and ϕ is the electrical potential. Rearranging Eq. 2 yields Eq. 3.

(24) $\begin{array}{cc}\frac{F\left({\varphi }^{\mathrm{waste}}-{\varphi }^{\mathrm{recovery}}\right)}{\mathrm{RT}}={\ln \left(\frac{a_{P\left(V\right)}^{\mathrm{recovery}}}{a_{P\left(V\right)}^{\mathrm{waste}}}\right)}^{\frac{1}{2_{P\left(V\right)}}}={\ln \left(\frac{a_{\mathrm{draw}}^{\mathrm{recovery}}}{a_{\mathrm{draw}}^{\mathrm{waste}}}\right)}^{\frac{1}{2_{\mathrm{draw}}}}& \left(\mathrm{Eq}.3\right)\end{array}$

(25) The second part of Eq. 3 is solved for a generic species, labeled draw here to refer to a draw ion present in the recovery solution. If the activity corrections for P(V) and the draw ion are similar on either side of the ion exchange membrane, Eq. 3 can be collapsed to Eq. 4, where C is molar concentration.

(26) $\begin{array}{cc}{\left(\frac{C_{P\left(V\right)}^{\mathrm{recovery}}}{C_{P\left(V\right)}^{\mathrm{waste}}}\right)}^{2_{\mathrm{draw}}}={\left(\frac{C_{\mathrm{draw}}^{\mathrm{recovery}}}{C_{\mathrm{draw}}^{\mathrm{waste}}}\right)}^{2_{P\left(V\right)}}& \left(\mathrm{Eq}.4\right)\end{array}$

(27) If HPO.sub.4.sup.2− is being exchanged with Cl.sup.− (or any other monovalent ion), then Eq. 5 describes the corresponding equilibrium ratios in the recovery and waste compartments.

(28) $\begin{array}{cc}\frac{{\left[{\mathrm{HPO}}_4^{2-}\right]}^{\mathrm{recovery}}}{{\left[{\mathrm{HPO}}_4^{2-}\right]}^{\mathrm{waste}}}={\left(\frac{{\left[{\mathrm{Cl}}^{-}\right]}^{\mathrm{recovery}}}{{\left[{\mathrm{Cl}}^{-}\right]}^{\mathrm{waste}}}\right)}^2& \left(\mathrm{Eq}.5\right)\end{array}$

(29) Therefore, by maintaining a molar ratio of [Cl.sup.−].sup.recovery to [Cl.sup.−].sup.waste of 10, the concentration of HPO.sub.4.sup.2− in the recovery side of the reactor should be approximately 100× that in the waste chamber. In practice, this means that 99% of phosphorus can be recovered into a “clean” solution. Since solids and cations cannot cross the anion exchange membrane, the recovery solution contains phosphorus, the draw ion (Cl.sup.− in this example), and the co-ion added with Cl.sup.− (e.g., Na.sup.+, if NaCl was used to generate the draw solution).

(30) A similar scheme using a cation exchange membrane can recover Mg.sup.2+, Ca.sup.2+, NH.sub.4.sup.+, and K.sup.+ (FIG. 2b). These cations are important for recovery of struvite, potassium struvite and hydroxyapatite solids. By maintaining a molar ratio of [Na.sup.+].sup.recovery to [Na.sup.+].sup.waste of 10, the Mg.sup.2+, Ca.sup.2+, NH.sub.4.sup.+, and K.sup.+ recovery efficiencies would be 99%, 99%, 90%, and 90%, respectively. Since dissolved NH.sub.4.sup.+ and K.sup.+ levels are typically greater than P(V) concentrations, the lower recovery of these species does not affect our ability to precipitate struvite-like minerals. The concentration effect observed during the Donnan Membrane Principle is illustrated in FIG. 3. These two streams, namely the P(V) and Mg—NH.sub.4—K rich solutions, can be mixed at the proper ratio to produce struvite or potassium struvite. The mixing ratio will be dependent on the total phosphorus concentration in the recovery solution from FIG. 2a and the magnesium and ammonium/potassium concentrations in the recovery solution from FIG. 2b. The dissolution reactions (Rxns. 1-2) and equilibrium constants (Eq. 7-8) for struvite and potassium struvite are shown below, respectively.
MgNH.sub.4PO.sub.4.6H.sub.2O(s)Mg.sup.2++NH.sub.4.sup.++PO.sub.4.sup.3−+6H.sub.2O  (Rxn. 1)
K.sub.sp.NH.sub.4.sub.MgPO.sub.4.sub..6H.sub.2.sub.O=10.sup.−18.8=[NH.sub.4.sup.+][Mg.sup.2+][PO.sub.4.sup.2−]  (Eq. 6)
MgKPO.sub.4.6H.sub.2O(s)Mg.sup.2++K.sup.++PO.sub.4.sup.3−+6H.sub.2O  (Rxn. 2)
K.sub.sp.KMgPO.sub.4.sub..6H2O=10.sup.−10.6=[K.sup.+][Mg.sup.2+][PO.sub.4.sup.8−]  (Eq. 7)

(31) The nutrient extraction technology of the present invention can be developed into a suite of commercial products aimed at providing on-site nutrient recovery. These products include chamber-, tubular-, and envelope-type systems. The chamber- and tubular-nutrient extraction devices of the present invention are expected to be most relevant to on site nutrient recovery from animal manure pits and lagoons. These devices can be easily assembled into a manifold that can be lowered into pits/lagoons and lifted for cleaning purposes. Operational units will involve a continuous flow of draw solution to allow collection of precipitated fertilizer products. In that case, nutrient extraction systems will contain a separate gravimetric separation that allows collection of solids and recirculation of bulk draw solutions.

(32) The chamber-type devices can be constructed of PVC piping. Cation (CM1-7000) and anion (AMI-7001) exchange membranes from Membranes International Inc. (Ringwood, N.J.) may be employed. Salient properties of the ion exchange membranes are provided in Table 1.

(33) TABLE-US-00001 TABLE 1 Salient information for the ion exchange membranes Parameter CMI-7000 AMI-7001 Functionality Strong Acid Strong base Polymer structure Gel polystyrene Gel polystyrene Cross-linking Divinylbenzene Divinylbenzene Functional group Sulfonic acid Quaternary ammonium Parent form Sodium Chloride Thickness (mm) 0.45 ± 0.25 0.45 ± 0.25 Capacity (meq/g) 1.6 ± 0.1 1.3 ± 0.1 Water permeability <3 <3 (mL/hr-ft.sup.2 at 5 psi) Chemical stability range (pH) 1-10 1-10

(34) A generalized schematic of the chamber-type passive sampling devices is provided in FIG. 4. The main section of the proposed device is a three-way-tee piece of PVC piping; this piping has one outlet on the z-axis and two outlets along the x-axis. The outlet on the z-axis is fitted with a male adaptor to allow for capping; therefore, this outlet represents the filling/emptying port for the device. The cap is fitted with a rubber septum to allow for easy sampling. The two side outlets (along the x-axis) are fitted with PVC flanges; corresponding pieces of PVC pipe are also fitted with PVC flanges. Cross-sections of cation and anion exchange membranes are fitted between these pieces as indicated in FIG. 4. Flanges may be secured using stainless steel screws, washers, and nuts.

(35) A prototype reactor with 2-L waste and recovery chambers separated by an anion exchange membrane (FIG. 6). For all preliminary experimentation, a AMI-7001 (Membranes International) was used which is a strong base anion exchange membrane consisting of a gel polystyrene polymer cross-linked with divinylbenzene and quaternary ammonium functional groups (total exchange capacity=1.3 meq/g). Preliminary experimentation was conducted for P(V) recovery from synthetic wastewater, wastewater effluent, and animal manure. The reactor body was constructed using clear polycarbonate, silicon frames (to prevent water leakage around the membrane), and stainless steel screws, washers, and nuts. The reactor chambers were continuously mixed using magnetic stirrers.

(36) Optimization of Nutrient Recovery Efficiency and Kinetics

(37) Results from an experiment with synthetic wastewater are shown in FIG. 7. The synthetic wastewater was comprised of 100 mg/L of Na.sub.2HPO.sub.4 (pH, 9.8; conductivity, 113 μS/cm), while the draw solution contained 10 g/L NaCl (pH, 6.22; conductivity, 18.1 mS/cm). Phosphorus in the waste compartment rapidly exchanged with chloride from the recovery compartment in the first eight hours of operation. After 24 hours, almost all of the phosphorus was recovered. For this scenario, the maximal chloride transfer is equivalent to two times the initial HPO.sub.4.sup.2− concentration. The corresponding chloride ratio in the waste/recovery chambers will be as high as 120 mol/mol. Then, the P(V) recovery will be as high as 99.99%.

(38) A similar experiment was run using a synthetic wastewater containing of 100 mg/L of Na.sub.2HPO.sub.4 (pH, 9.8; conductivity, 113 μS/cm), while the draw solution contained 100 mM NaOH (pH, 12.7; conductivity, 22.7 mS/cm). The P(V) recovery was >99%, as indicated in FIG. 8.

(39) Selective Recovery of Struvite-Based Minerals

(40) Using the reactor in FIG. 6, experiments were conducted to investigate the selective and continuous recovery of struvite minerals. FIG. 9 shows data from an experiment with a 100 mg/L Na.sub.3PO.sub.4 synthetic wastewater (pH, 10.4; conductivity, 135 μS/cm) with a 10 g/L NaCl draw solution (pH, 6.2; conductivity, 18.1 mS/cm). Over the first 24 hours of operation, P(V) was effectively recovered in the draw solution. At 24 hours, we dosed another 100 mg/L of Na.sub.3PO.sub.4 into the waste chamber and simultaneously added MgCl.sub.2 and NH.sub.4Cl into the recovery chamber in equimolar fashion to the recovered P(V). These treatments caused the P(V) concentration to increase in the waste compartment and decrease in the recovery chamber due to struvite precipitation. In combination, these changes also re-established the electrochemical potential gradient across the anion exchange membrane, resulting in continued recovery from 24 to 48 hours. At 48 hours, over 95% P(V) recovery was achieved.

(41) P(V) was recovered using draw solutions containing MgCl.sub.2 and NH.sub.4Cl or KCl. Because the Mg.sup.2+ and NH.sub.4.sup.+ or K.sup.+ were present in the recovery compartment in excess of P(V), the recovered phosphorus was driven towards precipitation as struvite or potassium struvite. Scanning electron microscopy (SEM) microphotographs of the recovered solids are shown in FIG. 10. The particles in FIG. 10 (a-b) were recovered using a draw solution with MgCl.sub.2/NH.sub.4Cl, whereas the images in FIG. 10 (c-d) stem from an experiment with a MgCl.sub.2/KCl draw solution. Note that energy-dispersive X-ray spectroscopy (EDS) analyses confirmed mineral composition. From the SEM images, the morphological differences between struvite and potassium struvite are clear, with “needle-like” struvite crystals and “flake-like” potassium struvite precipitates.

(42) Nutrient Recovery from Wastewater, Activated Sludge, & Animal Manure

(43) A study was conducted to recover phosphorus from a poultry litter slurry (FIG. 11). After 38 hours, over 70% of the P(V) was recovered. While the rate of recovery was slower than the synthetic solutions described above, the extent of recovery indicates that the overall recovery potential is still high. Furthermore, the AMI-7001 membranes that were used in this experiment were relatively thick, 450±25 μm. Notably the thickness of the ion exchange membranes may be thinner (i.e., 200 μm or less), and should provide faster recovery rates in real wastewaters.

REFERENCES

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