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WO2018150690A1 - Procédé et système de traitement d'eau - Google Patents

Procédé et système de traitement d'eau Download PDF

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Publication number
WO2018150690A1
WO2018150690A1 PCT/JP2017/043819 JP2017043819W WO2018150690A1 WO 2018150690 A1 WO2018150690 A1 WO 2018150690A1 JP 2017043819 W JP2017043819 W JP 2017043819W WO 2018150690 A1 WO2018150690 A1 WO 2018150690A1
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WIPO (PCT)
Prior art keywords
membrane
temperature
forward osmosis
solution
draw
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Ceased
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PCT/JP2017/043819
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English (en)
Japanese (ja)
Inventor
秀人 松山
智輝 高橋
英治 神尾
政宏 安川
熊野　淳夫
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kobe University NUC
Toyobo Co Ltd
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Kobe University NUC
Toyobo Co Ltd
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Priority to JP2018568008A priority Critical patent/JP7117718B2/ja
Publication of WO2018150690A1 publication Critical patent/WO2018150690A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/58—Multistep processes
    • 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
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis

Definitions

  • the present invention relates to a water treatment method and a water treatment system.
  • the forward osmosis (FO) phenomenon is a phenomenon in which a solvent (such as water) on a low concentration side moves toward a solution on a high concentration side.
  • Patent Document 1 Japanese Patent Publication No. 2014-512951 discloses a water treatment method including a forward osmosis treatment using a draw solute whose solubility is reduced by heating (temperature increase).
  • a draw solute lower critical solution temperature (LCST) type draw solute
  • LCST lower critical solution temperature
  • the draw solution can be separated from the low concentration fraction (low concentration draw solution) by increasing the temperature.
  • concentration fraction high-concentration draw solution
  • the diluted draw solution is phase-separated into a low-concentration draw solution and a high-concentration draw solution in the separation tank 3 by heating or the like by forward osmosis treatment in the forward osmosis module 1.
  • the separation membrane module 2 performs membrane separation treatment on the low-concentration draw solution, thereby recovering water (separating the draw solute).
  • the thermal energy for raising the temperature of a draw solution is required, the influence on the cost side by consumption of a thermal energy is comparatively small by utilizing the waste heat of other facilities.
  • the low concentration draw solution often contains several to several tens of mass% draw solute.
  • membrane separation is required.
  • a high pressure needs to be applied, and a lot of energy for pressurization is required.
  • the energy efficiency of water treatment could not be sufficiently improved, and it was difficult to sufficiently reduce the cost of water treatment.
  • an object of the present invention is to provide a water treatment method and a water treatment system that can separate a draw solute from a draw solution with low energy and can further increase the energy efficiency of water treatment.
  • the present invention it is possible to provide a water treatment method and a water treatment system that can separate a draw solute from a draw solution with low energy and can further increase the energy efficiency of water treatment.
  • the water treatment method of the present invention is a method for separating water from a target solution (liquid containing water and components other than water).
  • a target solution liquid containing water and components other than water.
  • the target solution include seawater, river water, lake water, industrial wastewater, and the like.
  • the water treatment method of the present invention includes at least a forward osmosis step, a phase separation step, and a membrane separation step described below.
  • the forward osmosis membrane is not particularly limited, and various membranes that can be used for forward osmosis can be used.
  • the semipermeable membrane examples include a reverse osmosis membrane (RO membrane: Reverse Osmosis Membrane), a forward osmosis membrane (FO membrane: Forward Osmosis Membrane), a nanofiltration membrane (NF membrane: Nanofiltration Membrane), and an ultrafiltration membrane (UF membrane). : Semipermeable membrane called Ultrafiltration Membrane).
  • the semipermeable membrane is preferably a reverse osmosis membrane, a forward osmosis membrane, or a nanofiltration membrane.
  • the pressure of the target solution in the first chamber is preferably 0.01 to 10 MPa.
  • the pore size of the RO membrane and the FO membrane is about 2 nm or less, and the pore size of the UF membrane is about 2 to 100 nm.
  • the NF membrane has a relatively low blocking rate of ions and salts among the RO membrane, and the pore size of the NF membrane is usually about 1 to 2 nm.
  • the salt removal rate of the RO membrane, FO membrane, or NF membrane is preferably 90% or more.
  • the material constituting the semipermeable membrane is not particularly limited, and examples thereof include cellulose resins, polysulfone resins, and polyamide resins.
  • the semipermeable membrane is preferably composed of a material containing at least one of a cellulose resin and a polysulfone resin.
  • the cellulose resin is preferably a cellulose acetate resin.
  • Cellulose acetate resin is resistant to chlorine, which is a bactericidal agent, and has a feature that it can suppress the growth of microorganisms.
  • the cellulose acetate resin is preferably cellulose acetate, and more preferably cellulose triacetate from the viewpoint of durability.
  • Examples of the cellulose semipermeable membrane include CTA (manufactured by Toyobo Co., Ltd.).
  • the polysulfone resin is preferably a polyethersulfone resin.
  • the polyethersulfone resin is preferably a sulfonated polyethersulfone.
  • the shape of the semipermeable membrane is not particularly limited, and examples thereof include a flat membrane, a spiral membrane, and a hollow fiber membrane.
  • Hollow fiber membranes are smaller in thickness than spiral type semipermeable membranes, and can increase the membrane area per module and increase the penetration efficiency. It is advantageous.
  • the draw solute used in the present invention is not particularly limited as long as the solubility of the draw solute decreases with increasing temperature. Note that such a decrease in solubility is reversible, and conversely, if the temperature decreases, it is preferable that the solubility increase.
  • Examples of such draw solutes include LCST (lower critical solution temperature) type phase change materials.
  • LCST lower critical solution temperature
  • an aqueous solution containing an LCST type phase change substance causes dehydration of a solute as the solution temperature rises, and causes a temperature phase transition (liquid-liquid phase separation) due to aggregation of solute molecules.
  • the polymolecular association is formed even in the temperature range below the phase transition temperature (homogeneous phase range below the LCST curve)
  • the osmotic pressure of the solution decreases due to the temperature rise even in the temperature range below the phase transition temperature. It is done.
  • LCST type phase change material examples include LCST type temperature responsive polymers.
  • LCST type temperature-responsive polymer dissolves in water at a relatively low temperature, and when the temperature exceeds a predetermined temperature (specific lower critical solution temperature: LCST), a dilute phase (low concentration draw solution) and a concentrated phase Phase separation into (high concentration draw solution).
  • the LCST type temperature-responsive polymer preferably has at least one hydrophilic group in at least some or all of the structural units (monomer units). Moreover, the temperature-responsive polymer may have a hydrophobic group in some structural units while having a hydrophilic group. In addition, it is considered that the balance between the hydrophilic group and the hydrophobic group contained in the molecule is important for the temperature responsive polymer to have temperature responsiveness.
  • hydrophilic group examples include a hydroxyl group, a carboxyl group, an acetyl group, an aldehyde group, an ether bond, and an ester bond.
  • Specific temperature-responsive polymers include, for example, polyvinyl ether polymers, polyvinyl acetate polymers, (meth) acrylic acid polymers, and the like.
  • polyvinyl ether polymer examples include polymethyl vinyl ether, vinyl ether having an oxyethylene chain, and polyhydroxybutyl vinyl ether.
  • polyvinyl ether polymers include the polymers shown in Table 1.
  • phase transition temperature shown in Table 1 is a lower critical solution temperature (LCST) in aqueous solution.
  • References 1 to 4 listed in Table 1 are as follows. Reference 1: Journal of Japan Rubber Association, Vol. 63, No. 1, 29-39 (1990). Reference 2: Journal of Polymer Science Part A: polymer Chemistry Vol. 30, 2407-2413 (1992). Reference 3: Journal of Polymer Science Part A: polymer Chemistry Vol. 41, 3300-3312 (2003). Reference 4: Macromolecules, 36, 8312-8319 (2003).
  • polyvinyl acetate polymer examples include polyvinyl acetate part saponified products.
  • Examples of the (meth) acrylic acid polymer include poly (meth) acrylate having an oxyethylene chain, (meth) acrylic acid copolymer, and the like.
  • LCST type temperature-responsive polymers examples include polypropylene glycol (PPG), for example.
  • PPG polypropylene glycol
  • FIGS. 3 and 4 The phase separation characteristics and osmotic pressure characteristics of PPG (molecular weight 400, diol type) are shown in FIGS. 3 and 4, respectively.
  • FIG. 3 shows that PPG phase-separates into a low concentration phase of about 15% by mass and a high concentration phase of about 80% by mass in an aqueous solution at about 70 ° C., for example.
  • FIG. 4 shows that the osmotic pressure of PPG decreases as the temperature increases.
  • FIG. 9 shows a case where the temperature-responsive draw solution is a 20% by mass polypropylene glycol (molecular weight 400, PPG400) solution, and the values of the water permeability flux are different when reverse osmosis treatment is performed by applying pressure to the draw solution side.
  • the temperature is shown (25 ° C. and 60 ° C.).
  • the applied pressure at which the water permeation amount becomes 0 is 19 bar when the temperature is 25 ° C. and 11 bar when the temperature is 60 ° C., and the concentration of the draw solution is the same. Nevertheless, the pressure at which the amount of water permeation becomes zero decreases due to an increase in temperature.
  • the osmotic pressure of PPG 400 varies with temperature.
  • the permeability flux obtained at a pressure of 25 bar is about 2 L / (m 2 ⁇ H), which corresponds to the permeability flux obtained at a pressure of about 12 bar at 60 ° C. This shows that the applied pressure at which the same permeable flux can be obtained can be greatly reduced.
  • LCST type temperature-responsive polymer products examples include Pluronic (manufactured by BASF), which is a block copolymer of polyoxypropylene and polyoxyethylene.
  • LCST type phase transition materials other than LCST type temperature responsive polymers include LCST type ionic liquid, glycol ether type LCST type phase change material, acid amide type LCST type phase change material, and amine type LCST type. Examples include phase change substances.
  • LCST type ionic liquid for example, Tetrabutylammonium-2,4,6-trimethylbenzenesulfonate (N 4444 -TMBS), Tetrabutylammonium -trifluoroacetate (N 4444 -CF 3 COO), Tetrabutylphosphonium-2,4,6-trimethylbenzenesulfonate (P 4444 -TMBS), Tetrabutylphosphonium-trifluoroacetate (P 4444 -CF 3 COO) Etc.
  • N 4444 -TMBS Tetrabutylammonium-2,4,6-trimethylbenzenesulfonate
  • N 4444 -CF 3 COO Tetrabutylammonium -trifluoroacetate
  • P 4444 -TMBS Tetrabutylphosphonium-2,4,6-trimethylbenzenesulfonate
  • P 4444 -CF 3 COO Tetrabutylphosphonium-trifluoroacetate
  • glycol ether type LCST type phase transition materials include: Diethylene glycol hexyl ether, Propylene glycol butyl ether, Dipropylene glycol propyl ether, Ethylene glycol n-butyl ether, Ethylene glycol n-pentyl ether, Diethylene glycol n-pentyl ether, Ethylene glycol 2-methyl-1-butyl ether, Diethylene glycol 2-methyl-1-butyl ether, Ethylene glycol n-hexyl ether, Triethylene glycol n-hexyl ether, Ethylene glycol n-heptyl ether, Diethylene glycol n-heptyl ether, Triethylene glycol n-heptyl ether, Propylene glycol n-propyl ether, Tripropylene glycol n-propyl ether, Dipropylene glycol n-butyl ether, And tripropylene glycol n-but
  • acid amide LCST type phase transition materials include: N, N-bis (2-butyramidoethyl) butyramide (nBu-DETA) N- (2- (Diethylamino) ethyl) pentanamide (Val-DEEA) N- (2- (Diethylamino) ethyl) isobutyramide (iBu-DEEA) N, N ′-((Methylazanediyl) bis (propane-3,1-diyl)) dibutyramide (nBu-DAPMA) N, N ′-((Methylazanediyl) bis (propane-3,1-diyl)) dipentanamide (Val-DAPMA) N-Butylpropionamide (N-BPA) N- (2- (diisopropylamino) ethyl) butyramide (nBu-DIPA) N-Butylated polyethyleneimine (nBu-
  • amine-based LCST type phase change materials include: Triethylamine, N-ethylpiperidine, 2-methylpiperidine, N-methylpiperidine and the like.
  • N 4444 -TMBS ([N 4444 ] [TMBS]) is, for example, in an aqueous solution at about 70 ° C., a low concentration phase of about 12% by mass, a high concentration phase of about 65% by mass, Are shown to phase separate.
  • FIG. 6 shows that N 4444 -TMBS has a lower osmotic pressure as the temperature is higher.
  • the osmotic pressure of the low-concentration phase (about 12% by mass) phase-separated at 70 ° C. is about 4.6 bar at room temperature (25 ° C.) from FIG. is there.
  • the present inventors constructed a method for measuring the actual osmotic pressure of the above-mentioned draw solute (LCST type phase change material), and from the measurement result, the osmotic pressure of the aqueous solution (draw solution) decreased due to temperature rise. I found out. The reason why the osmotic pressure of the aqueous solution (draw solution) decreases due to the temperature rise is estimated as follows.
  • the draw solute (DS) used in the present invention is solvated (hydrated) in a solvent (water) at a low temperature.
  • a solvent water
  • the interaction between DS molecules works relatively strongly compared to the interaction between solvent molecules (water molecules) and DS molecules. Molecules are thought to form aggregates (aggregates).
  • the osmotic pressure ⁇ [bar] of the ideal solution is the solute molar concentration c [mol ⁇ L ⁇ 1 ] and the gas constant R [bar ⁇ L ⁇ K ⁇ 1]. -Proportional to mol -1 ] and absolute temperature T [K]. Since the solute molar concentration is the molar molar concentration of all solute particles, the calculated solute molar concentration decreases when an association of solute particles occurs. For this reason, it is thought that the osmotic pressure of a solution falls by formation of an aggregate.
  • the osmotic pressure of the draw solution (after raising the temperature) used for the membrane separation step is preferably 0.01 to 2 MPa, more preferably 0.01 to 1 MPa.
  • a target solution (FS: feed solution) is caused to flow into a first chamber 11 provided in contact with one surface of the forward osmosis membrane 10, and the target solution is supplied to one side of the forward osmosis membrane 10. Touch the surface.
  • a draw solution (DS) containing a draw solute is caused to flow into the second chamber 12 provided in contact with the other surface of the forward osmosis membrane 10, and the draw solution is introduced into the other surface of the forward osmosis membrane 10.
  • phase separation process In the phase separation step, after the forward osmosis step, the temperature of the draw solution is increased to separate the draw solution into a low concentration draw solution and a high concentration draw solution (phase separation).
  • the temperature after the rise of the draw solution in the phase separation step is preferably 40 ° C. or higher and 90 ° C. or lower, more preferably 40 ° C. or higher and 85 ° C. or lower, and further preferably 40 ° C. or higher and 80 ° C. or lower.
  • the draw solution containing water in the target solution is allowed to flow into the separation tank 3 where the temperature of the draw solution is raised to separate the dilute phase (low concentration draw solution) and the concentrated phase (high concentration draw solution).
  • the draw solute contains an LCST-type temperature-responsive polymer
  • the draw solution temperature is raised to LCST or higher to separate the dilute phase (low concentration draw solution) and the concentrated phase (high concentration draw solution).
  • the separation tank 3 has a heating mechanism.
  • the membrane separation step the low-concentration draw solution is separated into water and a concentrate containing a draw solute using a separation membrane as a driving force by a pressure difference due to pressurization, decompression, or the like.
  • a separation membrane for example, a UF membrane, NF membrane, RO membrane or the like can be used.
  • the temperature of the membrane separation process is preferably higher than the temperature of the forward osmosis process. Further, a temperature lower than the phase separation temperature is preferable.
  • the temperature in the membrane separation step is more preferably 40 ° C. or higher and 90 ° C. or lower, still more preferably 40 ° C. or higher and 85 ° C. or lower, and even more preferably 40 ° C. or higher and 80 ° C. or lower.
  • the water which is the target object of a water treatment method can be obtained by collect
  • the obtained water may be subjected to a treatment for further improving the quality of the water.
  • the draw solute separated in the membrane separation step and the concentrated liquid (high concentration draw solution) containing the draw solute obtained in the phase separation step are preferably reused as a draw solution in the forward osmosis step.
  • FIG. 1 is a schematic diagram showing an example of a water treatment system according to the present invention.
  • the water treatment system used for said water treatment method is as follows.
  • Forward osmosis module 1 comprising two chambers 12;
  • a separation tank 3 having a heating mechanism for separating the draw solution into a low-concentration draw solution and a high-concentration draw solution by increasing the temperature of the draw solution;
  • a separation membrane 20 separation membrane module 2 for separating the low-concentration draw solution into water and a draw solute.
  • the separation tank 3 has a heating mechanism. That is, warm water such as waste hot water is supplied around the separation tank 3 in order to raise the temperature of the dilution DS supplied to the separation tank 3 and cause phase separation. What is necessary is just to adjust the temperature of warm water according to the target value of the temperature after DS raises in a phase-separation process.
  • the draw solution (diluted DS) is phase-separated into a low concentration DS and a high concentration DS as the temperature rises.
  • the high-concentration DS separated in the separation tank 3 and the low-concentration DS concentrated in the separation membrane module 2 are sent to the tank 5 by the pump 44 and temporarily stored. Can be reused as DS.
  • the separation membrane examples include a semipermeable membrane called an ultrafiltration membrane (UF membrane: Ultrafiltration Membrane), a nanofiltration membrane (NF membrane: Nanofiltration Membrane), and a reverse osmosis membrane (RO membrane: Reverse Osmosis Membrane).
  • UF membrane Ultrafiltration Membrane
  • NF membrane Nanofiltration Membrane
  • RO membrane Reverse Osmosis Membrane
  • the separation membrane module preferably has heat resistance at high temperatures (for example, 40 ° C. or higher). This is because the membrane separation process can be performed on the high-temperature low-concentration DS discharged from the separation tank 3.
  • heat-resistant separation membrane examples include polyethersulfone (PES) resin, polyamide (PA) resin, polyvinyl alcohol (PVA) resin, and the like. Further, in the separation membrane module, parts other than the separation membrane also have heat resistance, and preferably have heat resistance as a whole.
  • heat-resistant separation membrane module products include Thermo Plus (manufactured by Nitto Denko Corporation), Durathermo (manufactured by GE Water Technologies), and Romenbra (registered trademark) TS series (manufactured by Toray Industries, Inc.). Can be mentioned.
  • heat-resistant separation membrane examples include ceramics such as alumina and silica.
  • examples of the silica for the heat resistant membrane include silica derived from bistryl ethoxysilyl ethane (Atsushi Tsuru, “Development of a Robust RO / NF Membrane That Can Correspond to Various Water Sources”, Journal of Water Environment Society, vol. 36 (A), No.1, pp.8-10, 2013).
  • FIG. 2 is a schematic view showing another example of the water treatment system according to the present invention.
  • the water treatment system shown in FIG. 2 includes heat exchangers 61 and 62 in addition to the water treatment system shown in FIG. This reduces the heat energy required for the phase separation process by heating the diluted DS using the low-concentration DS and high-concentration DS waste heat discharged from the separation tank 3, and the energy efficiency of the water treatment Can be increased.
  • the separation membrane module 2 used for normal water treatment is often used at room temperature, the heat resistance at high temperature (for example, 40 ° C. or more). Often does not have. For this reason, the separation membrane module 2 is provided downstream from the heat exchanger 61, and in the separation membrane module 2, the membrane separation step is performed on the low concentration DS after the temperature is lowered.
  • the separation membrane module 2 (separation membrane 20) is arranged on the upstream side of the heat exchanger 61. Thereby, the membrane separation process is performed on the high-temperature low-concentration DS discharged from the separation tank 3.
  • the present inventors reduce the energy required for the pump. It has been found that the energy efficiency of water treatment is improved.
  • 1 forward osmosis module 10 forward osmosis membrane, 11 first chamber, 12 second chamber, 2 separation membrane module, 20 separation membrane, 3 separation tank, 41-48 pump, 5 tanks, 61, 62 heat exchanger.

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  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Organic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

L'invention concerne un procédé de traitement d'eau caractérisé en ce qu'il comprend les étapes suivantes : l'osmose directe, destinée à faire passer l'eau contenue dans une solution à traiter, qui comprend de l'eau et des constituants autres que l'eau, à travers une membrane d'osmose directe jusque dans une solution d'extraction en amenant une surface de la membrane d'osmose directe en contact avec la solution à traiter et en amenant l'autre surface de la membrane d'osmose directe en contact avec une solution d'extraction comportant un soluté d'extraction, dont la solubilité diminue lorsque la température augmente ; la séparation de phases après l'étape d'osmose directe afin de séparer la solution d'extraction en une solution d'extraction à faible concentration et en une solution d'extraction à forte concentration en élevant la température de la solution d'extraction ; la séparation sur membrane afin de séparer la solution d'extraction de faible concentration pour donner de l'eau et une solution concentrée contenant le soluté d'extraction à l'aide d'une membrane de séparation, la température de l'étape de séparation sur membrane étant supérieure à la température de l'étape d'osmose directe.
PCT/JP2017/043819 2017-02-17 2017-12-06 Procédé et système de traitement d'eau Ceased WO2018150690A1 (fr)

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WO2020049579A1 (fr) * 2018-09-07 2020-03-12 Jani Jigar Systèmes combinatoire à base de membranes et procédés de déshydratation et de concentration d'applications
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