WO2013111372A1 - Procédé de traitement de l'eau et système de traitement de l'eau - Google Patents

Procédé de traitement de l'eau et système de traitement de l'eau Download PDF

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Publication number
WO2013111372A1
WO2013111372A1 PCT/JP2012/073216 JP2012073216W WO2013111372A1 WO 2013111372 A1 WO2013111372 A1 WO 2013111372A1 JP 2012073216 W JP2012073216 W JP 2012073216W WO 2013111372 A1 WO2013111372 A1 WO 2013111372A1
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WIPO (PCT)
Prior art keywords
water
filter aid
solid
filtration membrane
treated
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PCT/JP2012/073216
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English (en)
Japanese (ja)
Inventor
深谷　太郎
厚 山崎
剣治 堤
伊知郎 山梨
Original Assignee
株式会社 東芝
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Publication of WO2013111372A1 publication Critical patent/WO2013111372A1/fr

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    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3242—Layers with a functional group, e.g. an affinity material, a ligand, a reactant or a complexing group
    • B01J20/3268—Macromolecular compounds
    • B01J20/3272—Polymers obtained by reactions otherwise than involving only carbon to carbon unsaturated bonds
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009—Magnetic properties
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204—Inorganic carriers, supports or substrates
    • 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
    • C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
    • C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
    • 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
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C02F1/004—Processes for the treatment of water whereby the filtration technique is of importance using large scale industrial sized filters

Definitions

  • the embodiment described herein relates to a water treatment method and a water treatment apparatus for purifying factory effluent and domestic effluent using a filter aid.
  • the membrane separation method is one of the most commonly employed methods for removing insoluble substances in water.
  • the membrane separation method is often used in the form of using a filter aid such as a so-called precoat method or body feed method from the viewpoint of protecting the filtration membrane or from the viewpoint of increasing the flow rate of water containing a hardly dehydrated substance. It is used.
  • the embodiments described herein are made to solve the above-described problems, and are a water treatment method and a water treatment capable of efficiently removing fine solids in water and easily reusing a filter aid.
  • An object is to provide an apparatus.
  • a water treatment method comprises: (a) a magnetic primary particle or an aggregate thereof, and a coating having the critical surface tension ⁇ c of 22 ⁇ 10 ⁇ 3 N / m or less, which coats the magnetic primary particle or the aggregate.
  • Preparing a filter aid containing a material (b) mixing a dispersion medium with the filter aid, producing a suspension in which the filter aid is dispersed in the dispersion medium, and (c) a filtration membrane
  • the suspension is filtered by the above, a precoat layer containing a filter aid is formed on the filter membrane, and then the water to be treated containing solids is passed through the precoat layer and the filter membrane.
  • the solid content is captured by adsorption, thereby separating the solid content from the water to be treated; and (d) the precoat layer is peeled off from the filtration membrane by pouring water into the precoat layer. , Solids trapped in the precoat and water poured into the precoat layer Obtaining a mixture, (e) magnetically separating the filter aid from the mixture, and (f) reusing the separated filter aid in the step (b) to make a suspension. .
  • the characteristic diagram which shows an example of the Zisman plot used when calculating
  • (A) is a cross-sectional schematic diagram which shows the aggregate which the magnetic particle aggregated
  • (b) is a cross-sectional schematic diagram which shows the magnetic particle coat
  • Schematic which shows an example of the apparatus used in the water treatment method which concerns on 1st Embodiment. Process drawing which shows an example of the water treatment method (precoat method) which concerns on 1st Embodiment. Schematic which shows an example of the apparatus used in the water treatment method which concerns on 2nd Embodiment. Process drawing which shows an example of the water treatment method (body feed method) which concerns on 2nd Embodiment.
  • a water treatment method comprises: (a) a magnetic primary particle or aggregate thereof and a magnetic primary particle or aggregate thereof, and a coating material having a critical surface tension ⁇ c of 22 ⁇ 10 ⁇ 3 N / m or less And (b) preparing a suspension in which the filter aid is dispersed in the dispersion medium, and (c) using a filter membrane.
  • the suspension is filtered, a precoat layer containing a filter aid is formed on the filter membrane, and then water to be treated containing solids is passed through the precoat layer and the filter membrane, and the solid is added to the filter aid of the precoat layer.
  • the water treatment method according to the first embodiment is a method corresponding to a so-called precoat method.
  • this water treatment method is a filtration comprising magnetic primary particles or aggregates thereof and a coating material having a critical surface tension ⁇ c of 20 ⁇ 10 ⁇ 3 N / m or less that coats the particles. Including providing an auxiliary agent.
  • the critical surface tension ⁇ c is a parameter related to the wettability of a solid liquid.
  • the solid is not wetted by a liquid having a surface tension ⁇ L greater than its critical surface tension ⁇ c .
  • the critical surface tension ⁇ c is obtained by dripping a liquid with various surface tensions onto a solid, obtaining the surface tension of the liquid whose contact angle becomes zero by extrapolation, and calculating the surface tension value of the liquid.
  • the critical surface tension can be obtained by the Zisman method.
  • it is good also as a literature value with a close composition. For example, values described in a plastic data book (Asahi Kasei Amidus Co., Ltd., “Plastics” editorial department, P. 35, (1999)) are used.
  • the critical surface tension ⁇ c can be determined using the Jisman method.
  • various liquids having a known surface tension ⁇ L are brought into contact with the surface of a solid that is difficult to wet with water, and the contact angle ⁇ is measured.
  • a value of cos ⁇ is obtained from the measured contact angle ⁇ , the obtained cos ⁇ value is taken on the vertical axis (Y axis), and the corresponding surface tension ⁇ L of the liquid is taken on the horizontal axis (X axis), for example, as shown in FIG.
  • each measurement result is plotted one after another on the XY coordinates. As a result, a figure with a large number of plots is completed.
  • the tendency of the plot group in the created figure is obtained by using a calculation method such as the least square method, and a straight line Z having the obtained inclination is drawn in the figure.
  • This straight line Z is called a Zisman plot.
  • the value (surface tension value) of the X-axis intercept of the obtained straight line Z is particularly called critical surface tension ⁇ c .
  • the solid is not wetted by a liquid having a surface tension ⁇ L greater than the critical surface tension ⁇ c .
  • the critical surface tension ⁇ c of 22 ⁇ 10 ⁇ 3 N / M or less is smaller than the surface tension of water. Therefore, by using a filter aid including a coating material having a critical surface tension ⁇ c of 22 ⁇ 10 ⁇ 3 N / M or less, the filter aid and solids in water can be easily obtained by performing simple operations. Can be separated. That is, since this filter aid has a low critical surface tension ⁇ c , solid matter in water can be separated into solid and liquid using stirring or ultrasonic waves in water, and only the filter aid is adsorbed on a magnet and recovered. Can do.
  • the shape of the magnetic particles can be various shapes such as a spherical shape and a polyhedron, but is not particularly limited. Alternatively, the magnetic particles may be indefinite. What is necessary is just to select suitably the particle size and shape of a magnetic particle desirable in use in view of manufacturing cost. In particular, a polyhedral structure having a spherical shape or rounded corners is preferable.
  • the specific gravity of the filter aid becomes relatively high.
  • a filter aid having a relatively large specific gravity is used in combination with sedimentation by gravity and centrifugal separation using a cyclone in combination with magnetic separation in the separation of the mixture containing the filter aid, the capture target and water. Filter aid can be quickly separated from the mixture.
  • Ferromagnetic materials can be generally used as the magnetic material.
  • iron, iron-base alloys, magnetite (magnetite), titanite (ilmenite), pyrrhotite (pilotite), magnesia ferrite, manganese magnesium ferrite, manganese Zinc ferrite, cobalt ferrite, nickel ferrite, nickel zinc ferrite, barium ferrite, copper zinc ferrite and the like can be used.
  • a ferrite-based compound such as magnetite, magnesia ferrite, or manganese magnesium ferrite having excellent stability in water.
  • Magnetite Fe 3 O 4
  • the magnetic particles may be single magnetic single particles (primary particles) or aggregates (secondary particles) obtained by aggregating the primary particles.
  • the average particle diameter of the primary particles is preferably in the range of 0.5 to 5 ⁇ m. If the average particle diameter of the magnetic primary particles is in the range of 0.5 to 5 ⁇ m, the distance between the particles becomes too large, and there is a risk of generating a through-pass that allows fine precipitates in water to be described later to pass through. Can be reduced. Further, when the average particle diameter of the magnetic primary particles is in the range of 0.5 to 5 ⁇ m, it becomes easy to provide an effective water flow rate due to the gaps between the particles.
  • a silicone resin or a fluororesin can be used as the covering material having a critical surface tension ⁇ c of 22 ⁇ 10 ⁇ 3 N / m or less.
  • Silicone resin is a polymer compound made of organopolysiloxane, and there are two types, one-pack type and two-pack type. Examples include the KE series and KR series, which are products of Shin-Etsu Chemical Co., Ltd.
  • Fluorine resin is a general term for fluorine-containing polymers.
  • PTFE polytetrafluoroethylene
  • PFA tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer
  • FEP tetrafluoroethylene-hexafluoropropylene copolymer
  • ETFE Tetrafluoroethylene-ethylene copolymer
  • PVDF polyvinylidene fluoride
  • ECTFE chlorotrifluoroethylene-ethylene copolymer
  • PCTFE polychlorotrifluoroethylene
  • PVF polyvinyl fluoride
  • the critical surface tension ⁇ c of PTFE is about 18 ⁇ 10 ⁇ 3 N / m.
  • a resin obtained by copolymerizing these resins with an epoxy resin, polyimide, polyamide or the like is used to improve the adhesion with the magnetic particles. Even when these resins are copolymerized, since the fluororesin is localized on the resin surface, the critical surface tension of the fluororesin may be used as the surface tension of the coating material.
  • the filter aid containing the magnetic primary particles can be obtained by, for example, applying a solution of these resins to the surface of the magnetic primary particles 11 and curing (solidifying) the resin, for example, as shown in FIG.
  • the filter aid 10 including the magnetic primary particles 11 and the coating material 12 covering the primary particles 11 can be produced.
  • the diameter of the filter aid containing the magnetic primary particles is D1.
  • a method of making a filter aid composed of aggregates a method of applying a coating material having a critical surface tension ⁇ c of 22 ⁇ 10 ⁇ 3 N / m or less after forming aggregates first with a granulator or the like, There is a method in which primary particles are granulated using a material having a surface tension ⁇ c of 22 ⁇ 10 ⁇ 3 N / m or less as a binder.
  • the former, the primary particles and an organic binder or an inorganic binder was kneaded by a spray dryer or a Henschel mixer, the after critical surface tension gamma c is 22 ⁇ 10 -3 N / m or less of the material that made granular material.
  • coating material is mentioned.
  • the latter is granulated directly with a Henschel mixer or spray dryer using a binder with a material with a critical surface tension of 22 ⁇ 10 ⁇ 3 N / m or less.
  • a filter aid containing aggregated magnetic particles 10 and a binder 13 that binds these primary particles 10 to each other is obtained.
  • the diameter of the filter aid made of the aggregate is D2.
  • the average particle size of the filter aid is preferably in the range of 1 to 50 ⁇ m.
  • a filter aid having an average particle size in the range of 1 to 50 ⁇ m fine particles in water can be captured by adsorption.
  • an effective amount of treated water can be obtained, and the possibility of spilling particles to be captured can be reduced.
  • the average particle size is in the range of 2 to 35 ⁇ m. When the average particle diameter is 2 ⁇ m or more, a more effective amount of treated water can be obtained. Further, when the average particle size is 35 ⁇ m or less, the particles to be captured can be captured more reliably by adsorption.
  • the average particle diameter of the filter aid is obtained by calculation using a plurality of actual measurement values measured by a laser diffraction method.
  • the particle size of the filter aid can be measured using a SALD-DS21 measuring device (product name) manufactured by Shimadzu Corporation.
  • the average particle diameter of a filter aid is a volume average particle diameter (Mean Volume Diameter).
  • the volume average particle size is a value obtained by calculating the average particle size based on the volume of the particles.
  • Such a filter aid is excellent in separability and durability, and the filter aid can be repeatedly used in a cycle of dispersion ⁇ adsorption ⁇ separation ⁇ recovery ⁇ dispersion.
  • FIG. 3 is a schematic view showing an example of an apparatus used in the water treatment method according to the first embodiment.
  • FIG. 4 is a process diagram showing an example of a water treatment method (precoat method) according to the first embodiment.
  • the water treatment apparatus 1 shown in FIG. 3 is an apparatus used in the precoat method, and is effectively used particularly when the concentration of a substance insoluble in water in the water to be treated is low.
  • the water treatment apparatus 1 includes a treated water tank 2, a solid-liquid separation apparatus 3, a magnetic separation tank 4, a filter aid supply apparatus 5, a mixing tank 6, an untreated water supply source (not shown), and a waste water storage tank. These devices and apparatuses are connected to each other by a plurality of piping lines L1 to L8.
  • Various pumps P1 to P9, valves V1 to V3, measuring instruments and sensors (not shown) are attached to the piping lines L1 to L8.
  • a detection signal is input from these measuring instruments and sensors to an input section of a controller (not shown), and control signals are output from the output section of the controller to pumps P1 to P9 and valves V1 to V3, respectively, and their operations are controlled. It has become so. As described above, the entire water treatment apparatus 1 is comprehensively controlled by a controller (not shown).
  • the treated water tank 2 has a stirring screw 21 for stirring the water to be treated.
  • treated water containing a substance insoluble in water for example, factory wastewater, is introduced from a treated water supply source (not shown) via the line L1.
  • the solid-liquid separator 3 has a built-in filtration membrane 33 that partitions the interior into an upper space 31 and a lower space 32.
  • the upper space 31 of the solid-liquid separator is connected to the treated water tank 2 via a treated water supply line L2 having a pressure pump P1. Further, a water supply line (first treated water utilization line) L31 having a pump P5 and a peeled material discharge line L4 are connected to the side portions of the upper space 31, respectively.
  • the lower space 32 of the solid-liquid separator is connected to a treated water distribution line L3 having three three-way valves V1, V2, and V3.
  • the separation water supply line (first treated water utilization line) L31 is branched from the treated water distribution line L3.
  • a treated water supply line L32 having a pump P2 branches off from the treated water distribution line L3 at the second three-way valve V2.
  • two lines L33 and L34 are branched from the treated water distribution line L3.
  • One branch line (second treated water utilization line) L33 has a pump P4 and is connected to a separation tank 4 described later.
  • the other branch line (third treated water utilization line) L34 has a pump P5 and is connected to a mixing tank 6 described later.
  • filtration membrane 33 various materials such as woven fabric, nonwoven fabric, paper, wire mesh (mesh), resin mesh (mesh), porous polymer membrane, porous ceramic membrane can be used.
  • a cloth is most preferred.
  • fabrics such as double weave, twill weave, plain weave and satin weave are used.
  • the material of the filter cloth may be any of synthetic fibers such as polypropylene, nylon and polyester, or natural fibers such as cotton and hemp.
  • the average pore size of the filtration membrane 33 is set to a size that does not allow the filtration aid to pass through.
  • Silicone resin and fluororesin that covers the surface of the filter aid are highly hydrophobic, so multiple particles of the filter aid adhere to each other and form a bridge, and even with a pore size larger than the average particle size, the layers are sufficiently laminated. Because it can.
  • the filtration membrane 33 preferably has a filtration surface orthogonal to the direction in which gravity acts.
  • the filter aid Since the above-mentioned filter aid has a low critical surface tension ⁇ c , it is difficult to hold the filter aid on the filter membrane 33. For this reason, if the surface is not perpendicular to the direction of gravity (that is, a horizontal surface), the filter aid slips on the filtration membrane 33 and may not be easily laminated to a uniform thickness. In the filtration membrane 33 having a filtration surface orthogonal to the direction of gravity, this worry is small.
  • the filtration surface of the filtration membrane 33 is orthogonal to the direction in which gravity acts, the gravity acts on the suspension and the water to be treated to the maximum, and the filtration action allows water molecules to pass through the filtration membrane 33. Is promoted.
  • the suspension or water to be treated is pressurized, the water flow rate passing through the filtration membrane 33 is increased, and the filtration efficiency is further improved.
  • the magnetic separation tank 4 has a stirring screw 41 for stirring the washing discharge water received from the upper space 31 of the solid-liquid separation device through the peeled material discharge line L4, and is separated into a solid and a filter aid.
  • the magnet 42 for carrying out is built in.
  • the magnet 42 is in a cylindrical pipe whose one end is closed, and is controlled by a controller (not shown).
  • the controller can control, for example, vertical movement of the magnet 42 and on / off of the magnetic field of the magnet 42.
  • a second treated water use line L33 branched from the treated water distribution line L3 is connected to the upper part of the magnetic separation tank 4, and has passed through the filter 33 of the solid-liquid separator. A part of the treated water is supplied to the magnetic separation tank 4, and a part of the treated water is reused in the magnetic separation tank 4.
  • a concentrated water discharge line L8 and a filter aid return line L5 are connected to the lower part of the magnetic separation tank 4, respectively.
  • the concentrated water discharge line L8 has a pump P9 and is a pipe for discharging water-insoluble matter concentrated water from the magnetic separation tank 4 to a storage tank (not shown).
  • the filter aid return line L5 is a pipe having a pump P6 for returning the filter aid separated and recovered from the magnetic separation tank 4 to the filter aid supply device 5.
  • the filter aid supply device 5 is newly replenished with a filter aid supply source (not shown), and the filter aid separated in the magnetic separation tank 4 passes through the filter aid return line L5 described above. It is supposed to be returned. Moreover, the filter aid supply apparatus 5 supplies an appropriate amount of filter aid to the mixing tank 6 through a filter aid supply line L6 having a pump P7.
  • the mixing tank 6 has a stirring screw 61 for stirring the filter aid and the dispersion medium.
  • the mixing tank 6 is configured to add a dispersion medium to the filter aid supplied from the filter aid supply device 5 and stir and mix using the stirring screw 61 to produce a suspension containing the filter aid. ing. It is preferable to use water as the dispersion medium.
  • a third treated water utilization line L34 branched from the treated water distribution line L3 is connected to the upper part of the mixing tank 6, and a part of the treated water that has passed through the filter 33 of the solid-liquid separator is supplied to the mixing tank 6. In the mixing tank 6, a part of the treated water is reused as a dispersion medium.
  • a suspension supply line L7 having a pump P8 communicates with an appropriate place of the mixing tank 6.
  • the suspension supply line L7 is connected and joined at an appropriate position of the treated water supply line L2.
  • the slurry suspension from the suspension supply line L7 is added to the water to be treated flowing through the water supply line L2.
  • the suspension supply line L7 is provided with a flow control valve (not shown) so that the flow rate of the suspension is adjusted by the controller.
  • the suspension supply line L7 does not have to be connected at an appropriate position of the to-be-treated water supply line L2.
  • the treated water can flow through the suspension supply line L7.
  • the suspension prepared in the mixing tank 6 has a large solid content, when this is directly sent from the line L7 to the filtration membrane of the solid-liquid separator, a part of the filter aid remains in the line L7.
  • the suspension supply line L7 is connected and joined at an appropriate position of the treated water supply line L2
  • the treated water can flow through the suspension supply line. Since the treated water is sent to the solid-liquid separation device together with the filter aid remaining in the line when passing the treated water, a prescribed precoat thickness can be obtained.
  • FIG. 4 is a process diagram showing an example of a water treatment method (precoat method) according to the first embodiment.
  • the water treatment apparatus 1 shown in FIG. 3 can be used.
  • the precoat method is particularly effective when the concentration of substances insoluble in water to be treated is low.
  • the substance insoluble in water contained in the water to be treated is not particularly limited to organic substances and inorganic substances. Even if the particles are hardly dewatering particles such as heavy metal hydroxides or contain non-water-removing components other than particles, such as oil, they can be easily filtered by the structure of the filter aid. In this case, it is preferable to appropriately select a coating material for the filter aid according to the properties of the wastewater that is the water to be treated.
  • the filter aid and the dispersion medium are mixed in the mixing tank 6 to prepare a suspension containing the filter aid (step S1).
  • the filter aid can be produced by the method described above.
  • water is mainly used as the dispersion medium, other dispersion medium can be appropriately used in addition to water.
  • the concentration of the filter aid in the suspension is not particularly limited as long as a precoat layer, that is, a filter aid deposited layer can be formed by the following operation, but is adjusted to, for example, about 10,000 to 200,000 mg / L.
  • the suspension is passed through the filtration membrane 33 of the solid-liquid separator 3, and the filter aid in the suspension is filtered off and left on the filtration membrane 33, and the particle deposition is formed by laminating the filter aid.
  • a layer (precoat layer) is formed (step S2).
  • the water flow to the filtration membrane 33 by the pressurization pump P1 is performed at a predetermined pressure.
  • the filtration membrane 33 is attached so as to close the inlet of the solid-liquid separation device 3, and the suspension membrane is filtered by the filtration membrane 33 so that the pressure drop of the suspension in the solid-liquid separation device 3 is minimized. Do it. Specifically, by reducing the upper space 31 defined by the container wall of the solid-liquid separator 3 and the filtration membrane 33 and pushing the pressurized suspension into the small space 31 with a small volume, Separation of solid (filter aid) and liquid by the filter membrane 33 is promoted. At this time, the liquid component of the suspension quickly permeates through the filtration membrane 33 and the solid component of the suspension (filter aid) passes through the filtration membrane 33 due to the synergistic action of the pressure and gravity caused by driving the pressurizing pump P1. As a result, a precoat layer is formed on the filtration membrane 33. The thickness of the precoat layer varies depending on the concentration of the liquid to be treated, but is about 0.1 to 10 mm.
  • the water to be treated is pumped from the treated water tank 2 to the solid-liquid separation device 3 through the line L2 by driving the pump P1, and the treated water is passed through the filter 33 and the precoat layer (step S3).
  • the water-insoluble solid in the water to be treated is captured by adsorption by the filter aid in the precoat layer.
  • the valve V1 When the water to be treated is filtered, the valve V1 is switched, the pump P3 is started, and the pump P3 is driven to pass a part or all of the treated water to the upper space 31 of the solid-liquid separator through the line L3 ⁇ L31. return.
  • the returned treated water is used as water for peeling the precoat layer from the filter 33.
  • Treated water is sprayed onto the precoat layer from the side of the upper space 31 to peel off the precoat layer from the filter 33. Further, treated water is sprayed onto the peeled material to decompose the peeled material apart, and the filter aid and solid content are dispersed Disperse in the medium (step S4).
  • the separation and decomposition of the precoat layer may be performed in a container in which a filter is installed, or may be performed in another container.
  • the precoat layer is peeled and decomposed in another container, the precoat layer is decomposed into a decomposed product having a certain size by using means such as an injection nozzle and then transported.
  • the line L31 may be replenished with water from another location.
  • Water is preferably used for peeling and decomposing the precoat layer, but it is also possible to exfoliate and decompose the precoat layer using a surfactant or an organic solvent.
  • the treated water generated from the solid-liquid separation device 3 is sent to the solid-liquid separation device 31 via the line L31, it can be effectively used as peeling water for peeling the precoat.
  • a treated water storage tank for temporarily storing the treated water is provided, and the solid-liquid separation device 3 is provided from the storage tank as necessary. The treated water can be sent to the upper space 31.
  • the water for peeling off the precoat layer does not include the treated water generated from the solid-liquid separator 3, and may be water from other places.
  • the suspension containing the peeled material of the precoat layer is sent from the upper space 31 to the magnetic separation tank 4 through the line L4, and the decomposition product of the precoat layer is stirred in the magnetic separation tank 4 by the stirring screw 41. Further break down to particle level and disperse filter aid and solids. When this stirring is sufficiently performed, the filter aid and the solid content are more uniformly dispersed in the suspension, and the filter aid is easily separated.
  • Magnetic separation methods include a method of collecting permanent magnets or electromagnets in the container of the magnetic separation tank 4 and a method of collecting particles by collecting them with a metal mesh magnetized by a magnet and releasing a magnetic field. Is mentioned.
  • the filter aid can be recovered by the following method.
  • the permanent magnet 42 is installed in a cylindrical pipe whose one end is closed, and the filter aid is adsorbed and fixed by the magnet 42 in the suspension.
  • the waste liquid containing the solid content is discharged from the container of the magnetic separation tank 4 to the storage tank (not shown) via the line L8.
  • the magnet 42 is pulled up by an air cylinder (not shown) attached to the upper part of the magnet 42 to turn off the magnetic field, and the filter aid is dropped from the magnet 42.
  • a part of the treated water is supplied from the solid-liquid separation device 3 into the container via the line L33, and the treated water is added to the dropped filter aid to form a slurry or suspension.
  • the liquid filter aid is sent from the separation tank 4 to the filter aid supply device 5 via the line L5.
  • the filter aid is moved to another container together with the magnet 42, the magnetic field of the magnet 42 is turned off in the other container, and the filter aid is removed from the magnet 42. It is possible to drop off and collect the filter aid in another container.
  • the recovered filter aid is supplied from the filter aid supply device 5 to the upper space 31 of the solid-liquid separation device 3 via the line L6, and the recovered filter aid is reused to form the precoat layer.
  • the filter aid can be used repeatedly in the cycle of precoat layer formation ⁇ filtration ⁇ separation ⁇ recovery ⁇ precoat layer formation.
  • the filter aid excellent in separability and durability since the filter aid excellent in separability and durability is used, the operation cost of water treatment and the maintenance cost of the water treatment device can be kept low.
  • the filter aid and the solid matter (water insoluble substance such as SS) captured by the magnetic adsorption means such as an electromagnet can be quickly and It can be reliably separated. Therefore, according to the first embodiment, the separated filter aid can be recovered efficiently and smoothly, and the recovered filter aid can be reused repeatedly. It is easy to reuse the filter aid, and fine solid matter in water can be removed without adding chemicals.
  • This water treatment method comprises: (A) a magnetic primary particle or an aggregate thereof and a magnetic primary particle or an aggregate thereof, and a coating material having a critical surface tension ⁇ c of 22 ⁇ 10 ⁇ 3 N / m or less Preparing a filter aid containing, and (B) mixing the water to be treated containing the solid content and the filter aid, producing a suspension in which the filter aid is dispersed in the water to be treated; (C) The suspension is filtered through a filtration membrane, a deposition layer containing a filter aid and solid content is formed on the filtration membrane, and the solid content is captured by adsorption in the filtration aid in the deposition layer.
  • the water treatment method according to the second embodiment is a method corresponding to the so-called body feed method.
  • the water to be treated is used as a dispersion medium for dispersing the filter aid, and the suspension containing the water to be treated and the filter aid is prepared without forming a precoat layer. It differs from the water treatment method according to the first embodiment in that it is filtered to form a deposition layer containing a filter aid and a solid content contained in the water to be treated.
  • the supply of the water-insoluble matter and the supply of the filter aid are performed at the same time, particularly when the amount of solid content in the water to be treated (suspension) is large. Therefore, the water-insoluble matter excessively adsorbed by the filter aid does not embed the gap of the filter aid. For this reason, the method according to the second embodiment can maintain the filtration rate for a long time. As a result, the water treatment method of the second embodiment is effective when the concentration of water insoluble matter in the water to be treated is high.
  • FIG. 5 is a schematic view showing an example of an apparatus used in the water treatment method according to the second embodiment.
  • FIG. 6 is a process diagram showing an example of a water treatment method (body feed method) according to the second embodiment.
  • 5A differs from the water treatment apparatus 1 shown in FIG. 3 in that there is no mixing tank 6 and in that a mixed raw water tank 2A is provided instead of the treated water tank 2.
  • the mixing raw water tank 2A has a function of temporarily storing the water to be treated and leveling the flow rate of the water to be treated, and a mixing function of adding a filter aid to the water to be treated and mixing them. Yes. That is, in the apparatus 1A of the present embodiment, the filter aid is directly supplied from the filter aid supply device 5 into the mixed raw water tank 2A via the line L6 without going through the mixing tank. .
  • FIG. 6 is a process diagram showing an example of a water treatment method (body feed method) according to the second embodiment.
  • the filter aid and the dispersion medium are first mixed to prepare a suspension, and the dispersion medium used in this case is treated water existing in the mixing raw water tank 2A. . That is, in the second embodiment, a filter aid is directly added to the water to be treated to prepare a suspension from the water to be treated (Step K1).
  • the concentration of the filter aid in the suspension is not particularly limited as long as a filtration layer can be formed by the following operation, but is adjusted to, for example, about 10,000 to 200,000 mg / L.
  • the suspension (water to be treated) is passed through the filtration membrane 33, the filter aid in the suspension is filtered off and left on the filter membrane 33, and the deposited layer formed by laminating the filter aid is formed.
  • Form (step K2) the water flow with respect to the filtration membrane 33 is performed under pressure. At this time, the formation of the deposited layer and the filtration treatment of the water to be treated are performed in parallel. In the method of the second embodiment, it is preferable that the filter surface is horizontal.
  • the filtering described above is performed by, for example, arranging the filtration membrane so as to close the container opening of the predetermined container, and the filtration thus arranged.
  • the filter aid remains on the membrane so that it can be aligned and stacked.
  • the deposited layer is formed and held by the external force from the wall surface of the container and the downward external force (gravity) due to the weight of the filter aid positioned above.
  • the filter layer is dispersed in the dispersion medium, the filter layer is decomposed into a filter aid, and the filter aid is washed (step K3).
  • This washing may be performed in a container in which the filtration membrane 33 is installed, or may be performed in another container.
  • the deposited layer is decomposed into a filter aid by means of cleaning or the like and then transported.
  • water is used for washing, washing with a surfactant or an organic solvent is also possible.
  • the washed filter aid is recovered using a magnetic separation method (step K4).
  • the method used for the magnetic separation method is not particularly limited, but a method of collecting a permanent magnet or an electromagnet in a container and a method of collecting particles by collecting them with a metal mesh magnetized by a magnet and releasing a magnetic field Etc.
  • the filter aid it is easy to reuse the filter aid, and fine solid matter in water can be removed without adding chemicals.
  • the filter aid constituting the deposition layer is contained in the water to be treated, that is, the suspension prepared using this water, and should be removed.
  • a filter aid is always supplied together with the water to be treated (suspension) containing water-insoluble solids.
  • the supply of the water-insoluble matter and the supply of the filter aid are performed at the same time even when the amount of solid content in the water to be treated (suspension) is large.
  • the filtration rate can be maintained for a long time.
  • the water treatment method of the second embodiment is effective when the concentration of water insoluble matter in the water to be treated is high.
  • (Preparation of filter aid) (Filter aid A) Manganese magnesium ferrite particles were placed in a Henschel mixer. Next, a resin dispersion containing 2% polyamide imide comprising a reaction product of maleic anhydride and diaminodiphenylmethane and 10% copolymer of fluorinated ethylene and fluorinated polypropylene is put into the Henschel mixer. The resin dispersion was sprayed onto the surface of the manganese magnesium ferrite particles. By hardening the ferrite particles coated with the resin dispersion on the surface at 200 ° C.
  • a filter aid containing manganese magnesium ferrite particles and a fluororesin coating coated on the surface of the particles was obtained ( Spherical, average particle size 35 ⁇ m).
  • the critical surface tension ⁇ c of the fluororesin coating was 18.5 ⁇ 10 ⁇ 3 N / m.
  • Filter aid E Manganese magnesium ferrite particles having an average particle diameter of 35 ⁇ m were prepared as filter aids for comparative examples.
  • Filter aid F a filter aid containing manganese magnesium ferrite particles and a fluororesin coating coated on the surface thereof was prepared (spherical, average particle size 14 ⁇ m).
  • (Filter aid G) A metal oxide mixture in which the molar ratio was adjusted to 40% manganese, 10% magnesium, and 50% iron was prepared. This was dispersed in water, and a granulated body having an average particle diameter of 40 ⁇ m was produced by spray drying at 200 ° C. using polyvinyl alcohol as a binder. The granulated body was sintered at 1200 ° C. to obtain a porous manganese magnesium ferrite. In the same manner as the filter aid A, this porous manganese magnesium ferrite was spray-coated with a fluororesin dispersion on the surface thereof and subjected to curing. As a result, a filter aid containing porous manganese magnesium ferrite and a fluororesin coating coated on the surface thereof was obtained (spherical, average particle size 40 ⁇ m).
  • Filter aid H a filter aid containing manganese magnesium ferrite particles and a fluororesin coating coated on the surface thereof was prepared (spherical, average particle diameter 85 ⁇ m).
  • Example 1 Water treatment equipment (Example 1) A device as schematically shown in FIG. 3 was produced.
  • the water to be treated containing solid matter is supplied to the treated water tank 2 and temporarily received in the tank.
  • the time fluctuation of the treated water is averaged by mixing with a mixer.
  • a filter aid is sent from the filter aid supply device 5 to the mixing tank 6 and mixed with treated water that is partially reused to produce a filter aid slurry.
  • This filter aid slurry is first sent to the solid-liquid separator 3 to form a filter aid membrane on the filter membrane 33.
  • a filter cloth made of woven cloth was used as the filter membrane.
  • the filtrate (treatment liquid) is the one from which the solid matter has been removed and may be drained after necessary treatment, but the washing water for the solid-liquid separation device 3 and the washing water for the magnet of the magnetic separation tank 4 are mixed. It can also be used as a liquid when preparing the filter aid slurry in the tank 6.
  • a filter aid and a solid deposit (cake) in water are present in the filter membrane 33 in the solid-liquid separator 3.
  • the magnetic separation tank 4 includes a stirring mechanism 41 and an electromagnet (magnetic separation mechanism) 42, and separates the filter aid and the solid matter while mixing and stirring, and collects and separates only the filter aid with the magnet 42.
  • the liquid collected from the filter aid is collected as concentrated water containing a high-concentration solid material, washed with the supplied wash water, and returned to the filter aid supply device 5.
  • the filter aid returned in this way is supplied again to the mixing tank 6 and is reused for producing a suspension for forming the precoat layer.
  • a simulated drainage containing 200 mg / L bentonite was prepared as the water to be treated. This was supplied to the treated water tank 2 and mixed. Moreover, the filter aid was supplied to the mixing tank 6 from the filter aid supply apparatus 5 filled with the filter aid A, and water was mixed, and the filter aid slurry was produced. This was supplied to the solid-liquid separator 3, and a precoat layer having an average thickness of 1 mm was produced on the filtration membrane 33. Then, when to-be-processed water was supplied from the treated water tank 2 to the solid-liquid separator 3, and it filtered, it has confirmed that 90% of the bentonite in filtered water (treated water) was removed.
  • Example 2 A test was conducted in the same manner as in Example 1 except that filter aid B was used instead of filter aid A.
  • the bentonite removal rate was 88%.
  • the water flow rate of the solid-liquid separator was 1.5 times that of Example 1, it could be operated without any problem, and the bentonite recovery rate was 99% or more.
  • Example 3 A test was conducted in the same manner as in Example 1 except that filter aid C was used instead of filter aid A. The removal rate of bentonite was 99% or more. Compared with Example 1, the water flow rate of the solid-liquid separator became almost 1/4, but it could be operated without any problem, and the bentonite recovery rate was 99% or more.
  • Example 4 A test was conducted in the same manner as in Example 1 except that filter aid D was used instead of filter aid A. The bentonite removal rate was 90%. Compared with Example 1, the water flow rate of the solid-liquid separator was almost the same, and the recovery rate of bentonite was 91%.
  • Example 5 A test was conducted in the same manner as in Example 1 except that filter aid F was used instead of filter aid A. The removal rate of bentonite was about 100%. Compared with Example 1, the water flow rate of the solid-liquid separator was almost the same, and the bentonite recovery rate was 96%.
  • Example 6 A test was conducted in the same manner as in Example 1 except that filter aid G was used instead of filter aid A. The bentonite removal rate was 98%. Compared with Example 1, the water flow rate of the solid-liquid separator was 1.5 times, and the recovery rate of bentonite was 90%.
  • Example 1 A test was conducted in the same manner as in Example 1 except that filter aid D was used instead of filter aid A.
  • the bentonite removal rate was 90%.
  • the water flow rate of the solid-liquid separator was about 80%, but the recovery rate of bentonite was 25%.
  • Example 7 An apparatus schematically shown in FIG. 5 was produced. Water to be treated containing bentonite as a solid is supplied to the mixed raw water tank 2A and temporarily received by the mixed raw water tank 2A. Further, the filter aid is supplied also from the filter aid supply device 5 to the mixed raw water tank 2A, and a mixed slurry of bentonite and filter aid is made. When this filter aid slurry is first sent to the solid-liquid separator 3, a deposited layer composed of the filter aid and bentonite is formed on the filter membrane 33. In this deposited layer, bentonite is trapped by the filter aid.
  • the filtrate (treated water) is a bentonite-removed liquid, it may be appropriately treated and drained, but it is also used as the separation water for the solid-liquid separator 3 and the washing water for the magnetic separation tank 4. Is possible.
  • a filter aid and a deposited bentonite layer (cake) are present in the filter membrane 33 in the solid-liquid separator 3.
  • peeling water is sprayed from the side of the filtration membrane 33 to peel the deposited layer (cake), and the peeled material is discharged to the magnetic separation tank 4.
  • the magnetic separation tank 4 includes a stirring mechanism 41 and a magnet 42 (magnetic separation mechanism), separates the filter aid and bentonite while mixing and stirring, and adsorbs and collects only the filter aid with the magnet 42.
  • the liquid collected from the filter aid is collected as concentrated water containing high-concentration bentonite, washed with the supplied wash water, and returned to the filter aid supply device 5.
  • the recovered filter aid was supplied to the mixing tank 6 and the same operation as described above was performed, but the recovered filter aid could be reused without any problem.
  • a simulated waste water containing 200 mg / L bentonite was prepared as the treated water. This was supplied to the mixing raw water tank 2A and mixed. Moreover, the filter aid was supplied to the mixed raw water tank 2A from the filter aid supply device 5 filled with the filter aid A so as to be 2000 mg / L, thereby preparing a slurry of the filter aid and bentonite. When this was supplied to the solid-liquid separator 3 and filtered on the filtration membrane 33, it was confirmed that 97% of bentonite in the filtrate (treated water) was recovered.
  • Example 8 A test was conducted in the same manner as in Example 1 except that filter aid H was used instead of filter aid A, cellulose particles having an average particle diameter of 50 ⁇ m and gear oil of the same amount were used instead of bentonite. The removal rate of cellulose was 100%. The cellulose recovery rate was 90%.
  • Example 2 A test was conducted in the same manner as in Example 8 except that filter aid E was used instead of filter aid H. Although the removal rate of cellulose was 100%, cellulose could not be separated from the magnetic material and cellulose could not be recovered.

Abstract

Un mode de réalisation de la présente invention concerne un procédé de traitement de l'eau. Ce procédé de traitement de l'eau comprend : un processus de préparation d'un assistant de filtration, qui contient des particules primaires de matériau magnétique ou leurs agrégats et un matériau de revêtement qui recouvre les particules primaires de matériau magnétique ou leurs agrégats et qui présente une tension superficielle critique (γc) inférieure ou égale à 22 × 10-3 N/m; un processus de mélange de l'assistant de filtration avec un milieu de dispersion, formant ainsi une suspension dans laquelle l'assistant de filtration est dispersé dans le milieu de dispersion; un processus de filtration de la suspension à travers une membrane de filtration de façon à former une précouche contenant l'assistant de filtration sur la membrane de filtration, puis passage de l'eau à traiter contenant des solides à travers la précouche et la membrane de filtration de manière à ce que les solides soient adsorbés et piégés par l'assistant de filtration dans la précouche, les solides étant ainsi séparés de l'eau à traiter; un processus de versement d'eau sur la précouche de façon à ce que la précouche soit séparée de la membrane de filtration, un mélange composé de la précouche séparée, des solides piégés dans la précouche et de l'eau versée dans la précouche étant ainsi obtenu; et un processus de séparation magnétique de l'assistant de filtration du mélange.
PCT/JP2012/073216 2012-01-23 2012-09-11 Procédé de traitement de l'eau et système de traitement de l'eau WO2013111372A1 (fr)

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