WO2005056175A1 - 多孔性成形体及びその製造方法 - Google Patents
多孔性成形体及びその製造方法 Download PDFInfo
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- WO2005056175A1 WO2005056175A1 PCT/JP2004/018659 JP2004018659W WO2005056175A1 WO 2005056175 A1 WO2005056175 A1 WO 2005056175A1 JP 2004018659 W JP2004018659 W JP 2004018659W WO 2005056175 A1 WO2005056175 A1 WO 2005056175A1
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- Prior art keywords
- molded body
- ion
- water
- column
- porous molded
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01J20/30—Processes for preparing, regenerating, or reactivating
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- 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
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- 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
- B01J20/3234—Inorganic material layers
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
- Y10T428/249975—Void shape specified [e.g., crushed, flat, round, etc.]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
- Y10T428/249978—Voids specified as micro
Definitions
- the present invention relates to a porous molded body, a method for producing the same, an application thereof, an apparatus using the same, and a method for operating the apparatus.
- the present invention relates to a porous molded body suitable for an adsorbent that selectively adsorbs and removes phosphorus, boron, arsenic, and fluorine ions contained in river water, treated sewage water, and industrial wastewater.
- Phosphorus is one of the causative substances of eutrophication, and regulations are getting stronger in closed waters. In addition, it is an element that is concerned about drought, and there is a need for technology to recover it from wastewater and reuse it.
- Boron is an indispensable element for the growth of a spot, but it is known that when it is present in excess, it will adversely affect plant growth. Furthermore, it has been pointed out that the presence of drinking water in the human body may cause health problems, particularly health problems such as reduced reproductive function.
- Arsenic is used for wastewater from non-ferrous metal mills, geothermal power plants, and groundwater in certain areas.
- arsenic include. It has been known for a long time about the toxicity of arsenic. It has the ability to accumulate in the body, and is said to cause chronic poisoning, weight loss, sensory injury, liver damage, skin deposition, skin cancer and the like.
- Fluorine is often abundant in wastewater from metal refinery, glass, electronic material industries, and the like. There is concern about the effects of fluorine on the human body, and it is known that excessive consumption may cause chronic fluorine poisoning such as patchy teeth, osteosclerosis, and thyroid disorders.
- a hydrous ferrite of Ti, Zr, or Sn is used, and a three-dimensional network structure made of polyurethane or polyacrylic acid resin using an appropriate binder.
- Those attached to the body are known (see Patent Document 1).
- This known adsorbent is obtained by adhering hydrous ferrite to a three-dimensional network structure using a binder, and the binding agent is a fine particle that exists on the surface of hydrous ferrite that is an adsorption substrate. Since the pores are blocked, the inherent ion exchange ability of the adsorption substrate is not fully exhibited, and the adsorption rate is slow. Moreover, since it has a large void, there is a problem that the amount of the adsorbed substrate supported in a unit volume is low. Also, the manufacturing method is complicated.
- Non-Patent Document 1 an adsorbent in which a hydrous cerium powder is supported on a polymer material is known (see Non-Patent Document 1). Although this adsorbent is porous, there is a thin film called a skin layer on the surface, so there is a drawback in that the diffusion rate of adsorption objects such as phosphorus and boron into the adsorbent becomes slow. .
- Patent Document 2 discloses an adsorbent in which an adsorbent substrate made of hydrous zirconium oxide is supported on a porous molded body made of cellulose later by an impregnation method. Since this adsorbent is supported later by the impregnation method, the adsorbent substrate flows out during repeated use due to its weak binding force.
- cellulose has a problem that when it is swelled in water and packed in a squeezing force ram, the molded body is compressed and the pressure loss increases.
- Cellulose is also degradable by living organisms, and there is a problem that it is difficult to adapt to water treatment in which miscellaneous microorganisms such as sewage are mixed in terms of durability in repeated use.
- Patent Document 1 Japanese Patent Laid-Open No. 9-187646
- Patent Document 2 JP 2002-38038 A
- the present invention is a porous molded body suitable for an adsorbent that can absorb and remove low-concentration phosphorus, boron, fluorine, arsenic, etc. contained in irrigation water and wastewater at high speed and has high durability. And a method of manufacturing the same, a device using the same, and a method of operating the device Objective.
- the present invention is as follows.
- a porous molded body having a communication hole opened on an outer surface comprising an organic polymer resin and an inorganic ion adsorbent
- porous molded article wherein an inorganic ion adsorbent is supported on the outer surface of the fibril and the inner void surface.
- the organic polymer resin contains at least one selected from the group consisting of ethylene vinyl alcohol copolymer (EVOH), polyacrylonitrile (PAN), polysulfone (PS), polyvinylidene fluoride (PVDF) force.
- EVOH ethylene vinyl alcohol copolymer
- PAN polyacrylonitrile
- PS polysulfone
- PVDF polyvinylidene fluoride
- n 1 to 4
- m 0.5-6
- ⁇ 0-3
- ⁇ is Ti, Zr, Sn, S c, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm,
- + represents a mixture.
- the inorganic ion adsorbent comprises at least one selected from the group consisting of activated alumina loaded with aluminum sulfate and activated carbon loaded with aluminum sulfate.
- the good solvent for the organic polymer resin is dimethyl sulfoxide (DMSO), N-methyl_2pyrrolidone (NMP), dimethylacetamide (DMAC), and dimethylformamide (D (MF)
- DMSO dimethyl sulfoxide
- NMP N-methyl_2pyrrolidone
- DMAC dimethylacetamide
- D (MF) dimethylformamide
- the molding method scatters an organic polymer resin, a good solvent of the organic polymer resin, an inorganic ion adsorbent, and a slurry mixed with a water-soluble polymer from a nozzle provided on the side surface of the rotating container.
- a crystallization tank, a crystallization apparatus equipped with an addition means for adding a crystallization agent, a stirring means, and a solid-liquid separation apparatus for solid-liquid separation of the precipitate generated in the crystallization tank were installed (20).
- the ion adsorption device according to any one of (24).
- the column was provided with a liquid feed means for feeding a P H conditioning liquid (20) ion-adsorbing device according to any one of (27).
- the pH of the porous molded body packed in the column can be adjusted (28)
- a ion-adsorbing device comprising pH adjusting tank, P H controller and the pH controller and communicates the dynamic to liquid injection pump, and pH adjusting solution feeding means, and a line that passed through the water in the pH adjustment tank to the column
- the above ion adsorption device adjusts the pH by repeatedly circulating a pH adjusting solution between the column and the pH adjusting tank.
- a method for treating ions comprising bringing the porous molded body according to any one of (13) and a liquid into contact with each other.
- a gas separation method comprising contacting the porous molded body according to any one of (13) and a gas.
- a porous adsorbent comprising the porous molded article according to any one of (13). The invention's effect
- the porous molded body of the present invention has high openability on the outer surface, the processing speed at which diffusion of the substance to be adsorbed into the molded body is fast is fast.
- the fibril carrying the adsorption substrate is also porous, even the adsorption substrate embedded in the fibril can function effectively as an adsorbent, and the contact efficiency with the substance to be adsorbed is extremely high. . Therefore, the adsorption capacity increases and the apparatus can be made compact.
- the organic polymer resin carrying the inorganic ion adsorbent of the present invention hardly swells in water, it is excellent in pressure resistance and durability in water treatment applications. Furthermore, since it is not degradable by living organisms, it is excellent in terms of durability in repeated use even in water treatment applications where miscellaneous microorganisms such as sewage are mixed.
- the water-soluble polymer does not block the active site by coating between the adsorption substrate and the supported fibril, the adsorption activity of the inorganic ion adsorbent is high and the ion adsorption performance is excellent. Furthermore, since the polymer chain of the water-soluble polymer exists on the surface of the fibril, the surface is hydrophilic and has excellent antifouling property.
- the molded body of the present invention has a porous structure having communication holes. Furthermore, the outer surface is excellent in the openability of the surface without the skin layer. Further, there is a void inside the fibril forming the communication hole, and at least a part of the void is opened on the surface of the fibril.
- the opening ratio of the outer surface of the molded article of the present invention refers to the ratio of the sum of the opening areas of all the holes in the area of the field of view when the surface is observed with a scanning electron microscope.
- the surface of the compact was observed at a magnification of 10,000, and the outer surface aperture ratio was measured.
- a preferable range of the surface opening ratio is 10 to 90%, and 15 to 80% is particularly preferable. If it is less than 10%, the diffusion rate of substances to be adsorbed, such as phosphorus and boron, into the inside of the molded body becomes slow. On the other hand, if it exceeds 90%, the molded body has insufficient strength, and a molded body having excellent mechanical strength can be realized. Have difficulty.
- the outer surface opening diameter of the molded article of the present invention is determined by observing the surface with a scanning electron microscope. If the hole is circular, use its diameter. If it is not circular, use the equivalent circle diameter of a circle with the same area.
- the preferred range of the surface opening diameter is 005 ⁇ m—100 ⁇ m, especially 0 ⁇ 01 ⁇ m—50 / im. Less than 0.005 ⁇ , compacts of adsorption target substances such as phosphorus and boron On the other hand, if the diffusion rate into the interior is slow, the strength of the molded product is insufficient.
- the molded body of the present invention has voids in the fibrils forming the communication holes, and at least a part of the voids are opened on the surface of the fibrils.
- the inorganic ion adsorbent is supported on the outer surface of the fibril and the void surface inside the fibril. Since the fibril itself is also porous, the inorganic ion adsorbent, which is the adsorption substrate loaded inside, can also come into contact with the adsorption target substance such as phosphorus boron, effectively functioning as an adsorbent. Ability to rub.
- the portion where the adsorption substrate is supported is also porous as described above, the fineness of the adsorption substrate, which has been a drawback of the conventional method of kneading the adsorption substrate and the binder, is known. It is possible to effectively use an adsorption substrate in which the adsorption site is less clogged with a binder.
- the fibril means a fibrous structure made of an organic polymer resin and forming a three-dimensionally continuous network structure on the outer surface and inside of the molded body.
- the void inside the fibril and the opening of the fibril surface are determined by observing the cut section of the molded body with a scanning electron microscope.
- Fig. 1 is an electron micrograph of the cut surface of the molded body observed at 5,000 times
- Fig. 2 is an electron micrograph of the cut surface of the molded body observed at 10,000 times.
- There is a void in the cross-section of the fibril and it is observed that the surface of the fibril is open.
- the inorganic ion adsorbent powder is supported on the outer surface of the fibril and the inner void surface.
- the thickness of the fibrinole is 0 ⁇ 01 111-50 / 1 111 preferred.
- the opening diameter of the fibril surface is preferably 0.001 111-5 111.
- a method of forming a porous material by immersing a mixture of a polymer and a good solvent of the polymer in a poor solvent and causing the polymer to gel by solvent exchange is called a wet phase separation method.
- the proportion of good solvent decreases, and as a result, microphase separation occurs, polymer globules form, grow, entangle and form fibrils, and the fibril gaps become communication holes.
- the determination of the compact structure (solidification) proceeds sequentially from the outer surface to the inner part due to the diffusion of the poor solvent into the inner part.
- a dense layer called a skin layer is generally formed on the surface of the molded body.
- the water-soluble polymer is dispersed and intervened between the polymer entanglements in the process of phase separation, so that the pores are mutually connected.
- the inside of the fibril becomes porous, and the fibril surface also opens.
- a molded body having no skin layer is obtained by opening holes on the outer surface of the molded body.
- the porous molded body of the present invention can use almost all of the adsorption capacity of the supported inorganic ion adsorbent and is highly efficient.
- the water-soluble polymer partially extends its molecular chain from the surface of the fibril as if it were a beard, the surface of the fibril is kept hydrophilic, and an antifouling effect from hydrophobic adsorption can be expected.
- the communicating holes preferably have a maximum pore diameter layer in the vicinity of the surface of the molded body.
- the maximum pore diameter layer refers to the largest portion in the pore diameter distribution of the communication holes extending from the surface of the molded body to the inside.
- the layer where the void exists is called the maximum pore size layer.
- the vicinity of the surface means the inner side up to 25% of the cut diameter of the molded body from the outer surface toward the center.
- adsorption target substances such as phosphorus and boron can be quickly taken into the molded body and removed from the treated water.
- the position of the maximum pore diameter and the maximum pore diameter layer is obtained by observing the surface and the cut surface of the molded body with a scanning electron microscope.
- For the hole diameter use the circle equivalent diameter if the hole is circular, or the equivalent circle diameter of a circle with the same area if it is not circular.
- the form of the molded body can take any form such as a particulate form, a thread form, a sheet form, a hollow fiber form, a cylindrical form, and a hollow cylindrical form.
- the method for forming the particulate molded body is not particularly limited, and examples thereof include a method in which a polymer solution is sprayed from 1 fluid nozzle or 2 fluid nozzle to solidify in a coagulation bath.
- the following rotary nozzle method is particularly preferable in that particles having a uniform particle size distribution can be obtained.
- a polymer solution an organic polymer resin, a good solvent for the organic polymer resin, an inorganic ion adsorbent, a water
- This is a method of forming droplets by scattering a mixed slurry of a conductive polymer.
- Nozzle diameter is preferably in the range of 0.1 mm-10 mm, more preferably in the range of 0.1 mm and 5 mm. If it is less than 0.1 mm, the droplets tend not to scatter, and if it exceeds 10 mm, the particle size distribution tends to be wide.
- Centrifugal force is expressed in terms of centrifugal acceleration and is preferably in the range of 5-1500G, more preferably in the range of 10-1000G. More preferably, it is in the range of 10-800G. If the centrifugal acceleration is less than 5G, the formation and scattering of droplets tend to be difficult, and if it exceeds 1000G, the polymer liquid tends to be discharged in a thread form, and the particle size distribution tends to be wide.
- a method of extruding a polymer solution from a spinneret or die having a corresponding shape and solidifying it in a poor solvent can be employed.
- the hollow fiber-like molded body can be similarly molded by using a spinning nozzle composed of an annular orifice.
- the cylindrical and hollow cylindrical molded bodies may be solidified in a poor solvent while being cut, or may be solidified into a filament and then cut later.
- the particle shape is reduced from the point of pressure loss, the effectiveness of the contact area, and the ease of handling when packed in a column or the like and passed through.
- spherical particles (not only spherical but may be elliptical) are preferable.
- the average particle size of the spherical molded body of the present invention is such that the particles are regarded as spherical and are measured by laser light. Is the mode diameter (most frequent particle diameter) of the sphere equivalent diameter obtained from the angular distribution of the scattered light intensity of diffraction.
- the preferred range of the average particle diameter is 100 to 2500 / im, particularly 200 to 2000 ⁇ m. If the average particle size is less than 100 ⁇ m, the pressure loss will increase when the column or tank is packed, and if the average particle size is more than 2500 xm, the surface area when packed in the column tank will be increased. It becomes small and processing efficiency tends to decrease.
- the porosity Pr (%) of the molded body of the present invention is defined as the weight Wl (g) when the molded body is wet, the weight W0 (g) after drying, and the specific gravity of the molded body as p.
- the weight when water is contained may be determined by spreading a molded product sufficiently wet with water on dry filter paper, removing excess moisture, and measuring the weight when containing water. Drying may be performed under vacuum at room temperature in order to eliminate moisture.
- the specific gravity of the molded body can be easily measured using a specific gravity bottle.
- the preferred porosity Pr (%) range is 50% -90%, especially 60-85% force. If it is less than 50%, the contact frequency between the adsorption target substance such as phosphorus and boron and the inorganic ion adsorbent as the adsorption substrate tends to be insufficient. If it exceeds 90%, the strength of the molded product tends to be insufficient.
- the ash content is the residue when the molded product of the present invention is baked at 800 ° C. for 2 hours.
- a preferable loading range is 30 to 95%, more preferably 40 to 90%, and particularly preferably 65 to 90%. If it is less than 30%, the contact frequency between the substance to be adsorbed, such as phosphorus and boron, and the inorganic ion adsorbent that is the adsorption substrate becomes insufficient, and if it exceeds 95% immediately, the strength of the molded product tends to be insufficient.
- the adsorbing substrate and the organic polymer resin are kneaded and molded, it is possible to obtain a molded body that maintains a large amount of support and has high strength.
- S is a specific surface area (m 2 / g) per unit weight of the molded body.
- the specific surface area is measured using the BET method after vacuum drying the molded body at room temperature.
- a preferred specific surface area range is 5 m 2 Zcm 3 —500 m 2 / cm 3 . If it is less than 5 m 2 Zcm 3 , the loading amount and adsorption performance of the adsorption substrate tend to be insufficient. If it exceeds 500 m 2 Zcm 3 , the strength of the molded product tends to be insufficient.
- the adsorption performance (adsorption capacity) of an inorganic ion adsorbent that is an adsorption substrate is often proportional to the specific surface area. If the surface area per unit volume is small, it is difficult to achieve high-speed processing with small adsorption capacity and adsorption performance when packed in a column or tank.
- the molded article of the present invention has a three-dimensional network structure that is porous and intricately intertwined with fibrils. Furthermore, since the fibril itself has voids, it has a feature that the surface area is large. Since this has an adsorption substrate (inorganic ion adsorbent) having a larger specific surface area, the surface area per unit volume is also increased.
- adsorption substrate inorganic ion adsorbent
- the method for producing a porous molded body of the present invention is characterized in that an organic polymer resin, a good solvent thereof, an inorganic ion adsorbent, and a water-soluble polymer are mixed and then molded and solidified in a poor solvent. And
- the good solvent used in the present invention is not particularly limited as long as it dissolves both the organic polymer resin and the water-soluble polymer.
- DMSO dimethyl sulfoxide
- NMP N-methyl_2pyrrolidone
- DMAC dimethylacetamide
- DMF dimethylformamide
- Examples of natural polymers include guar gum, locust bean gum, carrageenan, gum arabic, tragacanth, pectin, starch, dextrin, gelatin, casein, and collagen.
- Examples of the semi-synthetic polymer include methyl cellulose, ethyl cellulose, hydroxyethyl cellulose, ethyl hydroxyethyl cellulose, carboxymethyl starch, and methyl starch.
- examples of the synthetic polymer include polybutanol, polypyrrole pyrrolidone, polybutyl methyl ether, carboxybutyl polymer, sodium polyacrylate, and polyethylene glycols such as tetraethylene glycol and triethylene glycol.
- synthetic polymers are preferred in that they have biodegradability resistance.
- the content of the water-soluble polymer in the molded product of the present invention is expressed by the following formula when the weight of the molded product when dried is Wd (g) and the weight of the water-soluble polymer extracted from the molded product force is Ws (g). Value.
- the content of the water-soluble polymer depends on the type and molecular weight of the water-soluble polymer, but 0.001 to 10% is preferable, and more preferably 0.01 to 1%. If it is less than 001%, the effect is not necessarily sufficient to open the surface of the molded product. If it exceeds 10%, the polymer concentration becomes relatively thin and the strength may not be sufficient.
- the weight Ws of the water-soluble polymer in the molded body is measured as follows. First, after the dried molded body was pulverized with a mortar or the like, the water-soluble polymer was extracted from the pulverized product using a good solvent for the water-soluble polymer, and then the extract was evaporated to dryness and extracted. Obtain the weight of the water-soluble polymer. Furthermore, identification of the extracted evaporated and dried product and confirmation of the presence or absence of the water-soluble polymer remaining in the fibril and not extracted can be measured by infrared absorption spectrum (IR) or the like.
- IR infrared absorption spectrum
- the porous molded body of the present invention is dissolved in a good solvent for both the organic polymer resin and the water-soluble polymer, and then the inorganic ions are dissolved.
- a liquid obtained by removing the adsorbent by filtration can be prepared, and then the liquid can be analyzed using GPC or the like to quantify the content of the water-soluble polymer.
- the content of the water-soluble polymer can be appropriately adjusted depending on the molecular weight of the water-soluble polymer and the combination of the organic polymer resin and its good solvent. For example, when a water-soluble polymer having a high molecular weight is used, the entanglement of the molecular chain with the organic polymer resin becomes strong, and it becomes difficult to shift to the poor solvent side during molding, and the content can be increased.
- the inorganic ion adsorbent used in the present invention refers to an inorganic substance exhibiting an ion adsorption phenomenon.
- natural products include zeolite, montmorillonite, and various mineral substances
- synthetic compounds include metal oxides and insoluble substances. There are hydrous oxides.
- the former is represented by kaolin mineral with a single layer lattice of aluminosilicate, bilayered muscovite, sea green stone, Kanuma soil, pyrophyllite, talc, three-dimensional framework feldspar, and zeolite.
- the latter mainly consists of complex metal hydroxides, metal oxides, metal hydrated oxides, polyvalent metal acid salts, insoluble hexapolyacid salts, and insoluble hexocyanate salts.
- Examples of the composite metal hydroxide include a hydrated talcite compound represented by the following formula (III).
- M 2+ represents at least one divalent metal ion selected from the group consisting of Mg 2+ , Ni 2+ , Zn 2+ , Fe 2+ , Ca 2+ and Cu 2+.
- M 3+ represents at least one trivalent metal ion selected from the group consisting of Al 3+ and Fe 3+
- a n — represents an n-valent anion
- metal oxides include activated alumina, iron oxides such as FeO, Fe 0 and Fe 0, silica gel, etc.
- the metal hydrous oxide can be represented by the formula (I) or the formula (II). It is also possible to use formula (I), formula (II), or any combination of these.
- n 1 to 4
- m 0.5-6
- x 0 to 3.
- the formula (I) is a general formula of hydrated oxide, and the formula (II) is a mixture of hydrous ferrite and iron hydrated oxide.
- M is Ti, Zr, Sn, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Al, Cr, Co, Ga
- at least one metal selected from the group consisting of Fe, Mn, Ni, V, Ge, Nb, and Ta represents a mixture.
- Ti, Zr, Sn, and Ce are preferable in terms of adsorption capacity and resistance to dissolution in acids and alkalis.
- a mixture of the hydrous ferrite of formula (II) and the hydrated oxide of iron is preferable.
- the metal M of the hydrous ferrite of the formula (II) is Zr.
- hydrated oxide represented by the formula (I) include the following.
- the cerium hydrated oxide has the general formula
- mixture of the hydrous ferrite represented by the formula (II) and the hydrated oxide of iron include the following.
- the mixture of titanium hydrous ferrite and iron hydrated oxide has the general formula
- the mixture of tin hydrous ferrite and iron hydrated oxide has the general formula
- n 1 to 4
- m 0.5-6
- x is a number from 0 to 3
- n 1 to 4, m is 0.5-6, x is 0-3).
- the method for producing the hydrated oxide represented by the formula (I) is not particularly limited.
- the hydrated oxide is produced by the following method.
- a precipitate obtained by adding an alkali solution to an aqueous salt solution of metal hydrochloride, sulfate, nitrate or the like is filtered, washed, and dried. Drying is performed by air drying or by drying at about 150 ° C or lower, preferably about 90 ° C or lower for about 1 to 20 hours.
- the hydrated oxide represented by the formula (II) is a mixture of hydrated ferrite and iron hydrated oxide.
- the manufacturing method of this compound is not specifically limited, For example, it manufactures with the following methods. To a solution containing metal ions prepared by dissolving the metal salt, a ferrous salt equivalent to about 0.2 to 11 times moles of metal ions contained in this solution was added, and then alkali was added. To maintain the pH of the solution at about 6 or higher, preferably about 7-12. After this, if necessary, the temperature of the solution is adjusted to about 30-100 ° C, and then an oxidizing gas such as air, oxygen gas or ozone is blown in, or an oxidizing agent such as hydrogen peroxide is added.
- an oxidizing gas such as air, oxygen gas or ozone is blown in, or an oxidizing agent such as hydrogen peroxide is added.
- iron hydrated oxide means, for example, iron oxide hydrates such as FeO, Fe 0 and Fe 0 (monohydrate, dihydrate,
- the ratio of hydrous ferrite to hydrated iron oxide is such that the hydrous ferrite content is 24-100% by weight, preferably 50-99% by weight.
- Examples of the metal salt of titanium, zirconium, tin or cerium used in the above-mentioned production method include titanium tetrachloride (TiCl), titanium sulfate (Ti (SO)), titanyl sulfate (
- CeCl cerium nitrate (Ce (NO)), cerium sulfate (Ce (SO)), and the like.
- ferrous salts used as a solution of about 0.05 2.0 moles per liter.
- ferrous salts include ferrous sulfate (FeSO), ferrous nitrate (Fe (NO)), and ferrous chloride (FeCl).
- FeSO ferrous sulfate
- Fe ferrous nitrate
- FeCl ferrous chloride
- the These may also be hydrated salts such as FeSO 7 ⁇ .
- ferrous salts may be added in the form of a force solution usually added as a solid.
- alkali strength include sodium hydroxide, potassium hydroxide, calcium hydroxide, ammonia, sodium carbonate and the like. These are preferably used in an aqueous solution of about 520% by weight.
- oxidizing gas When oxidizing gas is blown, the time varies depending on the type of oxidizing gas, but it is usually about 110 hours.
- the oxidizing agent for example, hydrogen peroxide, sodium hypochlorite, potassium hypochlorite and the like are used.
- the particle size is smaller than 0.01 / m, the viscosity of the slurry increases during production, and it tends to be difficult to mold.
- it is larger than 100 / m, the specific surface area becomes smaller and the adsorption performance tends to decrease. It is in.
- the particle diameter of the inorganic ion adsorbent of the present invention is a mode diameter (most frequent particle diameter) of a sphere equivalent diameter obtained from an angular distribution of scattered light intensity of diffraction by laser light.
- a poor solvent for the method of the present invention are, for example, water or, Metanonore, alcohol such as ethanol, ethers, n - hexane, organic high such aliphatic hydrocarbons such as n- heptane
- a liquid that does not dissolve the molecular resin is used, but it is preferable to use water.
- the mixing ratio of the good solvent of the polymer resin and water is preferably 0-40%, more preferably 0-30%. If the mixing ratio exceeds 40%, the coagulation rate will slow down.
- Wastewater from chemical factories, food factories, fertilizer factories and sewage treatment plants is first temporarily stored in raw water storage tank 2 via raw water supply channel 1.
- the flow path 3 and the pump 4 are used to send to a membrane separation apparatus 5 which is a solid-liquid separation apparatus.
- the raw water from which the turbid components have been removed by the membrane separator 5 is stored in the pH adjustment tank 8 through the flow path 6.
- the water in which the turbid components in the wastewater are concentrated by the membrane separator 5 is returned from the circulation path 7 to the raw water storage tank 2.
- the pH adjustment tank 8 is adjusted to pH 2-7, which is a pH range suitable for phosphate ion adsorption, using the pH adjuster addition mechanism 9.
- the pH-adjusted raw water is sent to the column 12 via the pipe 10 and the pump 11.
- column 12 phosphate ions contained in the waste water are adsorbed in contact with the porous molded body of the present invention.
- the purified wastewater from which ions in the solution have been adsorbed and removed is temporarily stored in the treated water tank 14 via the flow path 13, and is neutralized by the pH adjuster addition mechanism 15 and then discharged.
- the ion adsorption apparatus of the present invention comprises a column 12 packed with the porous molded body of the present invention and a means for feeding liquid to the column.
- the column liquid feeding means such as a pump, a water head difference, suction, and watering.
- the solid-liquid separation device is not particularly limited, Examples thereof include a device, a sand filtration device, and a centrifugal dehydrator.
- a membrane separator is preferable in that a space-saving and clear filtrate can be obtained.
- Preferred membrane separation techniques include reverse osmosis membrane (RO), ultrafiltration membrane (UF), microfiltration membrane (MF) and the like.
- RO reverse osmosis membrane
- UF ultrafiltration membrane
- MF microfiltration membrane
- the form of the membrane is not limited to flat membranes, hollow fibers, pleats, spirals, tubes and the like.
- valve c and valve h are closed to stop the feed of raw water.
- valve g and the valve b are opened, and the treated water in the treated water tank 14 is fed from below the column 12 through the flow path 16 and the pump 17, and the porous molded body in the column 12 is expanded. And wash.
- the cleaning liquid is returned to the pH adjusting tank 8 through the flow path 18.
- the backwashing process is intended to wash turbid components, dirt, etc. accumulated in the porous molded body packed bed in the column. If the packed bed is fixed, air can be supplied simultaneously with the backwash water to loosen the fixed packed layer.
- the backwashing process is always performed in the direction opposite to the liquid feeding direction in the adsorption process.
- an operation to desorb the adsorbed ions is performed.
- an alkaline aqueous solution is used as the desorption liquid.
- the alkaline aqueous solution is preferably a sodium hydroxide aqueous solution in terms of cost and performance. That is, an aqueous solution of sodium hydroxide stored in the desorption liquid tank 19 is sent to the column 12 via the flow path 20 and the pump 21, and is brought into contact with the porous molded body to remove the adsorbed phosphate ions. It elutes into the aqueous sodium oxide solution and is stored in the crystallization tank 23 via the flow path 22.
- the sodium hydroxide aqueous solution from which phosphate ions are eluted in the desorption process is stored in the crystallization tank 23.
- the eluted phosphate ions are precipitated and recovered as calcium phosphate. That is, the calcium hydroxide slurry stored in the crystallization agent tank 24 is poured into the crystallization tank 23 through the channel 25 and the pump 26 into the sodium phosphate aqueous solution stored in the crystallization tank 23, and the agitator. Use 27 and stir to conduct a crystallization reaction to form calcium phosphate crystals. After the crystallization reaction, the cloudy liquid containing the crystallized calcium phosphate 28.
- the solution is sent to the membrane separation device 30 which is a solid-liquid separation device via the pump 29, and the solid-liquid separation is performed.
- the calcium phosphate slurry concentrated by solid-liquid separation is circulated to the crystallization tank 23 via the flow path 31.
- the calcium phosphate slurry concentrated in the crystallization tank 23 is discharged from the valve i and recycled as fertilizer.
- a clear alkaline aqueous solution (sodium hydroxide aqueous solution) obtained by solid-liquid separation of calcium phosphate is stored in the desorption liquid tank 19 via the flow path 32 and reused in the next desorption process.
- examples of the solid-liquid separation device include coagulation sedimentation, centrifugal dehydrator, belt press dehydrator, membrane separation device and the like.
- a membrane separator is preferable in that space saving and clear filtrate water can be obtained.
- a hollow fiber ultrafiltration membrane (UF) and a microfiltration membrane (MF) are preferable because of excellent contamination resistance and excellent stability of the amount of filtered water.
- the porous molded body in the column after the desorption step is alkaline, and if it remains as it is, the ability to adsorb phosphate ions in the raw water again is low. Therefore, an acidic aqueous solution is used to return the pH in the force ram to a predetermined value, that is, an activation treatment.
- the activation liquid (dilute sulfuric acid) in the pH adjustment tank 33 is sent to the column 12 via the flow path 34 and the pump 35, and is brought into contact with the porous molded body in the column to adjust the pH via the flow path 36. Circulate in tank 33. Since the activation liquid comes into contact with the porous molded body in the column 12 and becomes alkaline, it is stored in the activation liquid storage tank 38 using the pump 40 linked to the pH controller 37 installed in the pH adjustment tank 33.
- the activated solution (sulfuric acid solution) is sent to the pH adjustment tank 33 via the flow path 39 to control the pH to be acidic. Repeat this operation to adjust the pH in column 12 to the specified value. In order to increase the accuracy of pH control, the activation liquid may be stirred using a stirrer 41.
- a, d, e, and f also represent valves.
- a compact and closed phosphate ion adsorption treatment apparatus is constructed.
- liquids include drinking water, irrigation water, factory process water, river water, lake water, seawater, groundwater, sewage, factory wastewater, etc., activated sludge from sewage treatment plants and wastewater treatment facilities, Examples include desulfurization and flue gas treated water.
- the ions to be adsorbed by the porous molded body of the present invention are not particularly limited to anions and cations.
- anions phosphorus (phosphate ions), fluorine (fluoride ions), arsenic (arsenate ions, arsenite ions), boron (borate ions), iodine ions, chlorine ions, sulfate ions
- examples include ions of various organic acids such as nitrate ions, nitrite ions, and acetic acid.
- Examples of cations include sodium, potassium, calcium, cadmium, lead, chromium, cobalt, strontium, and cesium.
- P, B, F can be selected from various coexisting ions such as sewage and industrial wastewater. Suitable for removing ions such as As.
- inorganic ion adsorbents hydrated oxides of titanium, zirconium, tin; hydrous ferrites of titanium, zirconium, tin; It is preferable to select at least one selected from the group consisting of hydrous cerium oxide; hydrous lanthanum oxide; activated alumina; activated alumina loaded with aluminum sulfate; and activated carbon loaded with aluminum sulfate.
- porous molded body of the present invention When the porous molded body of the present invention is used as an adsorbent for water treatment, it is used by filling a column or an adsorption tower.
- the method of filling the column or adsorption tower and passing the water to be treated for contact can bring out the high contact efficiency characteristic of the porous molded body of the present invention.
- the column is a cylindrical container, and is provided with a solid-liquid separation means such as a plate or mesh so that the molded body does not flow out in at least one of the lower part and the upper part.
- the column material is not particularly limited, but includes stainless steel, FRP (reinforced plastic with glass fiber), glass, and various plastics.
- the inner surface can be made of rubber or fluororesin lining.
- the desorption operation and activation described later are performed. It is common to perform the operation at the same site where the adsorption operation is performed. However, if there is not enough space on site or the frequency of desorption is low, only the column can be removed from the system and replaced with a new column. The removed column can be separately removed and reused at a factory equipped with active facilities.
- the porous molded body of the present invention When the porous molded body of the present invention is used as an adsorbent for water treatment, it is preferable to provide means for solid-liquid separation of suspended substances in water as a pretreatment. By removing suspended substances in water in advance, it is possible to prevent clogging of the surface of the porous molded body and to sufficiently exhibit the adsorption performance of the porous molded body of the present invention.
- Preferred solid-liquid separation means includes coagulation sedimentation, sedimentation separation, sand filtration, and membrane separation.
- a membrane separation technique that has a small installation area and that provides clear filtrate water is preferable.
- Preferred membrane separation technologies include reverse osmosis membrane (R0), ultrafiltration membrane (UF), and microfiltration membrane (MF).
- R0 reverse osmosis membrane
- UF ultrafiltration membrane
- MF microfiltration membrane
- the form of the membrane is not limited to flat membranes, hollow fibers, pleats, spirals, tubes and the like.
- adsorption step of the present invention it is preferable to adsorb the ions to be adsorbed after adjusting the pH of the liquid to a suitable pH by a combination of the ions to be adsorbed and the inorganic ion adsorbent.
- the pH adjustment range when using hydrated zincite of dinoleconium as the inorganic ion adsorbent is in the range of pHl.5-10, more preferably PH 2-7.
- the pH adjustment range when hydrated cerium oxide or zirconium hydrated ferrite is used as the inorganic ion exchanger is in the range of pH 3-10. Yes, more preferably pH 58.
- the pH adjustment range when hydrated oxide of cerium oxide or hydrated zirconium ferrite is used for the inorganic ion exchanger is in the range of pH 1-17. Yes, more preferably pH25.
- the pH adjustment range when the cerium oxide hydrate is used as the inorganic ion exchanger is a pH range of 3-12, and more preferably pH 5-9. It is.
- the porous molded body of the present invention can adsorb an anion again by contacting with an aqueous alkali solution to desorb the adsorbed anions and then treating the adsorbent with an acidic aqueous solution ( Reuse). Reusing a porous molded body has the effect of reducing waste as well as reducing costs.
- the porous molded article of the present invention is excellent in durability, it is suitable for repeated use.
- the alkaline solution has a pH range of pHIO or higher, it can release anions, preferably pH12 or higher, more preferably pH13 or higher.
- the alkali concentration is in the range of 0.1 wt% -30 wt%, more preferably in the range of 0.5-20 wt%. 0. Less than lw t%, the desorption efficiency is low, 30wt. If it is higher than / o , the cost of alkali chemicals tends to increase.
- the flow rate of the alkaline aqueous solution is not particularly limited, but is usually preferably in the range of SV0.5-5 (hr- 1 ).
- the type of the alkaline aqueous solution is not particularly limited, but usually an aqueous sodium hydroxide solution, an aqueous potassium hydroxide solution, an inorganic alkali such as ammonium hydroxide, and organic amines are used. Of these, sodium hydroxide and potassium hydroxide are particularly preferred because of their high desorption efficiency.
- an alkaline aqueous solution is brought into contact with the porous molded body of the present invention that has adsorbed ions, ions are eluted in the alkaline solution,
- the alkali can be reused and the ions can be recovered as a precipitate.
- crystallization agent examples include metal hydroxides.
- metal hydroxides metal salts combine with anions such as phosphorus, boron, fluorine, and arsenic to form precipitates.
- hydroxide serves as an alkali source for the desorption liquid, a closed system can be obtained by collecting and recycling the regenerated liquid.
- Specific examples include sodium hydroxide, aluminum hydroxide, magnesium hydroxide, and calcium hydroxide.
- Inferiorly soluble precipitates that is, low-solubility and low-solubility precipitates, and polyhydric metal hydroxides Specifically, aluminum hydroxide, magnesium hydroxide, and calcium hydroxide are particularly preferred. In particular, calcium hydroxide is preferable in terms of cost.
- alkali when it exists as sodium phosphate, alkali can be recovered according to the following reaction formula. Furthermore, the crystallized calcium phosphate can be recycled into fertilizers.
- the amount of metal hydroxide added is not particularly limited, but is 14 to 14 equivalents of the target ion.
- the addition amount is less than equimolar, the precipitation removal efficiency is low, and when it exceeds 4 times the equivalent, the removal efficiency hardly changes and tends to be economically disadvantageous.
- the pH is preferably 6 or more. In consideration of collecting and reusing the alkaline aqueous solution, it is preferable to maintain the pH at 12 or more, preferably 13 or more. If the pH during the precipitation process is lower than 6, the solubility of the precipitate increases and the precipitation efficiency decreases.
- an inorganic flocculant such as aluminum sulfate or polyaluminum chloride or a polymer flocculant may be used in combination.
- the method for solid-liquid separation of the precipitate in the eluent of the present invention is preferably a membrane separation method.
- the membrane separation method is suitable for a closed system such as the present invention because it requires a small installation area and can provide clear filtered water.
- the porous molded body in the column after the desorption step is alkaline, and as it is, the ability to adsorb ions in the raw water again is low. Therefore, an acidic aqueous solution is used to return the pH in the column to a predetermined value, that is, an activation treatment.
- the acidic aqueous solution is not particularly limited, but an aqueous solution such as sulfuric acid and hydrochloric acid is used.
- the concentration should be about 0.001-10 wt%. 0. Less than 001 wt%, and a large amount of water volume is required by the end of activation. If it is thicker than 10 wt%, there is a risk of problems in handling acidic aqueous solutions.
- the flow rate is not particularly limited, but is usually preferably in the range of SV0.5-5-30 (hr-. If it is lower than SV0.5, the activation time tends to be long and inefficiency tends to increase. If it is larger, the contact time between the porous molded body and the acidic aqueous solution is shortened, and the activation efficiency tends to decrease.
- the most preferable method for the activation method is to circulate the active liquid between the column and the pH adjusting tank.
- the pH of the porous molded body in the column shifted to the alkali side by the desorption operation can be gently returned to the predetermined pH in consideration of the acid resistance of the inorganic ion adsorbent.
- iron oxide is known to be remarkably dissolved by acid at pH 3 or lower.
- the conventional activation method has a problem of dissolution of iron and the problem of iron, so there is only a method of treating with a thin acid having a pH of 3 or more.
- this method was not economically acceptable because it required a large volume of water.
- the activation method of the present invention is provided with a column and a pH adjusting tank and circulates the activation liquid, so that it can be activated while avoiding the pH range in which it is dissolved by an acid.
- the volume of water used for activation can be reduced, and the apparatus can be made compact.
- the flow rate at this time is usually selected within the range of SV1—SOO Oir— 1 ). More preferably, it is in the range of SV10-100. If it is lower than SV1, the activation time tends to be long and inefficient, and if it is larger than SV200, large pump power is required and it tends to be inefficient.
- This series of desorption and activation operations can be performed while the column is filled with the adsorbent.
- an alkaline aqueous solution, acidic water Regeneration can be easily performed by sequentially passing the solution through the column.
- the liquid flow direction may be either an upward flow or a downward flow.
- the porous molded article of the present invention is excellent in chemical resistance and strength, the ion adsorption performance hardly deteriorates even if this regeneration treatment is repeated several tens to several hundreds of times.
- the communication holes are developed in a three-dimensional network inside the molded body having a high opening on the surface of the molded body, and the fibrils forming the communication holes are also porous. Therefore, the contact efficiency is high.
- palladium or platinum when supported, it can be used as a freshness-preserving agent because it adsorbs ethylene.
- silver or copper when silver or copper is supported, it has a deodorizing effect because it can adsorb and decompose hydrogen sulfide, ammonia, methyl mercabtan, and odorous gases.
- the compact was observed with a scanning electron microscope (SEM) using an S-800 scanning electron microscope manufactured by Hitachi.
- the molded body is vacuum-dried at room temperature, and the dried molded body is added to isopropyl alcohol (IPA).
- IPA isopropyl alcohol
- the molded body was enclosed in a gelatin capsule having a diameter of 5 mm together with IPA and frozen in liquid nitrogen.
- the frozen molded body was cleaved with a carved sword.
- the cut molded body was selected as a microscope sample.
- the obtained SEM image is recognized as a grayscale image, and the threshold value is manually adjusted by dividing the dark portion as an opening and the light portion as a fibril, and dividing into an opening portion and a fibril portion. And the area ratio was calculated
- the particle sizes of the molded body and the inorganic ion adsorbent were measured with a laser diffraction / scattering particle size distribution measuring apparatus (LA-910 (trade name) manufactured by HORIBA). However, when the particle size was 1,000 ⁇ m or more, the longest diameter and the shortest diameter of the compact were measured using the SEM image, and the average value was taken as the particle size.
- LA-910 laser diffraction / scattering particle size distribution measuring apparatus
- Wa is the weight (g) of the ash content of the molded body
- Wd is the weight (g) when the molded body is dried.
- the specific surface area of the molded product of the present invention was determined from the following equation.
- Phosphorus concentration was measured using a phosphoric acid measuring device Phosfax 'Compact (trade name) manufactured by HACH. • Boron concentration measurement
- Ethylene butyl alcohol copolymer (EV ⁇ H, Nippon Synthetic Chemical Industry Co., Ltd., Soano Nore E3803 (trade name)) 10g, Polybul pyrrolidone (PVP, BASF Japan KK, Luvite c K30 Powder (trade name)) 10 g of dimethyl sulfoxide (DMS 0, Kanto Chemical Co., Inc.) 8 Og was dissolved by heating to 60 ° C. in a Separa flask to obtain a uniform polymer solution. To 100 g of this polymer solution, 92 g of the inorganic ion adsorbent powder prepared in Production Example 1 was added and mixed well to obtain a slurry.
- the resulting composite polymer slurry was heated to 40 ° C and supplied to the inside of a cylindrical rotating container with a 5 mm diameter nozzle on the side.
- the container was rotated, and the nozzle force liquid was generated by centrifugal force (15G).
- Drops were formed and discharged into a coagulation bath made of 60 ° C water to coagulate the composite polymer slurry. Further, washing and classification were performed to obtain a spherical molded body having an average particle size of 623 / m.
- Table 1 shows the physical properties.
- the molded body prepared in Example 1 was measured for the content of polybulurpyrrolidone (PVP), which is a water-soluble polymer, as follows.
- PVP polybulurpyrrolidone
- Example 1 the molded body prepared in Example 1 was vacuum-dried to determine the weight Wd (g). Next, dry The dried molded body was pulverized using a mortar. Next, the powdered rice cake was subjected to Soxhlet extraction using black mouth form to extract polyvinyl pyrrolidone. Next, the obtained extract was evaporated to dryness, and the weight Ws (g) of polyvinylpyrrolidone was measured.
- the water-soluble polymer content was determined from the following formula.
- the content of water-soluble polymer is 0.1. / 0 .
- Ethylene butyl alcohol copolymer (EVH, Nippon Synthetic Chemical Industry Co., Ltd., Sono Nore E3803) 10g, Polybul pyrrolidone (PVP, BASF Japan KK, Luvitec K30 Powder) 10g, Dimethyl sulfoxide (DMSO, Kanto Chemical) 80 g of Co., Ltd. was dissolved by heating to 60 ° C. in a Sepaflask to obtain a uniform polymer solution.
- a solution obtained by adjusting the pH to 7 with sulfuric acid was used as a model solution, that is, an adsorption stock solution.
- 8 ml of the molded body prepared in Example 1 and Example 2 was packed in a column (inner diameter 10 mm), and the above-mentioned adsorption stock solution was passed through at a rate of 240 ml / hr (SV30). Sampling the effluent (treatment solution) from the column every 30 minutes, and measuring the phosphate ion concentration (phosphorus concentration) in the treated water, 0.5 mg-PZ liter (ppm) The amount of water flow (adsorption amount) was determined. The results are shown in Table 1.
- Adsorption amount change rate (50th adsorption amount) / (1st adsorption amount) X 100
- Example 1 molded articles were obtained in the same manner except that polybulurpyrrolidone, which is a water-soluble polymer, was not used.
- Table 1 shows the physical properties. This molded body had a skin layer, had a surface opening ratio of 2%, and had a surface opening diameter of 0.01-0.55 / im and a poor surface opening property. In addition, voids inside the fibrils and pores on the fibril surface were not observed in this molded body.
- the phosphorus adsorption test was conducted in the same manner as in Example 3. The results are shown in Table 1. The amount of phosphorus adsorbed on SV30 was low and low.
- Adsorption desorption in a beaker using the same adsorption stock solution, desorption solution, and regeneration solution as in Example 3, The regeneration operation was repeated 50 times, and the rate of change in adsorption amount was determined, and it was found that the product prepared by the impregnation method as low as 50% had low durability.
- H BO Boric acid
- aqueous boric acid solution 22 mg—B / liter as boron
- Example 2 In the same manner as in Example 4, 2 ml of the porous molded body of Examples 1 and 2 was added to 1 liter of this aqueous solution, and the mixture was stirred with a mixer. Two hours after the start of stirring, the aqueous solution was sampled, and the fluoride ion concentration was measured to determine the adsorption amount. The results are shown in Table 2.
- Example 2 In the same manner as in Example 4, 2 ml of the porous molded body of Examples 1 and 2 was added to 1 liter of this aqueous solution, and the mixture was stirred with a mixer. Two hours after the start of stirring, the aqueous solution was sampled, and the arsenite ion concentration was measured to determine the adsorption amount. The results are shown in Table 2.
- Example 2 8 ml of the molded body prepared in Example 1 was packed in a column (inner diameter: 10 mm), and the previous adsorption stock solution was passed through at a rate of 80 ml / hr (SV10). Sampling the effluent (treatment solution) from the column every 30 minutes, measuring the phosphate ion concentration (phosphorus concentration) in the treated water, 0.1 mg
- FIG. 1 An embodiment of the water treatment apparatus of the present invention is shown in FIG. 1
- the solution was filtered through a membrane separator 5 (manufactured by Asahi Kasei Chemicals Co., Ltd., microfiltration membrane, nominal pore size 0.1 ⁇ m) using the channel 3 and the pump 4 and stored in the pH adjustment tank 8.
- a membrane separator 5 manufactured by Asahi Kasei Chemicals Co., Ltd., microfiltration membrane, nominal pore size 0.1 ⁇ m
- the 5 wt% sodium hydroxide aqueous solution stored in the desorption liquid tank 19 is sent to the column 12 through the flow path 20 and the pump 21 at 2 liter / hr (SVl) for 6 hours to form a porous molded body.
- the adsorbed phosphate ions were eluted into the aqueous sodium hydroxide solution and stored in the crystallization tank 23 via the flow path 22.
- the phosphate ion concentration in the crystallization tank 23 was 570 mg_P / liter. Next, the crystallization process will be described.
- the calcium hydroxide slurry stored in the crystallizing agent tank 24 is added to the sodium phosphate aqueous solution stored in the crystallizing tank 23 via the calcium hydroxide equivalent 3gZ liter, the flow path 25, and the pump 26.
- the mixture was stirred for 20 hours using a stirrer 27, and a crystallization reaction was performed to form calcium phosphate crystals.
- the cloudy liquid containing the crystallized calcium phosphate is passed through the flow path 28 and the pump 29 through a membrane separator 30 (Asahi Kasei Chemicals Corporation, ultrafiltration membrane, nominal molecular weight 6, 000) and separated into solid and liquid.
- the aqueous sodium hydroxide solution has a phosphate ion concentration of 10 mg—P / liter, calcium.
- the muon concentration was 1 mg_Ca / liter.
- the calcium phosphate slurry concentrated by solid-liquid separation is circulated to the crystallization tank 23 via the flow path 31.
- the calcium phosphate slurry concentrated in the crystallization tank 23 was discharged from the valve i. Next, the activation process will be described.
- the pH adjusting tank 33 activated solution adjusted to P H3 with sulfuric acid was prepared 10 liters.
- the liquid is fed to the column 12 through the flow path 34 and the pump 35 at 120 liter / hr (SV60), is contacted with the porous molded body in the column, and is circulated through the flow path 36 to the pH adjustment tank 33. It was. Since the activation liquid comes into contact with the porous molded body with force ram 12 and becomes alkaline, it is stored in the activation liquid storage tank 38 using the pump 40 linked with the pH controller 37 installed in the pH adjustment tank 33.
- the 5 Owt% sulfuric acid aqueous solution was fed to the pH storage tank 33 via the flow path 39 and controlled in the pH 3-5 range.
- the molded body of the present invention is excellent in the surface opening property without the skin layer, it can be applied to the interior of the molded body.
- Material diffusion is fast. Therefore, it is suitable for adsorbents and filter agents, deodorants, antibacterial agents, hygroscopic agents, food freshness-preserving agents, various chromatographic carriers, catalysts and the like used for liquid and gas treatment.
- FIG. 3 is an electron micrograph (magnification 150 times) showing a cut section of the molded body of Example 1.
- FIG. 5 is an electron micrograph (magnification 10,000 times) showing a cut section of the molded body of Example 1.
- FIG. 11 shows a water treatment apparatus showing Example 8 of the present invention.
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Abstract
Description
Claims
Priority Applications (5)
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EP04807018.9A EP1695760B1 (en) | 2003-12-15 | 2004-12-14 | Porous formed article and method for production thereof |
US10/582,339 US8597778B2 (en) | 2003-12-15 | 2004-12-14 | Porous formed article and method for production thereof |
CN2004800373980A CN1894029B (zh) | 2003-12-15 | 2004-12-14 | 多孔成形物及其生产方法 |
JP2005516232A JP4671419B2 (ja) | 2003-12-15 | 2004-12-14 | 多孔性成形体及びその製造方法 |
IL176150A IL176150A (en) | 2003-12-15 | 2006-06-06 | Porous formed article and method for production thereof and ion-adsorbing device containing said porous article |
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EP (1) | EP1695760B1 (ja) |
JP (1) | JP4671419B2 (ja) |
KR (1) | KR100804360B1 (ja) |
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Cited By (44)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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EP1695760B1 (en) | 2020-01-01 |
EP1695760A1 (en) | 2006-08-30 |
IL176150A (en) | 2011-07-31 |
EP1695760A4 (en) | 2011-04-13 |
US20070128424A1 (en) | 2007-06-07 |
CN1894029B (zh) | 2011-05-11 |
JPWO2005056175A1 (ja) | 2007-07-05 |
CN1894029A (zh) | 2007-01-10 |
US8597778B2 (en) | 2013-12-03 |
KR100804360B1 (ko) | 2008-02-15 |
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KR20060103447A (ko) | 2006-09-29 |
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