WO2010013677A1 - 有機物含有水の処理方法及び装置 - Google Patents
有機物含有水の処理方法及び装置 Download PDFInfo
- Publication number
- WO2010013677A1 WO2010013677A1 PCT/JP2009/063352 JP2009063352W WO2010013677A1 WO 2010013677 A1 WO2010013677 A1 WO 2010013677A1 JP 2009063352 W JP2009063352 W JP 2009063352W WO 2010013677 A1 WO2010013677 A1 WO 2010013677A1
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- WIPO (PCT)
- Prior art keywords
- water
- hydrogen
- group metal
- platinum group
- organic substance
- Prior art date
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 232
- 239000005416 organic matter Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims description 62
- 230000008569 process Effects 0.000 title description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 115
- 229910052751 metal Inorganic materials 0.000 claims abstract description 98
- 239000002184 metal Substances 0.000 claims abstract description 98
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 95
- 239000001257 hydrogen Substances 0.000 claims abstract description 92
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 92
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000001301 oxygen Substances 0.000 claims abstract description 50
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 50
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 93
- 239000000126 substance Substances 0.000 claims description 72
- 238000001179 sorption measurement Methods 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 29
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 26
- 239000003957 anion exchange resin Substances 0.000 claims description 16
- 239000003729 cation exchange resin Substances 0.000 claims description 8
- 238000007872 degassing Methods 0.000 claims description 8
- 239000010419 fine particle Substances 0.000 claims description 7
- 238000005342 ion exchange Methods 0.000 claims description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
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- 238000000354 decomposition reaction Methods 0.000 description 10
- 230000003197 catalytic effect Effects 0.000 description 7
- 229910052697 platinum Inorganic materials 0.000 description 7
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
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- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
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- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
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- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
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- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910001252 Pd alloy Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
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- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
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- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
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- 239000011368 organic material Substances 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
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- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/0031—Degasification of liquids by filtration
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/13—Use of sweep gas
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- B01J35/23—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
-
- 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
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
-
- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/727—Treatment of water, waste water, or sewage by oxidation using pure oxygen or oxygen rich gas
-
- 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
- C02F2001/422—Treatment of water, waste water, or sewage by ion-exchange using anionic exchangers
-
- 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
- C02F2001/425—Treatment of water, waste water, or sewage by ion-exchange using cation exchangers
-
- 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
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/02—Non-contaminated water, e.g. for industrial water supply
- C02F2103/04—Non-contaminated water, e.g. for industrial water supply for obtaining ultra-pure water
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/08—Nanoparticles or nanotubes
Definitions
- the present invention relates to a method and apparatus for treating organic substance-containing water, and more particularly to a method and apparatus for removing organic substances in water to be treated with a metal catalyst.
- High-concentration chemicals and detergents are used for cleaning and surface treatment of electronic components, and a large amount of pure water is used to rinse them. Development of advanced water treatment technology is desired in order to improve the quality of pure water and the reuse rate of waste water.
- Biological treatment or physicochemical treatment is widely used as a method for removing the TOC (total organic carbon) component in the treated water in the ultrapure water production process.
- RO membrane reverse osmosis membrane
- the physicochemical treatment includes the following methods (1) to (3).
- the above methods (1) to (3) have a problem that energy consumption is large.
- the driving power of the pressurizing pump for supplying water to the RO membrane separation device is large.
- organic matter-containing wastewater is directly passed through the RO membrane separator, biofiling tends to occur in the RO membrane separator because the organic matter-containing wastewater has a high TOC concentration.
- the organic matter in the organic matter-containing wastewater is a hardly decomposable organic matter typified by a nitrogen compound having a low molecular weight (such as urea), the removal efficiency is extremely poor.
- An object of the present invention is to provide a method and apparatus for treating organic substance-containing water that can remove organic substances in water to be treated with low energy consumption.
- the method for treating organic substance-containing water according to the first aspect of the present invention is characterized in that water to be treated containing an organic substance is brought into contact with a platinum group metal catalyst to remove the organic substance.
- the method for treating organic substance-containing water according to the second aspect is characterized in that, in the first aspect, the platinum group metal catalyst adsorbs hydrogen.
- the method for treating organic substance-containing water according to the third aspect is characterized in that, in the second aspect, the water to be treated contains dissolved oxygen.
- the method for treating organic substance-containing water of the fourth aspect is the hydrogen adsorption step of supplying hydrogen to the platinum group metal catalyst and adsorbing hydrogen in the second or third aspect, and the platinum group adsorbing the hydrogen.
- An organic substance removing step of contacting the water to be treated with a metal catalyst to remove organic substances is performed alternately.
- a fifth aspect of the method for treating organic substance-containing water when a plurality of reaction vessels containing the platinum group metal catalyst are used and a hydrogen adsorption step is performed in some of the reaction vessels, An organic substance removing step is performed in the container.
- the organic substance-containing water treatment method of the sixth aspect is characterized in that, in any of the first to fifth aspects, the platinum group metal catalyst is composed of fine particles of a platinum group metal.
- the organic material-containing water treatment method of the seventh aspect is characterized in that, in the sixth aspect, the platinum group metal fine particles are supported on a carrier.
- the organic substance-containing water treatment method according to the eighth aspect is characterized in that, in any one of the third to seventh aspects, the dissolved oxygen concentration in the water to be treated is 1 ppb to 100 ppb.
- the method for treating organic substance-containing water according to the ninth aspect is the method according to any one of the first to eighth aspects, wherein after the water to be treated is brought into contact with the platinum group metal catalyst, the water is treated with an anion exchange resin and a cation. Contact with at least one of the exchange resins.
- the method for treating organic substance-containing water according to the tenth aspect is the method according to the ninth aspect, wherein the water to be treated is brought into contact with the platinum group metal catalyst, then the water is degassed, and then the degassed water is treated with an anion. It is characterized by contacting with at least one of an exchange resin and a cation exchange resin.
- the organic substance-containing water treatment method of the eleventh aspect is characterized in that, in any of the first aspect to the tenth aspect, the water to be treated is water to be treated for producing ultrapure water.
- the organic substance-containing water treatment apparatus is an apparatus for removing organic substances by bringing water to be treated containing organic substances and dissolved oxygen into contact with a platinum group metal catalyst adsorbing hydrogen.
- the present invention is characterized in that water to be treated is supplied to a reaction vessel other than the reaction vessel to perform the organic substance removing step.
- the treatment apparatus for organic substance-containing water comprises, in the twelfth aspect, an ion exchange means having at least one of an anion exchange resin and a cation exchange resin into which the treated water flowing out of the reaction vessel is introduced.
- the treatment apparatus for organic substance-containing water includes a deaeration device into which the treated water that has flowed out of the reaction vessel is introduced, and the deaeration treatment water from the deaeration device is the ion. It is introduced into the exchange means.
- water to be treated containing an organic substance is brought into contact with a platinum group metal catalyst, and the organic substance is removed by the catalytic action of the platinum group metal catalyst. It can be easily removed at low energy.
- RO membrane treatment and UV irradiation treatment are unnecessary, and energy consumption is small.
- the platinum group metal catalyst adsorbs hydrogen and the water to be treated contains dissolved oxygen, the organic substance removal efficiency is improved.
- the dissolved oxygen concentration in to-be-processed water is 1 ppb or more.
- a hydrogen adsorption step of supplying hydrogen to a platinum group metal catalyst to adsorb hydrogen, and bringing the water to be treated into contact with the platinum group metal catalyst having adsorbed hydrogen to treat the organic substance. It is preferable to alternately perform the organic substance removing step to be removed. Thereby, hydrogen can be sufficiently adsorbed to the platinum group metal catalyst, and the organic matter removal efficiency can be increased.
- the platinum group metal catalyst is accommodated in a plurality of reaction vessels, and while performing the hydrogen adsorption step in some reaction vessels, the organic substance removal step is performed in another reaction vessel, and this You may make it switch the reaction container which performs a hydrogen adsorption process sequentially. If it does in this way, the removal process of the organic substance in to-be-processed water can be implemented continuously.
- the platinum group metal catalyst may be composed of fine particles of platinum group metal.
- the platinum group metal fine particles may be supported on the surface of the carrier.
- the platinum group metal catalyst may be formed by forming a coating of a platinum group metal such as platinum on a substrate such as a ceramic ball by plating or the like.
- this water may be brought into contact with at least one of an anion exchange resin and a cation exchange resin. If it does in this way, the organic acid produced
- the present invention is suitable for treating raw water for producing ultrapure water, for example, city water, well water, surface water, waste water from a drawing process for semiconductors or electronic components, and the like.
- the present invention is suitable for the treatment of raw water having an organic substance concentration of 1 to 1000 ppb, particularly 1 to 50 ppb as TOC.
- FIG. 1 is a system diagram showing an embodiment of the method and apparatus for treating organic substance-containing water of the present invention.
- the open / close valve in the closed state is painted black, and the open / close valve in the open state is white.
- the configuration of the processing apparatus will be described.
- a raw water supply pipe 1 having an on-off valve 1 a is connected to an inlet of a catalyst packed column (reaction vessel) 4.
- a catalyst packed column (reaction vessel) 4 In the middle of the raw water supply pipe 1, an oxygen supply pipe 2 provided with an on-off valve 2a and a hydrogen supply pipe 3 provided with an on-off valve 3a are connected.
- a platinum group metal catalyst 4a is accommodated (packed in the present embodiment). Hydrogen is adsorbed on the platinum group metal catalyst 4a. Details of the catalyst packed column 4 will be described later.
- the outlet of the catalyst packed column 4 is connected to the liquid phase chamber 6a of the degassing membrane module 6 via an outflow pipe 5 provided with an on-off valve 5a. From the middle of the outflow pipe 5, an extraction pipe 12 provided with an on-off valve 12 a is branched.
- the deaeration membrane module 6 is partitioned into a liquid phase chamber 6a and a gas phase chamber 6b by a gas permeable membrane 6c.
- the gas phase chamber 6 b is connected to the vacuum pump 11 via the pipe 10.
- the gas permeable film 6c is a film that transmits gas such as oxygen, nitrogen, carbon dioxide, and water vapor but does not transmit water.
- a silicone film, a polytetrafluoroethylene film, a polyolefin film, a polyurethane film, and the like. can be used.
- the pressure on the decompression side (gas phase chamber 6b) of the membrane degassing module 6 is preferably 5 to 10 kPa. Since some water vapor passes through the gas permeable membrane 6c on the decompression side, it is preferable to flow a gas such as nitrogen on the decompression side to remove moisture and prevent deterioration of the membrane performance. If the pressure on the decompression side is less than 5 kPa, the amount of water vapor that passes through the gas permeable membrane 6c may be excessive. If the pressure on the decompression side exceeds 10 kPa, the gas removal efficiency may be reduced.
- the flow rate of a gas such as nitrogen in the gas phase chamber 6b is preferably 5 to 25% by volume of the amount of water flowing into the liquid phase chamber 6a.
- the liquid phase chamber 6 a of the degassing membrane module 6 is connected to the inlet of the ion exchange resin column 8 via the pipe 7.
- the ion exchange resin column 8 is filled with an ion exchange resin 8a.
- the ion exchange resin column 8 is preferably a non-regenerative mixed bed ion exchange apparatus in which a strongly acidic cation exchange resin and a strongly basic anion exchange resin are mixed and packed in accordance with the ion load as the ion exchange resin 8a.
- a mixed bed type ion exchange apparatus By using a mixed bed type ion exchange apparatus, cations and anions in water are completely removed, and ultrapure water having extremely low electrical conductivity can be obtained.
- residual organic substances and organic acids generated in the decomposition process of the organic substances are also removed.
- a treated water pipe 9 is connected to the outlet of the ion exchange resin column 8.
- platinum group metal of the platinum group metal catalyst 4a packed in the catalyst packed column 4 examples include ruthenium, rhodium, palladium, osmium, iridium and platinum. These platinum group metals can be used individually by 1 type, and can also be used in combination of 2 or more type. It can also be used as an alloy made of two or more metals. Moreover, the refined product of the mixture produced naturally can also be used without isolate
- the platinum group metal catalyst 4a may be platinum group metal fine particles or a metal supported catalyst in which platinum group metal nanocolloid particles are supported on the surface of the carrier.
- the platinum group metal catalyst may be formed by forming a coating of a platinum group metal such as platinum on a substrate such as a ceramic ball by plating or the like.
- the method for producing platinum group metal nanocolloid particles includes a metal salt reduction reaction method and a combustion method.
- the metal salt reduction reaction method can be suitably used because it is easy to produce and stable metal nanocolloid particles can be obtained.
- platinum group metal chloride such as platinum, nitrate, sulfate, metal complex, etc., alcohol, citric acid or a salt thereof
- a reducing agent such as formic acid, acetone, acetaldehyde and the like
- platinum group metal nanocolloid particles can be produced.
- a reducing agent such as ethanol, and heating and refluxing in a nitrogen atmosphere for 2 to 3 hours
- platinum Nanocolloid particles can be produced.
- the weight average particle diameter of the platinum group metal nanocolloid particles is preferably 1 to 50 nm, more preferably 1.2 to 20 nm, and still more preferably 1.4 to 5 nm. If the weight average particle diameter of the metal nanocolloid particles is less than 1 nm, the catalytic activity for TOC decomposition and removal may be reduced. When the weight average particle diameter of the metal nanocolloid particles exceeds 50 nm, the specific surface area of the nanocolloid particles becomes small, and the catalytic activity for TOC decomposition and removal may be reduced.
- the carrier on which the platinum group metal nanocolloid particles are supported examples thereof include magnesia, titania, alumina, silica-alumina, zirconia, activated carbon, zeolite, diatomaceous earth, and ion exchange resin.
- an anion exchange resin can be particularly preferably used.
- the platinum group metal nano-colloidal particles have an electric double layer and are negatively charged, so that they are stably supported on the anion exchange resin and hardly peeled off.
- This anion exchange resin is preferably a strongly basic anion exchange resin based on a styrene-divinylbenzene copolymer, and more preferably a gel type resin.
- the exchange group of the anion exchange resin is preferably in the OH form.
- the amount of platinum group metal nanocolloid particles supported on a carrier such as an anion exchange resin is preferably 0.01 to 0.2% by weight, more preferably 0.04 to 0.1% by weight. . If the supported amount of metal nanocolloid particles is less than 0.01% by weight, the catalytic activity for the decomposition and removal of organic substances may be insufficient. The supported amount of the metal nanocolloid particles is 0.2% by weight or less, and sufficient catalytic activity is exhibited for the decomposition and removal of the organic matter. Usually, it is not necessary to support the metal nanocolloid particles exceeding 0.2% by weight. In addition, when the amount of metal nanocolloid particles supported increases, the risk of metal elution into water also increases.
- the on-off valves 1a and 5a are opened, the on-off valves 3a and 12a are closed, and raw water is passed through the raw water supply pipe 1.
- the on-off valve 2a of the oxygen supply pipe 2 is opened to supply oxygen to the raw water in the raw water supply pipe 1.
- the supply amount of oxygen is such that the decomposition reaction of the organic matter in the raw water can sufficiently proceed.
- the total molar concentration of dissolved oxygen in the raw water and oxygen supplied from the oxygen supply pipe 2 is preferably one or more times the molar concentration of organic carbon in the raw water. Is more preferably 5 times or more in order to sufficiently proceed.
- the dissolved oxygen concentration of water introduced into the catalyst packed column 4 is preferably 1 ppb or more, for example, 1 to 100 ppb, particularly 5 to 50 ppb.
- the raw water containing organic matter and dissolved oxygen flows into the catalyst packed column 4 through the raw water supply pipe 1 and comes into contact with the platinum group metal catalyst 4a on which hydrogen is adsorbed. Thereby, the organic substance in the raw water and the platinum group metal catalyst come into contact with each other in the presence of hydrogen and oxygen, and the organic substance is efficiently decomposed and removed.
- the platinum group metal catalyst 4a is an anion exchange resin carrying 0.01 to 0.2% by weight of platinum group metal non-nano colloidal particles
- the water flow rate (SV) to the catalyst packed column 4 is 10 to 10%.
- 500 hr -1, especially about 50 ⁇ 300 hr -1 is preferred.
- the water from which organic substances have been removed in this way flows into the liquid phase chamber 6a of the degassing membrane module 6 through the pipe 5, and carbon dioxide, oxygen, nitrogen, and other gases are removed.
- the degassed water deaerated by the deaeration membrane module 6 flows into the ion exchange resin column 8 through the pipe 7.
- the ion exchange resin 8a in the ion exchange resin column 8 adsorbs and removes undecomposed organic matter contained in the degassed treated water, organic acids generated during the decomposition process of the organic matter, and the like.
- the ion exchange treated water is discharged out of the system from the pipe 9.
- Whether or not the hydrogen adsorption amount of the platinum group metal catalyst has decreased is determined by, for example, measuring the dissolved oxygen concentration of the inflow water and the outflow water to the catalyst packed column 4 and whether or not the difference in concentration is equal to or less than a predetermined value. Can be determined. That is, if the difference between the dissolved oxygen concentration of the inflowing water and the dissolved oxygen concentration of the effluent of the catalyst packed column 4 is not more than a predetermined value, the hydrogen adsorption amount is sufficient and the dissolved oxygen is removed by the reaction with hydrogen. On the contrary, when the value exceeds the predetermined value, the hydrogen adsorption amount is insufficient.
- the on-off valve 3 a is opened, hydrogen is introduced into the catalyst packed column 4 through the pipe 3 and the pipe 1, and hydrogen is adsorbed on the platinum group metal catalyst 4 a in the column 4.
- the on-off valve 12a may be closed and the inside of the catalyst packed column 4 may be pressurized to promote hydrogen adsorption.
- the on-off valve 12a may be opened so that hydrogen from the column 4 is discharged from the pipe 12 so that hydrogen flows through the catalyst packed column 4.
- the on-off valve 3a After sufficiently adsorbing hydrogen onto the platinum group metal catalyst 4a, the on-off valve 3a is closed, and the on-off valves 1a, 2a and 12a are opened to fill the catalyst packed column 4 with raw water.
- the on-off valve 12a is closed, the on-off valve 5a is opened, and the valve is opened and closed as shown in FIG. 1, and the process returns to the organic matter removing step.
- the above embodiment is an example of the present invention, and the present invention is not limited to the above embodiment.
- the hydrogen adsorption step may be omitted, and the platinum group metal catalyst 4a may be replaced with a new one when the amount of hydrogen adsorption of the platinum group metal catalyst 4a is reduced.
- hydrogen water may be supplied from the hydrogen supply pipe 3 instead of the hydrogen gas.
- the hydrogen water for example, treated water from the treated water pipe 9 or water in which TOC concentration is lower than that of the treated water is used.
- Oxygen water may be supplied from the oxygen supply pipe 2 instead of oxygen gas.
- oxygen water for example, treated water from the treated water pipe 9 or one in which oxygen is dissolved in water having a lower TOC concentration than the treated water is used.
- FIG. 2 is a system diagram showing another embodiment of the method and apparatus for treating organic substance-containing water of the present invention.
- the open / close valve in the closed state is painted black, and the open / close valve in the open state is white.
- two catalyst-packed columns are installed in parallel, and the treatment of water to be treated can be continuously performed by changing the timing of performing the hydrogen adsorption process of these catalyst-filled columns. It is what.
- the raw water supply pipe 20 branches into a branch pipe 21 having an on-off valve 21a and a branch pipe 22 having an on-off valve 22a.
- the branch pipes 21 and 22 are connected to the inlets of the catalyst packed columns 41 and 42.
- One end side of an oxygen water pipe 23 having an on-off valve 23 a is connected to the middle part of the raw water supply pipe 20, and the other end side of the pipe 23 is connected to the liquid phase chamber 50 a of the oxygen dissolving membrane module 50.
- the oxygen-dissolving membrane module 50 is partitioned into a liquid phase chamber 50a and a gas phase chamber 50b by a gas permeable membrane 50c.
- An oxygen gas supply pipe 51 and a discharge pipe 52 including a vacuum pump 53 are connected to the gas phase chamber 50b.
- the oxygen water pipe 23 having the on-off valve 23a is connected to the liquid phase chamber 50a, to which the water supply pipe 54 is connected.
- treated water from the treated water pipe 9 described later or water having a lower TOC concentration than the treated water is supplied.
- Oxygen water is produced by the oxygen dissolving membrane module 50 as follows. Oxygen gas is supplied from the oxygen gas supply pipe 51 to the gas phase chamber 50b, and water is supplied from the water supply pipe 54 to the liquid phase chamber 50a. Part of the oxygen gas supplied into the gas phase chamber 50b permeates the gas permeable membrane 50c and dissolves in the water in the liquid phase chamber 50a. The remainder of the oxygen gas in the gas phase chamber 50b is sucked by the vacuum pump 53 and discharged from the discharge pipe 52 together with the water vapor and its condensed water that have permeated the gas permeable membrane 50c from the liquid phase chamber 50a. Oxygen water in the liquid phase chamber 50 a is supplied to the raw water supply pipe 20 through the oxygen water pipe 23.
- the inside of the hydrogen dissolution membrane module 60 is partitioned into a liquid phase chamber 60a and a gas phase chamber 60b by a gas permeable membrane 60c.
- a hydrogen gas supply pipe 61 and a discharge pipe 62 are connected to the gas phase chamber 60b.
- a water supply pipe 64 and a hydrogen water pipe 30 are connected to the liquid phase chamber 60a.
- the hydrogen water pipe 30 is branched into a branch pipe 31 having an on-off valve 31a and a branch pipe 32 having an on-off valve 32a.
- the branch pipes 31 and 32 are connected to the branch pipes 21 and 22 of the raw water supply pipe 20.
- treated water from the treated water pipe 9 described later or water having a lower TOC concentration than the treated water is supplied.
- Hydrogen water is produced by the hydrogen-dissolving membrane module 60 as follows. Hydrogen gas is supplied from the hydrogen gas supply pipe 61 to the gas phase chamber 60b, and water is supplied from the water supply pipe 64 to the liquid phase chamber 60a. Part of the hydrogen gas supplied into the gas phase chamber 60b permeates the gas permeable membrane 60c and dissolves in the water in the liquid phase chamber 60a. The remainder of the hydrogen gas in the gas phase chamber 60b is discharged from the discharge pipe 62 together with the water vapor and its condensed water that have permeated the gas permeable membrane 60c from the liquid phase chamber 60a. The hydrogen water in the liquid phase chamber 60 a is supplied to the branch pipes 21 and 22 of the raw water supply pipe 20 through the hydrogen water pipe 30 and the branch pipes 31 and 32.
- One end side of the outflow pipes 43 and 44 is connected to the outlet of the catalyst packed columns 41 and 42.
- the other end sides of the outflow pipes 43 and 44 merge to form a pipe 45.
- the tip of the pipe 45 is connected to the gas phase chamber 6 a of the deaeration membrane module 6.
- the configuration of the catalyst packed columns 41 and 42 is the same as that of the catalyst packed column 4 in FIG.
- the outflow pipes 43 and 44 are provided with on-off valves 43a and 44a, respectively.
- deaeration membrane module 6 and the downstream side thereof are the same as those in FIG. 1, and members having the same functions are denoted by the same reference numerals.
- the open / close valve is set to the open / close state shown in FIG. Specifically, the on-off valves 21a, 23a, 32a, 43a are opened, and the on-off valves 22a, 31a, 44a, 46a, 47a are closed.
- raw water is treated by the catalyst packed column 41 and hydrogen is occluded in the platinum group metal catalyst 42a in the catalyst packed column 42.
- Raw Water Treatment The raw water passes through the raw water supply pipe 20, oxygen water from the oxygen-dissolving membrane module 50 is supplied from the pipe 23, and then supplied to the catalyst packed column 41 through the branch pipe 21.
- the organic matter in the raw water comes into contact with the metal catalyst 41a in the column 41 in the presence of hydrogen and oxygen, and the organic matter is efficiently decomposed and removed.
- the water from which the organic matter has been removed flows into the liquid phase chamber 6a of the degassing membrane module 6 through the pipes 43 and 45, and gases such as carbon dioxide, oxygen, and nitrogen are removed.
- the degassed treated water deaerated by the deaeration membrane module 6 flows into the ion exchange resin column 8 through the pipe 7, and undecomposed organic matter, organic acid generated in the process of decomposing the organic matter, and the like in the column 8. It is adsorbed and removed by the ion exchange resin 8a.
- the treated water is discharged out of the system from the treated water pipe 9.
- Hydrogen water produced by the hydrogen-dissolving membrane module 60 flows into the catalyst packed column 42 through the hydrogen water pipe 30 and the pipe 32. Thereby, hydrogen is adsorbed on the platinum group metal catalyst 42 a in the column 42.
- the open / close valve 32a is closed, the open / close valve 22a is opened, the inside of the catalyst packed column 42 is filled with raw water, and then the open / close valve 44a is opened. As a result, the raw water is passed through the catalyst packed column 42 and processed.
- the on-off valves 21 a and 43 a are closed, the on-off valve 46 a is opened, and the water in the catalyst packed column 41 is discharged from the pipe 46.
- the on-off valve 46 a is closed, the on-off valve 31 a is opened, hydrogen water is supplied into the catalyst packed column 41, and hydrogen is adsorbed on the platinum group metal catalyst 41 a in the column 41.
- the raw water can be treated continuously by changing the timing of the hydrogen adsorption treatment of the catalyst packed column 41 and the catalyst packed column 42.
- raw water is passed through the catalyst packed column 41 to treat the raw water, and hydrogen water is supplied to the catalyst packed column 42 to perform hydrogen adsorption treatment on the platinum group metal catalyst 42a.
- hydrogen water is supplied to the catalyst packed column 41 to perform hydrogen adsorption treatment on the platinum group metal catalyst 41a, and raw water is passed through the catalyst packed column 42 to treat the raw water.
- the raw water can be continuously treated by alternately switching between the catalyst packed column that performs the raw water treatment and the catalyst packed column that performs the hydrogen adsorption treatment.
- two catalyst-packed columns are used, but three or more catalyst-packed columns can be arranged in parallel, and continuous treatment can be performed by switching between raw water treatment and hydrogen adsorption treatment.
- Example 1 Using the apparatus of FIG. 1, the raw water was treated under the following conditions.
- Platinum group metal catalyst (catalyst resin): “Nano Saver” (platinum nano colloid carrying resin) manufactured by Kurita Kogyo Co., Ltd., 360 mL
- Degassing membrane module “Lixel G420” manufactured by Celgard Ion exchange resin: Strongly basic anion exchange resin “KR-U” manufactured by Kurita Kogyo Co., Ltd. A1 ”221.5 mL and Kurita Kogyo's strong acid cation exchange resin“ KR-UC1 ”138.5 mL mixed resin Water volume: 0.72 L / min
- the on-off valve 2a of the oxygen supply pipe 2 and the on-off valve 3a of the hydrogen supply pipe 3 were closed, and oxygen and hydrogen were not supplied to the raw water.
- the dissolved oxygen concentration of the raw water at the inlet of the catalyst packed column 4 was 20 ppb.
- the metal catalyst was previously adsorbed with hydrogen.
- Example 1 The raw water was treated in the same manner as in Example 1 except that a low-pressure UV lamp device (“AZ-26” manufactured by Nippon Photo Science Co., Ltd.) was used instead of the catalyst packed column 4 and the amount of raw water was 5 L / min. went.
- a low-pressure UV lamp device (“AZ-26” manufactured by Nippon Photo Science Co., Ltd.) was used instead of the catalyst packed column 4 and the amount of raw water was 5 L / min. went.
Abstract
Description
(1)有機物含有排水を直接RO膜分離装置に通水して有機物を除去する方法
(2)有機物含有排水に酸化剤を添加して有機物を加熱分解する方法
(3)有機物含有排水に紫外線(UV)を照射して有機物を分解する方法(例えば、特許文献2)
などがある。
第1図は本発明の有機物含有水の処理方法及び装置の実施の形態を示す系統図である。第1図において、閉状態の開閉弁は黒塗りとし、開状態の開閉弁は白ヌキとされている。先ず処理装置の構成を説明する。
第1図の通り、開閉弁1aを備えた原水供給配管1が、触媒充填カラム(反応容器)4の流入口に接続されている。原水供給配管1の途中には、開閉弁2aを備えた酸素供給配管2と、開閉弁3aを備えた水素供給配管3とが接続されている。
触媒充填カラム4に充填される白金族金属触媒4aの白金族金属としては、ルテニウム、ロジウム、パラジウム、オスミウム、イリジウム及び白金を挙げることができる。これらの白金族金属は、1種を単独で用いることができ、2種以上を組み合わせて用いることもできる。また、2種以上の金属よりなる合金として用いることもできる。また、天然に産出される混合物の精製品を単体に分離することなく用いることもできる。これらの中で、白金、パラジウム、白金/パラジウム合金の単独又はこれらの2種以上の混合物は、触媒活性が強いので特に好適に用いることができる。
次に、被処理水中の有機物(TOC成分)を除去する有機物除去工程について説明する。
この結果、白金族金属触媒表面の電子が粗の部分に尿素等の有機物の有する非共有電子対が結合(吸着)していると推測される。
そして、続いて水素を供給することで、酸素が水素と接触して水になる際に、非共有電子対の結合が切れて有機物が金属触媒上から脱離し元の状態に戻る。このように有機物の吸着、脱離を繰り返すことで、有機物が分解され、原水から除去されるものと考えられる。
上記の有機物除去工程を継続することにより、触媒充填カラム4内の白金族金属触媒4aの水素吸着量が少なくなった場合、水素吸着工程を実施する。
第2図は本発明の有機物含有水の処理方法及び装置の別の実施の形態を示す系統図である。第2図において、閉状態の開閉弁は黒塗りとし、開状態の開閉弁は白ヌキとされている。
原水供給配管20が、開閉弁21aを備えた分岐管21と開閉弁22aを備えた分岐管22とに分岐している。分岐管21,22が触媒充填カラム41,42の流入口に接続されている。原水供給配管20の途中部分に、開閉弁23aを備えた酸素水配管23の一端側が接続され、該配管23の他端側が酸素溶解膜モジュール50の液相室50aに接続されている。
酸素ガス供給配管51から気相室50bに酸素ガスが供給されると共に、給水配管54から液相室50aに水が供給される。気相室50b内に供給された酸素ガスの一部が、気体透過膜50cを透過して液相室50a内の水に溶解する。気相室50b内の酸素ガスの残部が、液相室50aから気体透過膜50cを透過してきた水蒸気やその凝縮水と共に、真空ポンプ53に吸引されて排出配管52から排出される。この液相室50a内の酸素水が、酸素水配管23を介して原水供給配管20に供給される。
水素ガス供給配管61から気相室60bに水素ガスが供給されると共に、給水配管64から液相室60aに水が供給される。気相室60b内に供給された水素ガスの一部が、気体透過膜60cを透過して液相室60a内の水に溶解する。気相室60b内の水素ガスの残部が、液相室60aから気体透過膜60cを透過してきた水蒸気やその凝縮水と共に排出配管62から排出される。この液相室60a内の水素水が、水素水配管30及び分岐管31,32を介して原水供給配管20の分岐管21,22に供給される。
開閉弁を第2図に示す開閉状態にする。具体的には、開閉弁21a,23a,32a,43aを開とし、開閉弁22a,31a,44a,46a,47aを閉とする。
原水は、原水供給配管20内を通り、酸素溶解膜モジュール50からの酸素水が配管23より供給された後、分岐管21を通って触媒充填カラム41に供給される。
水素溶解膜モジュール60で製造された水素水が、水素水配管30及び配管32を通って触媒充填カラム42に流入する。これにより、カラム42内の白金族金属触媒42aに水素が吸着する。
上記の運転例を継続することにより、触媒充填カラム41内の白金族金属触媒41aの水素吸着量が少なくなった場合、次の通り、原水の供給先を触媒充填カラム41から触媒充填カラム42に切り替えると共に、触媒充填カラム41内の白金族金属触媒41aに水素を吸着させる。
第1図の装置を用い、以下の条件で原水の処理を行った。
ナノコロイド担持樹脂)、360mL
脱気膜モジュール:セルガード社製「リキセルG420」
イオン交換樹脂:栗田工業(株)製強塩基性アニオン交換樹脂「KR-U
A1」221.5mLと栗田工業(株)製強酸性カチオ
ン交換樹脂「KR-UC1」138.5mLとの混合樹脂
水量:0.72L/min
触媒充填カラム4に代えて低圧UVランプ装置(日本フォトサイエンス社製「AZ-26」)を用い、原水の水量を5L/minとしたこと以外は実施例1と同様にして、原水の処理を行った。
Claims (14)
- 有機物を含有する被処理水を白金族金属触媒に接触させ、該有機物を除去することを特徴とする有機物含有水の処理方法。
- 請求項1において、該白金族金属触媒が水素を吸着していることを特徴とする有機物含有水の処理方法。
- 請求項2において、該被処理水が溶存酸素を含有していることを特徴とする有機物含有水の処理方法。
- 請求項2において、該白金族金属触媒に水素を供給して水素を吸着させる水素吸着工程と、この水素を吸着させた該白金族金属触媒に該被処理水を接触させて有機物を除去する有機物除去工程とを交互に実施することを特徴とする有機物含有水の処理方法。
- 請求項4において、該白金族金属触媒を収容した反応容器を複数個用い、一部の反応容器で水素吸着工程を行っているときに他の反応容器で有機物除去工程を行うことを特徴とする有機物含有水の処理方法。
- 請求項1において、該白金族金属触媒が白金族金属の微粒子よりなることを特徴とする有機物含有水の処理方法。
- 請求項6において、該白金族金属触媒の微粒子が担体に担持されていることを特徴とする有機物含有水の処理方法。
- 請求項3において、該被処理水中の溶存酸素濃度が1ppb~100ppbであることを特徴とする有機物含有水の処理方法。
- 請求項1において、該被処理水を該白金族金属触媒に接触させた後、この水をアニオン交換樹脂及びカチオン交換樹脂の少なくとも一方と接触させることを特徴とする有機物含有水の処理方法。
- 請求項9において、該被処理水を該白金族金属触媒に接触させた後、この水を脱気処理し、次いで、この脱気処理水をアニオン交換樹脂及びカチオン交換樹脂の少なくとも一方と接触させることを特徴とする有機物含有水の処理方法。
- 請求項1において、被処理水が超純水製造用の被処理水であることを特徴とする有機物含有水の処理方法。
- 有機物及び溶存酸素を含有する被処理水を、水素を吸着している白金族金属触媒に接触させて有機物を除去する装置であって、
それぞれ白金族金属触媒を収容した複数個の反応容器と、
該反応容器に被処理水を供給する給水手段と、
該反応容器に水素を供給する水素供給手段と、
該反応容器への被処理水の供給と水素の供給とを切り替える切替手段と
を有しており、
該切替手段は、水素を供給して水素吸着工程を行わせる反応容器を順次に切り替えるものであって、且つ水素吸着工程を行っている反応容器以外の反応容器に対して被処理水を供給して有機物除去工程を行わせるように構成されていることを特徴とする有機物含有水の処理装置。 - 請求項12において、前記反応容器から流出した処理水が導入される、アニオン交換樹脂及びカチオン交換樹脂の少なくとも一方を有するイオン交換手段を備えたことを特徴とする有機物含有水の処理装置。
- 請求項13において、前記反応容器から流出した処理水が導入される脱気装置を備えており、
該脱気装置からの脱気処理水が前記イオン交換手段に導入されることを特徴とする有機物含有水の処理装置。
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KR20110053946A (ko) | 2011-05-24 |
JP5447378B2 (ja) | 2014-03-19 |
US20110180491A1 (en) | 2011-07-28 |
TWI504569B (zh) | 2015-10-21 |
JPWO2010013677A1 (ja) | 2012-01-12 |
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