WO2015050125A1 - 超純水製造装置 - Google Patents
超純水製造装置 Download PDFInfo
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- WO2015050125A1 WO2015050125A1 PCT/JP2014/076109 JP2014076109W WO2015050125A1 WO 2015050125 A1 WO2015050125 A1 WO 2015050125A1 JP 2014076109 W JP2014076109 W JP 2014076109W WO 2015050125 A1 WO2015050125 A1 WO 2015050125A1
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- ultrapure water
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/58—Multistep processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/025—Reverse osmosis; Hyperfiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/04—Feed pretreatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/147—Microfiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/149—Multistep processes comprising different kinds of membrane processes selected from 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
- C02F1/44—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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- 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
- B01D2311/04—Specific process operations in the feed stream; Feed pretreatment
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- 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
- B01D2311/06—Specific process operations in the permeate stream
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- 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
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/2611—Irradiation
- B01D2311/2619—UV-irradiation
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- 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
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/2623—Ion-Exchange
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- 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
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/263—Chemical reaction
- B01D2311/2634—Oxidation
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- 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
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/2653—Degassing
- B01D2311/2657—Deaeration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2317/00—Membrane module arrangements within a plant or an apparatus
- B01D2317/02—Elements in series
- B01D2317/025—Permeate series
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2317/00—Membrane module arrangements within a plant or an apparatus
- B01D2317/04—Elements in parallel
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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
- 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
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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
- C02F2209/10—Solids, e.g. total solids [TS], total suspended solids [TSS] or volatile solids [VS]
- C02F2209/105—Particle number, particle size or particle characterisation
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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
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
Definitions
- the present invention relates to an ultrapure water production apparatus, and more particularly to an ultrapure water production apparatus including a primary pure water system and a subsystem.
- the ultrapure water used as semiconductor cleaning water is manufactured by an ultrapure water production apparatus including a primary pure water system, a subsystem (secondary pure water system), and the like.
- a pretreatment system may be provided before the primary pure water system.
- suspended substances and colloidal substances in raw water are removed by means of agglomeration, pressurized flotation (precipitation), filtration (membrane filtration) devices and the like.
- primary pure water is produced by removing ions, organic components, etc. from the water using a reverse osmosis membrane separation device, deaeration device, and ion exchange device (mixed bed type or 4 bed 5 tower type). Is done.
- primary pure water is highly processed into ultrapure water by a low-pressure ultraviolet oxidation device, an ion exchange pure water device, an ultrafiltration membrane (UF membrane) device, or the like.
- UF membrane ultrafiltration membrane
- a UF membrane device is arranged to remove fine particles generated from ion exchange resin or the like.
- UF membrane devices are mainly used as membrane devices installed at the last stage of the subsystem.
- MF membrane microfiltration membrane
- UF membrane microfiltration membrane
- RO membrane reverse osmosis membrane
- a membrane separator may be provided in two stages in series in the subsystem (Patent Documents 1 to 4).
- 2 and 3 of Patent Document 1 describe that a UF membrane device and an ion exchange group-modified MF membrane device are installed in series in this order at the last stage of the ultrapure water production device.
- FIG. 4A of Patent Document 2 describes that a reverse osmosis membrane (RO membrane) device is provided after the UF membrane device at the end of the secondary pure water device.
- Patent Document 3 describes that a secondary pure water device is provided with a UF membrane device and an anion adsorption membrane device having a pore diameter of 500 to 5000 mm.
- Patent Document 4 a pre-filter for blocking particles having a particle size of 0.01 mm (10 ⁇ m) or more is provided in front of a UF or MF (microfiltration) membrane device used as a separation membrane module for producing ultrapure water.
- UF or MF microfiltration
- Patent Document 3 specifically shows a hollow fiber membrane having a pore diameter of 0.2 ⁇ m (2000 mm), a porosity of 60%, and a film thickness of 0.35 mm as an anion-adsorbing membrane (paragraph 0023). According to this anion adsorption membrane, silica can be removed to a high degree, but there is a disadvantage that fine particles of ultrapure water level cannot be removed.
- the prefilter of Patent Document 4 is for preventing dust having a size of 10 ⁇ m or more from colliding with the UF or MF membrane in the last stage and causing membrane damage, and particles smaller than 10 ⁇ m are not removed.
- Patent Documents 1 to 4 describe that the membrane device is provided in multiple stages as the terminal fine particle removal unit of the subsystem. However, any of the sufficiently satisfactory fine particle removal effects can be obtained. It was not a thing.
- JP 2004-283710 A JP2003-190951 JP-A-10-216721 JP-A-4-338221
- An object of the present invention is to provide an ultrapure water production apparatus capable of stably producing high quality ultrapure water from which fine particles are highly removed.
- the ultrapure water production apparatus of the present invention has a subsystem for producing ultrapure water from primary pure water.
- a membrane device is provided at the last stage of the subsystem.
- the membrane devices are installed in multiple stages in series, the first membrane device is a UF membrane device, MF membrane device or RO membrane device, and the last membrane device is UF membrane device or ion-exchange group modified. There is no MF membrane device.
- UF membrane devices are preferably installed in two stages in series.
- an MF membrane device, an RO membrane device, and a UF membrane device may be installed in three stages in this order.
- fine particle measuring means for measuring the number of fine particles of treated water in the membrane device to manage the fine particles of treated water.
- one particle measuring means When measuring the number of treated water particles in two or more membrane devices, one particle measuring means may be provided for each membrane device, and one particle measuring means is provided for a plurality of membrane devices. In order to measure the number of fine particles, the number of fine particles of treated water in each membrane device is measured by one fine particle measuring means by sequentially switching the treated water supplied from each membrane device to the fine particle measuring means. It may be configured as follows.
- an automatic valve for branching to the treated water extraction pipe of each of the two or more membrane modules provided in parallel, collecting water for measuring the number of particles and feeding it to the particle measuring means is provided. It is preferable to provide a water sampling pipe to be provided, and to switch the membrane module to be sampled by this automatic valve so as to sequentially measure the number of treated water particles in each membrane module. Further, the treated water from the membrane modules constituting the membrane device merges, and the number of fine particles can be similarly measured for the treated water of the membrane device. It is preferable to branch off a water sampling pipe provided with an automatic valve. A manual valve may be used instead of the automatic valve.
- UF membrane devices and the like are provided in a multistage in the last stage of the subsystem, and ultrapure water with high water quality with a remarkably small number of fine particles is produced. According to the present invention, it is possible to produce high-quality ultrapure water having a particle diameter of 10 nm or more and a number of fine particles lower than 100 / L.
- the membrane device on the most downstream side is a UF membrane device or an MF membrane device not subjected to ion exchange group modification. There is no risk of occurrence. Since an MF membrane device that is not modified with an ion exchange group is used as the MF membrane device, there is no disadvantage that the exchange base is detached and becomes a fine particle source.
- a fine particle measuring means for measuring the number of fine particles of the treated water of the membrane device immediately before the last stage and / or the treated water of the final stage membrane apparatus is provided, and if necessary, based on the measurement result of the fine particle measuring means.
- By performing maintenance such as membrane exchange it is possible to stably and reliably produce high-quality ultrapure water having a particle diameter of 10 nm or more and a number of fine particles lower than 100 / L.
- the fine particles accumulate on the membrane surface over time, so that the fine particles may leak into the treated water, or when the membrane is damaged due to some external load. There is also a risk that fine particles may leak into the treated water and reduce the quality of the obtained ultrapure water, but by providing such a fine particle measuring means and monitoring and managing the number of fine particles in the membrane treated water, Leakage of fine particles to the treated water can be prevented in advance.
- the membrane device is installed in series in two or more stages on the last stage side of the subsystem.
- An example of the overall flow of the ultrapure water production apparatus having this subsystem is shown in FIGS.
- Each of the ultrapure water production apparatuses shown in FIGS. 1 to 3 includes a pretreatment system 1, a primary pure water system 2, and a subsystem 3.
- the pretreatment system 1 comprising agglomeration, pressurized flotation (precipitation), filtration device, etc.
- suspended substances and colloidal substances in raw water are removed.
- the primary pure water system 2 equipped with a reverse osmosis (RO) membrane separation device, a deaeration device, and an ion exchange device (mixed bed type, two-bed three-column type, or four-bed five-column type), ions and organic components in raw water are removed. I do.
- the RO membrane separation apparatus removes ionic and colloidal TOC in addition to removing salts.
- the ion exchange device in addition to removing salts, the TOC component adsorbed or ion exchanged by the ion exchange resin is removed.
- the degassing device nitrogen degassing or vacuum degassing
- the dissolved oxygen is removed.
- the primary pure water thus obtained (normally, pure water with a TOC concentration of 2 ppb or less) is used as a sub tank 11, a pump P, a heat exchanger 12, and a UV oxidation apparatus 13. Then, water is sequentially passed through the catalytic oxidant decomposition device 14, the deaeration device 15, the mixed bed deionization device (ion exchange device) 16, the first membrane device 17 for removing fine particles, and the second membrane device 18.
- the collected ultrapure water is sent to youth point 19.
- UV oxidizer 13 a UV oxidizer that irradiates UV having a wavelength near 185 nm, which is usually used in an ultrapure water production apparatus, for example, a UV oxidizer using a low-pressure mercury lamp can be used.
- This UV oxidation apparatus 13 primary pure water TOC is organic acid, further is decomposed into CO 2. Further, in the UV oxidizer 13, H 2 O 2 is generated from water due to the excessively irradiated UV.
- the treated water of the UV oxidizer 13 is then passed through a catalytic oxidant decomposition device 14.
- the oxidant decomposition catalyst of the catalytic oxidant decomposition apparatus 14 include noble metal catalysts known as redox catalysts, such as palladium (Pd) compounds such as metal palladium, palladium oxide, palladium hydroxide, or platinum (Pt), Of these, a platinum (Pt) catalyst having a strong reducing action can be preferably used.
- the catalytic oxidant decomposition device 14 efficiently decomposes and removes H 2 O 2 generated in the UV oxidizer 13 and other oxidants by the catalyst. Then, by decomposition of H 2 O 2, water is generated, almost no possible to produce oxygen as the anion exchange resin and activated carbon, do not cause DO increase.
- the treated water of the catalytic oxidant decomposition device 14 is then passed through the deaeration device 15.
- a vacuum deaerator, a nitrogen deaerator, or a membrane deaerator can be used as the deaerator 15. This deaeration device 15 efficiently removes DO and CO 2 from the water.
- the treated water from the deaerator 15 is then passed through the mixed bed ion exchanger 16.
- the mixed bed type ion exchange device 16 a non-regenerative type mixed bed type ion exchange device in which an anion exchange resin and a cation exchange resin are mixed and filled in accordance with an ion load is used.
- the mixed bed type ion exchange device 16 removes cations and anions in the water and increases the purity of the water.
- a multi-bed type ion exchange device, an electric regeneration type ion exchange device, or the like may be used.
- the ultrapure water production apparatus of the present invention is an example of the ultrapure water production apparatus of the present invention, and the ultrapure water production apparatus of the present invention can be combined with various devices other than those described above.
- the UV irradiation treated water from the UV oxidizer 13 may be introduced into the mixed bed deionizer 16 as it is.
- an anion exchange column 19 may be installed in place of the catalytic oxidant decomposition apparatus 14.
- an RO membrane separation device may be installed after the mixed bed ion exchange device.
- an apparatus for deionizing after decomposing urea and other TOC components in the raw water by heat-decomposing the raw water in an acidic condition of pH 4.5 or less and in the presence of an oxidizing agent may be incorporated.
- the UV oxidation device, the mixed bed ion exchange device, the deaeration device, and the like may be installed in multiple stages. Further, the pretreatment system 1 and the primary pure water system 2 are not limited to those described above, and various other combinations of apparatuses can be adopted.
- any of a UF membrane, an MF membrane, and an RO membrane may be used.
- a UF membrane or an MF membrane that is not modified with an ion exchange group is used. Accordingly, there are the following six combinations of the first film device 17 and the second film device 18. (1) UF membrane-UF membrane (2) UF membrane-MF membrane without ion exchange group modification (3) MF membrane-UF membrane (4) MF membrane-MF membrane without ion exchange group modification (5) RO Membrane-UF membrane (6) RO membrane-MF membrane without ion-exchange group modification
- the membrane device may be installed in three or more stages in series.
- membrane devices may be installed in three stages, such as MF membrane device-RO membrane device-UF membrane device.
- the pore size of the membrane is preferably 1 ⁇ m or less, particularly 0.001 to 1 ⁇ m, and particularly preferably 0.001 to 0.5 ⁇ m.
- the thickness is preferably 0.01 to 1 mm.
- the material include polyolefin, polystyrene, polysulfone, polyester, polyamide, cellulose, polyvinylidene fluoride, and polytetrafluoroethylene.
- a UF membrane apparatus or the like is provided in multiple stages in series at the last stage of the subsystem, and high quality ultrapure water with a remarkably small number of fine particles is produced.
- the most downstream membrane device is a UF membrane device or an MF membrane device that is not modified with an ion exchange group, so that fine particles are generated from the membrane device itself like the RO membrane device. There is no risk. Further, since an MF membrane device that is not modified with an ion exchange group is used as the MF membrane device, there is no disadvantage that the exchange base is detached and becomes a fine particle source.
- the membrane device is preferably a cross-flow type, and the recovery rate is preferably up to about 95% during operation. If the brine flow rate is further reduced, fine particles are deposited on the film surface, which may reduce the fine particle blocking rate.
- the recovery rate may be about 95%, and the number of series stages may be changed according to the quality of the feed water.
- Fine particle removal when the UF membrane device is used in two stages is given by the following equation.
- C 1 C 0 ⁇ (1-Re / 100) + B
- C 2 C 1 ⁇ (1-Re / 100) + B
- C 0 Concentration of fine particles in UF membrane water supply [units / mL]
- C 1 concentration of fine particles in the first-stage UF membrane treated water [units / mL]
- C 2 Concentration of fine particles in the second stage UF membrane treated water [units / mL]
- Re Fine particle rejection rate in UF membrane [%]
- B Number of fine particles generated from the UF membrane material itself [piece / mL]
- the particle rejection rate of the fine particle removal film is calculated by passing model nanoparticles through water and measuring the number of fine particles of water supply and treated water.
- the MF membrane has a larger pore size than the UF membrane, but an adsorption effect on the membrane can be expected due to the difference in membrane material. Since the UF membrane is superior to the MF membrane in terms of the fine particle rejection rate as a membrane, when using the MF membrane and the UF membrane in multiple stages, it is desirable to install a UF membrane device at the end, but this is not restrictive.
- the RO membrane is superior to the UF membrane in terms of the particulate rejection rate, fine particles are generated from the membrane material or potting member. Therefore, when the RO membrane device is installed as the first membrane device, the UF membrane is installed at the most downstream and It is preferable to remove it.
- a boosting pump and a valve may be provided in the middle of each stage of the membrane device installed in series in two stages or three or more stages.
- the membrane devices when the membrane devices are installed in series in multiple stages, the pressure loss increases, so that a pump can be provided between the membrane devices in consideration of the pressure loss.
- a particle filling facility such as a mixed bed type ion exchange device or a catalytic oxidizer decomposition device because fine particles are generated due to particle crushing. It is preferable not to install anything other than clean piping downstream from the last stage UF membrane.
- the apparatus of the present invention it is preferable to pay attention to the range of the recovery rate, because if the recovery rate is set too large, fine particles may be deposited on the film surface. It is preferable to design the particle removal film type and the number of installation stages from the particle diameter of the fine particles to be removed, the flow rate of the water to be treated, and the target water quality.
- the membrane device In the membrane device, if the processing is continued, fine particles accumulate on the membrane surface over time, so that the fine particles may leak into the treated water, and also when the membrane is damaged due to some external load. There is a risk that fine particles leak into the water and the quality of the obtained ultrapure water is lowered. Therefore, in the present invention, it is preferable to prevent the leakage of fine particles into the treated water by providing a fine particle measuring means and monitoring and managing the number of fine particles of the membrane treated water.
- the fine particle measuring means is not particularly limited, and commercially available fine particle measuring means can be used.
- FIG. 4 shows the particle management of the treated water by providing a particle measuring device 31 for measuring the number of treated water particles in the first membrane device 17 and a particle measuring device 32 for measuring the number of treated water particles in the second membrane device 18. It is a flowchart which shows the system which performs.
- first membrane water supply the first-stage treated water supplied to the first membrane device 17 (for example, treated water of the mixed-bed deionizer 16 in the case of the ultrapure water production device of FIGS. 1 to 3) is referred to as “first membrane water supply”.
- second membrane water supply the water supplied to the second membrane device 18 (usually treated water of the first membrane device 17) is referred to as “second membrane water supply”, and the treated water of the first membrane device 17 and the second membrane device 18
- the treated water is referred to as “first membrane treated water” and “second membrane treated water”, respectively.
- the first membrane device 17 and the second membrane device 18 are each provided with three membrane modules 17A to 17C and 18A to 18C in parallel.
- the first membrane feed water is introduced into the membrane modules 17A to 17C of the first membrane device 17 from the pipe 21 via the branch pipes 21a, 21b, 21c, respectively, and the first membrane treated water is supplied to the branch pipes 22a, 22b, 22c and
- the concentrated water is fed to the second membrane device 18 through the collecting pipe 22, and the membrane concentrated water passes through the branch pipes 23a, 23b, 23c and the collecting pipe 23, and enters the inlet side of the subsystem (the ultrapure water production apparatus in FIGS. 1 to 3). For example, it is configured to be returned to the sub tank 11).
- the second membrane supply water (first membrane treated water) is introduced into the membrane modules 18A to 18C of the second membrane device 18 from the collecting pipe 22 via the branch pipes 24a, 24b, and 24c, respectively.
- the treated water is supplied to the use point as ultrapure water through the branch pipes 25a, 25b, 25c and the collective pipe 25, and the membrane concentrated water is supplied to the inlet side of the subsystem through the branch pipes 26a, 26b, 26c and the collective pipe 26 (
- the ultrapure water production apparatus of FIGS. 1 to 3 is configured to be returned to the sub tank 11).
- the branch pipes 22a to 22c for taking the treated water from the respective membrane modules 17A to 17C of the first membrane device 17 and the collecting pipe 22 are used for collecting and feeding a part of the treated water to the particle measuring device 31, respectively.
- the water sampling branch pipes 27a, 27b, 27c, and 27d are connected, and the water sampled in each of the branch pipes 27a to 27d is supplied to the particle measuring device 31 via the collective water sampling pipe 27 to determine the number of particles. Measurement is performed.
- a part of the treated water is sampled and supplied to the particle measuring device 32 to the branch pipes 25a to 25c and the collecting pipe 25 for taking the treated water from the membrane modules 18A to 18C of the second membrane device 18, respectively.
- Water sampling branch pipes 28a, 28b, 28c, and 28d are connected to each other, and the water sampled in each of the branch water sampling pipes 28a to 28d is supplied to the particle measuring device 32 through the collective water sampling pipe 28. Then, the number of fine particles is measured.
- V 1 to V 18 , V 20 , V 30 are automatic valves provided in each pipe.
- the membrane module 17C of the first membrane device 17 and the membrane module 18C of the second membrane device 18 are spare membrane modules, and usually the particulate removal is performed by the membrane modules 17A and 17B and the membrane modules 18A and 18B.
- V 7 to V 9 and V 16 to V 18 are closed, and the automatic valves V 1 , V 2 , and V 4 are closed.
- V 5 , V 10 , V 11 , V 13 , V 14 are open.
- the automatic valve V 3 and V 6 and V 20 are opened and closed sequentially.
- the first membrane water supply is introduced into the membrane modules 17A and 17B from the pipe 21 via the branch pipes 21a and 21b and subjected to membrane treatment, and the treated water is supplied to the second membrane device 18 via the branch pipes 22a and 22b and the collecting pipe 22. Is done.
- the concentrated water in which the fine particles are concentrated by the membrane modules 17A and 17B is returned to the sub tank on the inlet side of the subsystem through the branch pipes 23a and 23b and the collecting pipe 23.
- the first membrane treated water is introduced into the membrane modules 18A and 18B from the collecting pipe 22 via the branch pipes 24a and 24b and subjected to membrane treatment, and the treated water (ultra pure water) is used via the branch pipes 25a and 25b and the collecting pipe 25. Sent to points.
- the concentrated water in which the fine particles are concentrated in the membrane modules 18A and 18B is returned to the sub tank on the inlet side of the subsystem through the branch pipes 26a and 26b and the collecting pipe 26.
- the leakage of fine particles or the fine particle removal rate for each membrane module is measured. While detecting the decrease, the performance of the membrane device itself can be monitored. If any of the membrane module leaks or a decrease in the particulate removal rate is detected, the supply of water to the membrane module is stopped and switched to the water supply to the spare membrane module. Perform removal. Specifically, when it is detected that fine particles begin to leak into the treated water of the membrane module 17A or the fine particle removal rate is lowered, the automatic valves V 1 , V 2 and V 3 are closed and the automatic valve is closed.
- V 7 and V 8 are opened, and V 9 is opened and closed in order with the automatic valve V 6 and the automatic valve V 20 , so that the membrane for removing particulates is treated with the treated water of the membrane module 17 B and the membrane module 17 C.
- a part of the treated water of the membrane module 17B, the treated water of the membrane module 17C, and a part of the first membrane treated water are collected in order, and the fine particle measuring device 31 measures the number of fine particles.
- the membrane module 17A is subjected to maintenance such as membrane exchange.
- the frequency of switching the automatic valve for collecting water for measuring the number of particles is not particularly limited, but the number of particles continuously for 30 to 60 minutes in the membrane treated water of one membrane module and the entire membrane device. It is preferable that the measurement can be performed.
- the membrane treatment is performed by measuring the particulates of the treated water and switching the flow path as necessary. It is possible to reliably prevent the leakage of fine particles into water and to stably obtain high-quality ultrapure water.
- the particle management system shown in FIG. 4 is configured so that the number of particles in each treated water can be measured with one particle measuring device 30 by being sequentially supplied to the particle measuring device 30 through 29. Unlike the others, the configuration is the same.
- the number of particle measuring devices By attaching the particle measuring device to the ultrapure water production apparatus, it is possible to prevent the ultrapure water production apparatus from becoming excessively large, thereby reducing the equipment cost and maintenance work.
- the number of membrane modules provided in the membrane device is not particularly limited, and is usually set in the range of 2 to 20 pieces. Further, the number of spare membrane modules is not limited to one, and two or more may be provided.
- the measurement of the number of fine particles of the membrane treated water may be performed for the last stage membrane apparatus, or may be performed for the last stage membrane apparatus. Further, the number of fine particles of treated water may be measured for all of the membrane devices provided in multiple stages.
- the last stage membrane device is a membrane device that removes fine particles in the final stage. If a certain degree of particulate removal rate is obtained in the membrane device up to the stage immediately before the last stage, the final stage membrane device can treat the treated water into the treated water. In order to prevent leakage of fine particles, it is preferable to provide a fine particle measuring means for measuring the number of fine particles of membrane treated water at least in the membrane device immediately before the last stage. It is preferable to provide fine particle measuring means in both of the stage membrane devices so as to measure the number of fine particles of treated water in these membrane devices.
- the first membrane device 17 and the second membrane device 18 also return their concentrated water (brine water) to the sub-tank, but are not limited to this, and supply it to a separately provided brine recovery tank. You may make it do.
- the fine particle concentration is a value obtained by measuring the number of fine particles having a particle diameter of 10 nm or more in water with a fine particle measuring device by centrifugal filtration-SEM method.
- Example 1 In the ultrapure water production apparatus shown in FIG. 1, a UF membrane device (external pressure type hollow fiber membrane, material: polysulfone, nominal molecular weight cut off: 6,000) is used as the first membrane device 17 and the second membrane device 18 at the end of the subsystem. (Insulin), rejection rate Re: 99.90%) was installed to produce ultrapure water. Table 1 shows the measurement results of the fine particle concentration of the water supply and treated water of each membrane device.
- the concentration of fine particles in the treated water of the first membrane device 17 in the first stage is 1,000 / L or more, but the concentration of fine particles in the treated water of the second membrane device 18 is 51 / L. It was confirmed that the fine particle concentration was 100 particles / L or less by installing the UF membrane device in two stages.
- Example 2 Ultrapure water was produced in the same manner as in Example 1 except that the combination of the membranes of the first membrane device and the second membrane device was as shown in Table 2, and the fine particle concentration was determined by measuring the number of fine particles in water. . The results are shown in Table 2.
- MF membrane device not modified with ion exchange groups external pressure type hollow fiber membrane, material: surface modified PTFE, pore diameter 50 nm RO membrane device: Spiral type, Material: Polyamide
- Example 7 Ultra pure water is produced in the same manner as in Example 1 except that the membrane device is a three-stage installation of MF membrane device-RO membrane device-UF membrane device, and the number of fine particles in water is measured to obtain the fine particle concentration. It was. The results are shown in Table 2. In addition, the above-mentioned thing was used as each film
- Example 8 In Example 1, as shown in FIG. 4, a fine particle measuring device (“NanoCount 25+” manufactured by Lighthouse) for measuring the number of fine particles in the treated water of each of the UF membrane device of the first membrane device 17 and the UF membrane device of the second membrane device 18. ]) 31 and 32 were provided to produce ultrapure water.
- NemoCount 25+ manufactured by Lighthouse
- the UF membrane devices of the first membrane device 17 and the second membrane device 18 have UF membrane modules 17A to 17C and UF membrane modules 18A to 18C, respectively.
- the UF membrane modules 17C and 18C are spare membrane modules, and are always UF. Processing was performed with the membrane modules 17A and 17B and the UF membrane modules 18A and 18B.
- the first membrane device 17 by switching the automatic valve V 3 and V 6 and V 20 (1 times the frequency 30 minutes), the treated water and the first treated water and the UF membrane module 17B of the UF membrane module 17A
- the first membrane treated water of the membrane device 17 was sequentially fed to the particle measuring device 31 to measure the number of particles.
- the second membrane unit 18 by switching the automatic valve V 12 and V 15 and V 30 (1 times the frequency 30 minutes), the treated water in the treated water and UF membrane module 18B of the UF membrane module 18A second
- the second membrane treated water of the membrane device 18 was sequentially fed to the particle measuring device 32 and the number of particles was measured.
- FIGS. 6A and 6B show the changes over time in the concentration of fine particles obtained from the measurement results of the number of fine particles of treated water in the UF membrane module 17A and the UF membrane module 17B.
- the UF membrane modules provided in the same membrane device are as shown in FIGS. Even in such a case, there was a difference in durability for each lot, and it was confirmed that fine particle leakage started earlier in the UF membrane module 18A than in the UF membrane module 18B.
- the automatic valve is switched to immediately pass the first membrane water supply from the flow path for supplying the UF membrane module 17A and the UF membrane module 17B to the spare UF membrane module 17B.
- high quality ultrapure water having a fine particle concentration of 100 particles / L or less was supplied from the second membrane device 18 over a long period of time as in the first embodiment. I was able to obtain it stably.
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Abstract
Description
(1) UF膜-UF膜
(2) UF膜-イオン交換基修飾されていないMF膜
(3) MF膜-UF膜
(4) MF膜-イオン交換基修飾されていないMF膜
(5) RO膜-UF膜
(6) RO膜-イオン交換基修飾されていないMF膜
C1=C0×(1-Re/100)+B
C2=C1×(1-Re/100)+B
C0:UF膜給水中の微粒子濃度[個/mL]
C1:1段目UF膜処理水中の微粒子濃度[個/mL]
C2:2段目UF膜処理水中の微粒子濃度[個/mL]
Re:UF膜での微粒子阻止率[%]
B:UF膜材自体から発生する微粒子数[個/mL]
微粒子除去膜の粒子阻止率は、モデルナノ粒子を通水して給水と処理水の微粒子数を測定することにより算出する。
V1~V18,V20,V30は各配管に設けられた自動弁である。
図1に示す超純水製造装置において、サブシステムの末端の第1膜装置17及び第2膜装置18としてUF膜装置(外圧型中空糸膜、材質:ポリスルホン、公称分画分子量:6,000(インシュリン)、阻止率Re:99.90%)を設置し、超純水を製造した。各膜装置の給水及び処理水の微粒子濃度の測定結果等を表1に示す。
第1膜装置と第2膜装置の膜の組み合わせを表2の通りとしたこと以外は実施例1と同様にして超純水を製造し、水中の微粒子数を測定して微粒子濃度を求めた。結果を表2に示す。なお、UF膜装置以外の各膜装置としては、次のものを用いた。
イオン交換基修飾されていないMF膜装置:外圧型中空糸膜、材質:表面改質PTFE、孔径50nm
RO膜装置:スパイラル型、材質:ポリアミド
膜装置をMF膜装置-RO膜装置-UF膜装置の3段直列設置としたこと以外は実施例1と同様にして超純水を製造し、水中の微粒子数を測定して微粒子濃度を求めた。結果を表2に示す。なお、各膜装置としては上記のものを用いた。
実施例1において、図4に示す通り、第1膜装置17のUF膜装置と第2膜装置18のUF膜装置のそれぞれの処理水中の微粒子数を測定する微粒子測定器(Lighthouse社製「NanoCount25+」)31,32を設けて超純水の製造を行った。
本出願は、2013年10月4日付で出願された日本特許出願2013-209175及び2014年1月28日付で出願された日本特許出願2014-013478に基づいており、その全体が引用により援用される。
2 一次純水システム
3 サブシステム
17 第1膜装置
17A,17B,17C 第1膜モジュール
18 第2膜装置
18A,18B,18C 第2膜モジュール
30,31,32 微粒子測定器
Claims (10)
- 一次純水から超純水を製造するサブシステムを有する超純水製造装置であって、
該サブシステムの最後段に膜装置が設けられている超純水製造装置において、
該膜装置が直列に多段に設置されており、第1段の膜装置はUF膜装置、MF膜装置又はRO膜装置であり、最後段の膜装置はUF膜装置又はイオン交換基修飾されていないMF膜装置であることを特徴とする超純水製造装置。 - 請求項1において、前記膜装置として、UF膜装置が直列に2段に設置されていることを特徴とする超純水製造装置。
- 請求項1において、前記膜装置として、MF膜装置、RO膜装置及びUF膜装置がこの順に3段に設置されていることを特徴とする超純水製造装置。
- 請求項1ないし3のいずれか1項において、前記最後段の直前の段の膜装置の処理水の微粒子数を測定する微粒子測定手段を設けたこと特徴とする超純水製造装置。
- 請求項1ないし4のいずれか1項において、前記最後段の膜装置の処理水の微粒子数を測定する微粒子測定手段を設けたこと特徴とする超純水製造装置。
- 請求項4又は5において、2以上の前記膜装置の処理水の微粒子数を測定する微粒子測定手段を設けたことを特徴とする超純水製造装置。
- 請求項6において、前記微粒子測定手段は、各膜装置毎に設けられていることを特徴とする超純水製造装置。
- 請求項6において、複数の膜装置に対して1台の前記微粒子測定手段が設けられており、微粒子数測定のために各膜装置から該微粒子測定手段に送給する処理水を順番に切り換えることにより、該1台の微粒子測定手段で各々の膜装置の処理水の微粒子数の測定が行われることを特徴とする超純水製造装置。
- 請求項1ないし8のいずれか1項において、前記膜装置は、並列に設けられた2以上の膜モジュールを有し、
該2以上の膜モジュールの各々の処理水の取出配管から分岐した、微粒子数測定のための水を採水して前記微粒子測定手段に送給するための、自動弁を備えた採水配管が設けられており、
該自動弁の切り換えにより、各膜モジュール毎の処理水の微粒子数の測定が行われるように構成されていることを特徴とする超純水製造装置。 - 請求項9において、更に、前記2以上の膜モジュールからの各処理水が合流する前記膜装置の処理水の取出配管に分岐して、微粒子数測定のための水を採水して前記微粒子測定手段に送給するための、自動弁を備えた採水配管が設けられており、
前記2以上の膜モジュールの各々の処理水の取出配管から分岐した採水配管に設けられた自動弁と、該膜装置の処理水の取出配管から分岐した採水配管に設けられた自動弁の切り換えにより、該各膜モジュール毎の処理水の微粒子数と該膜装置の処理水の微粒子数との測定が行われるように構成されていることを特徴とする超純水製造装置。
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CN201480048799.XA CN105517960A (zh) | 2013-10-04 | 2014-09-30 | 超纯水制造装置 |
US15/021,178 US20160220958A1 (en) | 2013-10-04 | 2014-09-30 | Ultrapure water production apparatus |
KR1020167005770A KR102092441B1 (ko) | 2013-10-04 | 2014-09-30 | 초순수 제조 장치 |
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- 2014-09-30 US US15/021,178 patent/US20160220958A1/en not_active Abandoned
- 2014-09-30 CN CN201480048799.XA patent/CN105517960A/zh active Pending
- 2014-09-30 KR KR1020167005770A patent/KR102092441B1/ko active IP Right Review Request
- 2014-09-30 WO PCT/JP2014/076109 patent/WO2015050125A1/ja active Application Filing
- 2014-09-30 JP JP2015540505A patent/JP6304259B2/ja active Active
- 2014-10-03 TW TW103134566A patent/TWI627995B/zh active
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Also Published As
Publication number | Publication date |
---|---|
JP6304259B2 (ja) | 2018-04-04 |
CN105517960A (zh) | 2016-04-20 |
KR102092441B9 (ko) | 2022-06-07 |
JPWO2015050125A1 (ja) | 2017-03-09 |
US20160220958A1 (en) | 2016-08-04 |
KR102092441B1 (ko) | 2020-03-23 |
KR20160065813A (ko) | 2016-06-09 |
TWI627995B (zh) | 2018-07-01 |
TW201532660A (zh) | 2015-09-01 |
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